Dionex applications

Anions in Brewed Coffee by High Pressure Capillary IC on IonSwift MAX-100 Column

2011-05-08T15:02:18.627

Anions and Organic Acids in Brewed Caffeinated Coffee by High Pressure Capillary IC on IonSwift MAX-100 column. This application demonstrates the separation of many organic acids commonly found in complex samples. The method uses the speed advantages of monoliths with the anion-exchange chemistry to separate many organic acids. Additionally, this is a capillary application on ICS-5000 capillary system.

Fast Determination of Anions in Municipal Drinking Water

2011-06-22T10:17:36.72

One of the important applications of ion chromatography is to determine common anions in water samples. A fast determination of anions in a municipal drinking water using IonPac AS18 Fast column is shown here.

AN223: Determination of Ten Active Ingredients in Sunscreen-Containing Products in a Single Injection

2010-02-12T17:40:45.38

In this Application Note (AN) we developed a separation of the following 10 compounds used in sunscreen: 2-phenyl-benzimidazole-5-sulfonic acid, benzophenone-3, diethylamino-hydroxybenzoylhexylbenzoate, 4-methylbenzylidine-camphor, octocrylene, methylanthranilate, octyl-methoxycinnamate, butylmethoxydibenzoylmethane, octyl-salicylate, and homosalate. A manufacturer of sunscreen products chose these 10 compounds and requested baseline resolution of all 10 in a single injection. Using a 3-μm Acclaim® 120 C18 column with an ethanol-containing mobile phase we were able to baseline resolve all 10 compounds in less than 12 min. The Acclaim 120 C18 column paired with a Dionex UltiMate® 3000 system is an ideal platform for developing methods to determine sunscreen ingredients in a variety of products.

Trace Anion Standard by Concentration Using Cap IC and ICW-3000 Online Water Purifier

2011-12-12T21:32:01.47

Trace Anion Standard by Concentration Using Cap IC and ICW-3000 Online Water Purifier. Here we show the chromatogram of 200 uL of a ~100 ng/L 7-Anion Standard concentrated on a IonSwift MAC-100 concentrator column. Trace ion determinations in Ultra-Pure Water (UPW) are important analysis for the electronic industry because ionic contamination at µg/L and ng/L concentrations can cause corrosion of important process equipment resulting in unplanned and costly maintenance. Additionally, ionic contamination in the electronic industry causes poor yields and early end-of-life failures of important semiconductor and disk drive components. Trace ion determinations have been thoroughly discussed in application documents published from 1996 to 2009. However, detection limits, sample handling, and blank stability have all been improved by recent advances in Dionex ion chromatography (IC) technology, including capillary IC, the Dionex AS-AP autosampler, and the ICW-3000 Online Water Purifier.

AN197: Determination of Glucosamine in Dietary Supplements Using HPAE-PAD

2010-02-19T15:20:54.597

Glucosamine (GlcN), an amino sugar, occurs naturally in the human body. It is a major structural component in the biosynthesis of glycosaminoglycans, compounds involved in normal joint function. Use of GlcN as a dietary supplement in the management of osteoarthritis has attracted considerable attention. Carbohydrates, glycols, alcohols, amines, and sulfur-containing compounds can be oxidized and therefore detected directly using amperometry. Pulsed amperometric detection (PAD) is ideally suited for determination of GlcN and related substances. This detection method is specific for those analytes such as GlcN that can be oxidized at a selected potential, leaving all other compounds undetected. High-performance anion-exchange with pulsed amperometric detection (HPAE-PAD) chromatography is a sensitive, direct-detection technique capable of separating mono- and disaccharides rapidly and efficiently. At approximately pH 12, the CarboPac® PA20 anion-exchange column will separate and elute neutral monosaccharides, aminosaccharides, and disaccharides while retaining oligosaccharides. Generating highly reproducible retention times for HPAE chromatographic systems relies on the use of a high purity hydroxide eluent mobile phase prepared with an accurate and precise concentration. An eluent generator (EG) produces such an eluent.

RSLC Resolution of PEG 3000 with Charged Aerosol Detection

2010-10-21T10:16:23.563

The characterization of complex mixtures such as PEG 3000 can be achieved using RSLC columns, the UltiMate 3000 system, and the Corona ultra detector (CAD ultra).

Determination of Cations in a Brewed Coffee Sample Using Capillary IC

2011-06-21T15:22:28.14

One of the important applications of ion chromatography is to analyze inorganic cations in beverages. This chromatogram shows the determination of common cations in a brewed coffee sample using capillary IC. The separation was carried on IonPac CS16 column.

Efficient Separations of Inorganic Anions in Sunnyvale Municipal Water Samples

2012-01-04T17:19:23.063

Five inorganic anions in Sunnyvale municipal water samples were determined on Thermo Scientific Dionex IonPac AS18-Fast analytical column with other well-established techniques (automated eluent generation, self-regenerating suppression, and highly sensitive and selective detection mode). The “Fast” (150 mm) version of the 2 mm column provides advantages to determination of inorganic anions by providing improved resolution and fast run time and excellent value to customers by high throughput, fast separations and high resolution.

Determination of oxyhelides in water using IonPac AS18 4um

2011-11-28T14:01:55.657

It is shown here that chorite and chlorate can be separated from other common inorganic anions within 10 minutes using IonPac AS18 4um column. The analysis was performed using capillary ICS-5000 with EG to generate 30 mM KOH.

Fast Analysis of Inorganic Anions in San Jose Municipal Drinking Water Samples

2012-01-04T17:03:23.61

The recent introduction of Thermo Scientific Dionex IonPac AS18-Fast analytical column provides new ways to achieve improved resolution of critical pairs with faster separations. Inorganic anions in San Jose municipal water samples are baseline resolved within 4 minutes on the “Fast” (150 mm) version of the 2 mm column. The improved resolution and column efficiency are particularly advantageous for fast version column when compared to longer length scale analytical column.

AN187: Determination of Sub-µg/L Bromate in Municipal and Natural Waters

2010-02-23T17:43:31.093

In this application, we demonstrate the use of a two-dimensional (2-D) ion chromatography (IC) system for the determination of trace concentrations of bromate in municipal and natural mineral waters with high ionic strength matrices. The first dimension uses a high capacity 4-mm IonPac AS19 column to resolve the bromate from the matrix ions. The matrix ions are diverted to waste while a 2 mL plug (cut volume) containing the bromate is transferred to the second dimension for analysis. Bromate is well resolved in the second dimension using a 2-mm IonPac AS24 column. This method is fully automated using an ICS-3000 Reagent-Free™ IC (RFIC™) system. In addition, this 2-D IC method achieves bromate detection limits equivalent to or better than postcolumn addition methods. The 2-D IC method avoids the cost and disposal of the chemicals required for postcolumn configurations and simplifies the experimental setup. Additionally, it avoids potential column overload during analysis of high ionic strength matrices.

Carbohydrates in Apple Juice Using Capillary HPAE-PAD

2010-11-14T13:59:48.657

cap IC_PA20_Apple Juice. Monosaccharides were determined in an apple juice sample on a capillary CarboPac PA2 column by capillary HPAE-PAD. An ICS-5000 capillary system was used for all of the analysis.

Determination of Inorganic Cations in Sports Drink G2 using CS12 and Capillary IC

2011-05-03T16:41:50.5

Inorganic cations in reduced carbonated sports drink G2 were separated on IonPac column CS12 using capillary ICS-5000 Reagent-Free Ion Chromatography (RFIC) system. Sample was diluted 10 fold prior to analysis. All peaks were eluted within 10 minutes.

Indometacin Suppositories Related Substances according to the Chinese Pharmacopoeia

2010-02-05T16:29:27.633

This method describes how to assess the Related Substances of Indometacin Capsules according to the Chinese Pharmacopoeia Preparing the Test Solution: Weigh accurately 10 suppositories, cut carefully and mix well. To a quantity, equivalent to about 25 mg of Indometacin, accurately weighed, add a quantity of ethanol to a 50 mL volumetric flask, heat on water bath to dissolve Indometacin, cool to room temperature, and dilute with ethanol to the volume, mix well, and filter. Measure accurately 5 mL of the successive filtrate in a 25 mL volumetric flask, dilute with 50% ethanol solution to the volume, and mix well. Preparing the Reference Solution: Measure accurately 1 mL of the test solution in a 100 mL volumetric flask and dilute with 50% ethanol solution to the volume.

Trace Anions in Plasma Grade Water by Cap IC Using the ICW-3000 Online Water Purifier

2011-12-13T08:57:44.077

Trace Anions in Plasma Grade Water by Cap IC Using the ICW-3000 Online Water Purifier. Here we show trace anions in plasma grade deionized water by concentrating 200 uL of sample on a concentrator column. The ICW-3000 provides deionized water inline without introducing contamination from containers. Trace ion determinations in Ultra-Pure Water (UPW) are important analysis for the power and electronic industries because ionic contamination at µg/L and ng/L concentrations can cause corrosion of important process equipment resulting in unplanned and costly maintenance in both industries. Additionally, ionic contamination in the electronic industry causes poor yields and early end-of-life failures of important semiconductor and disk drive components. Trace ion determinations have been thoroughly discussed in application documents published from 1996 to 2009. However, detection limits, sample handling, and blank stability have all been improved by recent advances in Dionex ion chromatography (IC) technology, including capillary IC, the Dionex AS-AP autosampler, and the ICW-3000 Online Water Purifier.

Fast Analysis of Inorganic Anions in UK Municipal Drinking Water

2012-01-05T12:53:22.937

The recent introduction of IonPac AS18, 2x250 mm high capacity analytical columns provides new ways to achieve with faster separations and improved resolution of critical pairs. All analysts of interests in UK municipal drinking water were baseline resolved at flow rate of 0.40 mL/min. The run time was reduced from 15 min to 8 min with good baseline resolution. The fast analysis of common anions in municipal waters samples by using 250mm column emphasizes the fast sample runs and higher resolution possible with high capacity column. Additionally, it demonstrates the fast analysis combined with high capacity column.

Nimodipine Tablets Assay according to the Chinese Pharmacopoeia

2010-02-05T12:15:23.87

This method describes how to assay Nimodipine Tablets according to the Chinese Pharmacopoeia Preparing the Test Solution: Accurately weigh and powder 20 tablets. Dissolve an accurately weighed quantity of the powder, equivalent to about 10 mg Nimodipine, in the mobile phase in a 50 mL volumetric flask, ultrasonicate for 15 minutes, cool to room temperature, dilute with the mobile phase to volume, mix well, and centrifuge at 3000 rpm for 10 minutes. Transfer accurately 5 mL of the supernatant liquid to a 50 mL volumetric flask, dilute with the mobile phase to volume, and mix well. Preparing the Reference Solution: Dissolve a quantity of Nimodipine CRS, accurately weighed, in mobile phase, to produce a solution of 20 µg/mL.

Quantification of Erythromycin Metabolites with CAD

2011-04-20T12:33:10.547

The publication of the U.S. FDA guidelines in 2008 on drug metabolites in safety testing (MIST) requires that the relative quantitation of human metabolites be obtained as soon as feasible in the drug development process. The goal is to ensure that at least one of the animal models used is not only producing the same metabolites found in humans but that these metabolites are found in the same relative abundance. Identification of drug metabolites is typically accomplished using various LC-MS or LC-MS/MS approaches. However, metabolite quantification is often difficult to accomplish with MS techniques alone. In some cases the addition of UV detection is sufficient for metabolite quantification. However, this requires that both parent drug as well as its metabolites possess a sufficiently active chromophore. Unfortunately, this is not always the case. The Corona Charged Aerosol Detector (CAD) can detect any nonvolatile, and many semivolatile compounds, typically with low-ng sensitivity. Furthermore, as response is similar for all compounds and independent of chemical structure, it is ideal for measurement drugs and metabolites. Presented here and in the attached poster note are the results from two test cases used to evaluate the usefulness of charged aerosol detection for MIST: buspirone (which has a strong UV chromophore) and erythromycin (which has a weak UV chromophore). These drugs were analyzed directly and following incubation with human liver microsomes (drugs at ≤100 μM). The five major metabolites for buspirone and the four major metabolites for erythromycin were identified using an LTQ-Orbitrap MS and quantified by charged aerosol detection. The range, linearity, and sensitivity of this approach will be discussed as well as techniques for lower concentration levels. Charged aerosol detection is an important complementary technique to those already being employed in an industry capable of extending the range of in vitro drug metabolites that can be monitored during the drug development stage of testing. In this example of 100 µM erythromycin post incubation the mass balance recovery results was 97% by comparing the raw area of the pre and post incubation results on the CAD. An inverse gradient was applied in this system to remove any nebulization efficiency changes during the gradient. The UV traces also shown did not detect any of the drug metabolites as the concentration was too low for these compounds with very weak chromophores.

Anions in Brand C Bottled Water by Capillary IC

2010-11-04T16:55:12.423

Cap AS19 Brand C bottled water. Common anions are determined in a bottled water sample using the capillary ICS-5000 ion chromatograph system and IonPac AS19 column. Anions in the bottled water sample were separated with a gradient using electrolytically generated hydroxide eluent.

Water-Soluble Vitamins on Acclaim RSLC PolarAdvantage II (PA2) with TFA Mobile Phase Additive

2010-02-19T10:29:21.657

Water-soluble vitamins are a chemically heterogeneous group including acids, bases, zwitterions, and neutrals with different spectroscopic properties. The amounts in samples can vary from a few micrograms to hundreds of milligrams. Each matrix presents a unique set of interferences and sample preparation problems. The Acclaim PolarAdvantage II (PA2) features an amide embedded functionality in the stationary phase, and provides unique selectivity and aqueous compatibility, making it suitable to separating water-soluble vitamins. The use of the 2.2 µm Acclaim RSLC column in 2.1 mm i.d. format allows fast analysis time with reduced solvent consumption. The diode-array detector confirms the identity and purity of each peak. In this example, trifluoroacetic acid (TFA) is used to improve the retention time and peak shapes of thiamine and pyridoxine. As the result, the Acclaim RSLC PA2 column baseline separates eight common water-soluble vitamins using a "green" method (iso-propanol as the organic modifier) in 5 min. Note that citric acid and other minor components can interfere with ascorbic acid or pyridoxine, which requires that the pH of the mobile phase be carefully adjusted.

Piracetam Tablets Related Substances according to the Chinese Pharmacopoeia

2010-02-22T17:36:25.46

This application describes how to measure related substances in Piracetam tablets according to the Chinese Pharmacopoeia Preparation: Prepare a test solution of 0.5 mg of piracetam per ml and a reference solution of 5 µg of piracetam CRS per ml with the mobile phase

Anthocyanins and Anthocyanidins from Bilberry

2010-02-18T16:21:58.43

Bilberry is a rich source of anthocyanin pigments for which various health benefits have been claimed. There are up to 15 anthocyanin glycosides based on 5 anthocyanidin aglycones. Most of these can be resolved using Acclaim 120 C18.

Determination of inorganic anions in a municipal drinking water

2011-11-22T14:49:54.36

Common Inorganic anions in a municipal drinking water were determined using IonPac AS18 4um column. This column utilizes the smaller particle size packing material to provide good resolution while reducing analysis time. All analytes are detected by suppressed conductivity detection. The eluent is electrolytically generated by a capillary EG.

Anions and Select Organic Acids in Cranberry Juice by Capillary IC

2010-11-04T13:30:21.627

Cap AS19_Cranberry Juice This method demonstrates determination of anions and select organic acids in cranberry juice using capillary IC on IonPac AS19 capillary column and the ICS-5000 capillary system

RSLC Analysis of Steviol Glycosides in Stevia Leaf Extracts with Charged Aerosol Detection

2011-12-08T08:45:23.61

A Thermo Scientific Acclaim RSLC Polar Advantage II column with 2.2µm particle size and dimensions of 2.1 x 250 mm and a simple gradient from 95% DI water with 0.1% trifluoroacetic acid (TFA) to 60% aceteonitrile + 0.1%TFA in 9 minutes was performed. The total method time for the analysis was reduced by nearly a factor of three while increasing resolution of the Reb A by more than 20% by changing to the small particle size from 5µm particle size method (see attached). The LOQ is < 10ng on column with the RSLC Corona ultra RS method. This level of sensitivity is more than tenfold lower than the observed LOQ with UV at 210 nm for this particular analytical method.

Analysis of a bitter acids standard using automated on-line SPE-UHPLC

2011-09-21T01:53:12.953

The main compound group contributing to the typical bitter taste of beer is iso-α-acids, the so-called isohumulones. The substances are the isomerization products of α-acids originating from hop (latin humulus lupulus) addition during the brewing process. The isohumulones are generated during wort boiling. The predominant congeners are the following six iso-α-acids: trans-isocohumulone, trans-iso-humulone, trans-isoadhumulone, cis-isocohumulone, cis-isohumulone, and cis-isoadhumulone. The monitoring of the content of isohumulones during the brewing process is mandatory to guarantee high quality beverages with stable flavor. Traditional analysis steps involve manual sample preparation by liquid/liquid or solid phase extraction followed by RP-HPLC separation with UV-detection. The Thermo Scientific Dionex UltiMate 3000 x2 Dual LC system is applied for an on-line SPE-UHPLC method suitable for direct injection of beer sample. The automated enrichment was done on a SolEx HRP UHPLC compatible SPE column followed by separation on a Hypersil Gold 1.9 µm column with UV detection at 270 nm. With a total run time of the 10 minutes the method allows easy monitoring of iso-α-acid sum parameter and profile during the brewing process making it a valuable tool for every brewery.

Analysis of Tryptic Digest of a Protein using UV and Charged Aerosol Detection

2011-07-19T18:30:19.157

The efficiency of the tryptic digestion of a protein is typically measured using HPLC or UHPLC with UV detection at 214 nm. Presented here is a comparison of the use of charged aerosol detection (CAD) with inverse gradient and UV detection for monitoring digestion of bovine serum albuminby trypsin (from porcine pancreas). The protein solution was incubated at 360C for 21 hours in a vial on the autosampler. Nine aliquots of sample were analyzed over the course of the incubation. The UHPLC system was comprised of both a UV and a Corona ultra RS detector. During analysis the salt void was diverted from the Corona ultra RS using the diverter valve. The sensitivity of the two techniques were comparable. The CAD ultra RS was the only detector capable of measuring the early eluting amino acid residues and low molecular weight peptides. The results for 18 hour sample are shown here and discussed further in the attached document.

Determination of inorganic anions and organic acids in beverages using IonPac AS18 column

2011-11-28T13:29:55.733

IonPac AS18 column is designed for inorganic anion analysis. Here it shows with hydroxide gradient, the low molecule weight organic acids can be separated from 7 common inorganic anions. The eluent is electrolytically generated by capillary ICS-5000 EG.

Anions in Decaffeinated Coffee by Capillary IC on IonPac AS19

2010-10-29T15:23:41.453

Capillary AS19: Decaffeinated Coffee. Anions are determined by capillary IC using a gradient separation on IonPac AS19 capillary column.

AN245: Fast HPLC Analysis of Dyes in Foods and Beverages

2010-03-10T01:45:35.86

Dyes have many applications in the food and beverage industries, such as being used to make food more appealing, hide defects, or to strengthen consumer perception of the association between color and flavor. For example, lime flavor is associated with the color green and thus, lime soft drinks are often colored with green food dye. Despite the existence of many dyes, only a few have been approved for use in foods and beverages. Reversed-phase chromatography is an excellent technique for the analysis of dyes. Many dyes are hydrophobic, readily soluble in reversed-phase eluents, and have strong visible and UV absorbance properties. This application note (AN) demonstrates fast separation of 10 dyes in less than 5 min using an Acclaim® PA2 (3 ?m) column in a 3 × 75 mm format. The Acclaim PA2 column is ideal for resolving mixtures of compounds with a wide range of hydrophobicities, including very polar compounds. This method was used to determine the quantity of food dyes in six soft drinks and a gelatin dessert. The combination of an UltiMate® 3000 Rapid Separation LC (RSLC) system and an Acclaim PA2 column is suitable for the fast analysis of food and beverage samples that have both approved and illegal dyes.

Analysis of bitter acids in beer using automated on-line SPE-UHPLC

2011-09-21T01:05:51.173

Quantification of Erythromycin Metabolites with CAD

2011-03-23T07:15:09.327

The publication of the U.S. FDA guidelines in 2008 on drug metabolites in safety testing (MIST) requires that the relative quantitation of human metabolites be obtained as soon as feasible in the drug development process. The goal is to ensure that at least one of the animal models used is not only producing the same metabolites found in humans but that these metabolites are found in the same relative abundance. Identification of drug metabolites is typically accomplished using various LC-MS or LC-MS/MS approaches. However, metabolite quantification is often difficult to accomplish with MS techniques alone. In some cases the addition of UV detection is sufficient for metabolite quantification. However, this requires that both parent drug as well as its metabolites possess a sufficiently active chromophore. Unfortunately, this is not always the case. Charged aerosol detection can detect any nonvolatile, and many semivolatile compounds, typically with low-ng sensitivity. Furthermore, as response is similar for all compounds and independent of chemical structure, it is ideal for measurement drugs and metabolites. Presented here and in the attached poster note are the results from two test cases used to evaluate the usefulness of charged aerosol detection for MIST: buspirone (which has a strong UV chromophore) and erythromycin (which has a weak UV chromophore). These drugs were analyzed directly and following incubation with human liver microsomes (drugs at ≤100 μM). The five major metabolites for buspirone and the four major metabolites for erythromycin were identified using an LTQ-Orbitrap MS and quantified by charged aerosol detection. The range, linearity, and sensitivity of this approach will be discussed as well as techniques for lower concentration levels. Charged aerosol detection is an important complementary technique to those already being employed in an industry capable of extending the range of in vitro drug metabolites that can be monitored during the drug development stage of testing.

Fluconazole Tablets Assay according to the Chinese Pharmacopoeia

2010-03-31T01:17:40.063

This method describes how to assay Fluconazole Tablets according to the Chinese Pharmacopoeia Preparing the Test Solution: Weigh accurately and powder 10 tablets. Dissolve an accurately weighed quantity (equivalent to about 50 mg of Fluconazole) with the mobile phase in a 100 mL volumetric flask. Dilute to volume, mix well, and filter. Inject 20 µL of the filtrate. Preparing the Reference Solution: Dissolve an accurately weighed quantity of fluconazole CRS in the mobile phase to produce a reference solution of 0.5 mg of fluconazole CRS per mL.

Fast Analysis of Inorganic Anions in Berkeley Municipal Drinking Water

2012-01-05T10:45:16.313

The standard length 250 mm format of IonPac AS18 analytical column has high capacity resulting in good retention of fluoride from the void volume and good resolution of critical inorganic anion pairs. Samples are less likely to overload these columns, thereby allowing larger injections of more concentrated and higher ionic strength matrix samples without dilution. AS18 high capacity analytical columns provides new ways to achieve improved resolution of critical pairs with faster separations . In this study, all analysts of interests in Berkeley municipal drinking water were baseline resolved at flow rate of 0.40 mL/min. The run time was reduced from 15 min to 8 min with good baseline resolution. The fast analysis of common anions in municipal waters samples by using 250mm column emphasizes the fast sample runs and higher resolution possible with high capacity column.

Fast determination of inorganic anions in water using high pressure capillary ICS-5000

2011-11-28T15:55:18.36

Dionex capillary high pressure system of ICS-5000 can tolerate 5000 psi backpressure which facilitates the fast analysis by increasing the flow rate. In this work, 0.03 mL/min flow rate is utilized to separate common anions in less than 3 minutes using IonPac AS18 4um column. At this flow rate, about 2800 psi backpressure was generated.

AN127: Monitoring Monoclonal Antibody Heterogeneity by Cation-Exchange Chromatography

2010-03-04T10:17:47.627

During the development and production of therapeutic proteins, characterization of structural variants is a critical Challenge. C-terminal processing of lysine residues on the heavy chain of monoclonal antibodies (MAbs) is a common structural variation that demands careful analysis. As a result of this processing C-terminal lysine or arginine residueas are often absent in proteins isolated form mammalian cell cultures, even though their presence may be expected on the basis of the gene sequence. This discrepancy, which is common in plasma-derived proteins, results from the activity of one or more basic carboxypeptidases. Incomplete protein processing results in charge heterogeneity which is readily identified by cation-exchange chromatography on the Dionex ProPac WCX-10, a weak cation-exchange column. This application note describes a method for analyzing a humanized IgG1 MAb for C-terminal lysine variants. These variants are baseline resolved from the native antibody using the ProPac WCX-10 column and a 4-morpholineethanesulfonic acid (MES)-mobile phase. Other acidic and basic variants are also better resolved than has been observed with traditional phosphate-based mobile phases buffered at pH 7, enabling detection of additional MAb variants, each with heavy chain C-terminal lysine heterogeneity.

Analysis of Pluronic F-68 with Charged Aerosol Detection (CAD)

2010-10-13T13:19:08.923

Pluronic® F68 is a non-ionic block copolymer of ethylene and propylene oxide. It is used in the pharmaceutical industry for cell culture work as an anti-foaming agent and stabilizer. This analysis looks at the compound over three orders of magnitude using size exclusion chromatography and Corona CAD. A full pdf report is attached.

Triclosan in Toothpaste on Acclaim RSLC C8

2011-01-26T09:40:07.547

Triclosan, 5-chloro-2-(2,4-dichlorophenoxy)phenol, is an antibacterial agent widely used in personal care products. In this example, it was found that methanol provides better selectivity than acetonitrile. The higher viscosity/operating pressure can be mitigated by using an elevated temperature. The separation took less than 3 minutes, and was performed on UltiMate 3000 RSLC system.

Deionized Water Blank with ICW-3000 Online Purifier Installed for Eluent and ASAP

2011-12-12T21:20:02.47

Deionized Water Blank with ICW-3000 Online Purifier Installed for Eluent and ASAP. Trace ion determinations in Ultra-Pure Water (UPW) are important analysis for the electronic industry because ionic contamination at µg/L and ng/L concentrations can cause corrosion of important process equipment resulting in unplanned and costly maintenance. Additionally, ionic contamination in the electronic industry causes poor yields and early end-of-life failures of important semiconductor and disk drive components. Trace ion determinations have been thoroughly discussed in application documents published from 1996 to 2009. However, detection limits, sample handling, and blank stability have all been improved by recent advances in Dionex ion chromatography (IC) technology, including capillary IC, the Dionex AS-AP autosampler, and the ICW-3000 Online Water Purifier.

Anions and Organic Acids in Apple Juice by High Pressure Capillary IC

2011-12-11T16:24:38.563

Anions and Organic Acids in Apple Juice by High Pressure Capillary IC. Determinations of organic acids in beverages are important to the beverage industry because these acidulants and flavoring agents maintain beverage freshness, minimize microbiological growth, and add a characteristic flavor. Additionally, analysis is required to meet product labeling requirements in 21 CFR part 101.1 High Pressure Capillary Reagent-Free™ ion chromatography (RFIC™) is the latest advancement in ion chromatography instrumentation. Typically with an RFIC system, the system pressure is limited to <3000 psi because of the limitations of materials in the RFIC accessories. Now with the upgrade to high pressure, the ICS-5000 IC capillary system can operate at system pressures <5000 psi. This advance in technology allows 2x to 3x the µL/min flow rates with all the same advantages as standard pressure capillary IC, resulting in low consumption of water (30 to 40 mL/d of water) and low waste generation. In capillary IC, the system can remain on without loss in resources, i.e., capillary IC is always on and ready for analysis. These advantages result in: 1. Greater ease-of-use, 2. Longer eluent generator cartridge life, 3. Lower cost of ownership. Additionally, the increase in mass sensitivity, comparable results are achieved as with standard bore system using a sample injection of only 0.4 µL. In this study, inorganic anions and organic acids from a diluted apple juice sample are separated by anion-exchange chromatography on a capillary size Thermo Scientific Dionex IonSwift MAX-100 monolith IC column. The IonSwift MAX-100 column is designed with a monolith backbone and optimized with Dionex IonPac AS11 anion-exchange chemistry. This column was selected for these high pressure cap IC experiments because of the high efficiency and high flow rate characteristics.

Carbohydrates in Dietary Fiber Using Capillary HPAE-IPAD

2010-11-14T12:53:24.28

Cap_PA20_Dietary Fiber. This method shows the separation of expected carbohydrates in dietary fiber sample using a capillary CarboPac PA20 column using electrolytically-generated eluents and a capillary ICS-5000 IC system.

Determination of Inorganic Cations in UK Municipal Drinking Water

2011-08-08T15:42:50.437

Inorganic cations are determined in UK municipal drinking water by capillary ICS 5000 using IonPac CS16 column

Piracetam Tablets Assay according to the Chinese Pharmacopoeia

2010-02-22T13:05:18.727

This application describes the assay of Piracetam tablets according to the Chinese Pharmacopoeia. Test Preparation: Weigh accurately and powder 20 tablets. Dissolve an accurately weighed quantity of powder equivalent to 0.1 g of piracetam with mobile phase in a 100 ml volumetric flask, dilute to volume, mix well, and filter. Transfer accurately 5 ml of the filtrate to a 50 ml volumetric flask, dilute with mobile phase to volume, and mix well. Reference Preparation: Dissolve a sufficient quantity, accurately weighed, and dilute with mobile phase to produce a solution of 0.1 mg of piracetam per ml.

Fast Determination of Inorganic Cations in Brewed Coffee

2011-11-30T14:25:34.36

One of the important applications of ion chromatography is to determine inorganic cations in different beverages. Here shows an example of separating inorganic cations in brewed coffee in less than 7 minutes using capillary ICS-5000 and IonPac CS16 column. The capillary format of IC system offeres reduced eluent consumption and reduced operating costs. This appliation was performed at 0.03 mL/min flow rate with an isocratic MSA eluent electrolytically generated by ICS-5000 EG. At this flow rate, about 2100 psi backpressure was generated.

Separation of Microcystins on Acclaim RSLC C18

2010-02-15T14:38:00.257

Microcystins are highly toxic peptides produced by blue-green algae and can contaminate sources of municipal drinking water. While the standard method takes about an hour to run, a straightforward conversion to rapid separation LC (RSLC) using the Acclaim RSLC 120 C18 2.2 µm column shortens the analysis time to six minutes. There are many microcystin variants according to the amino acid composition, with RR, YR, and LR being the most common.

Assay for Water-Soluble Vitamins in Vitamin Tablets

2010-02-10T12:15:50.333

Vitamin supplement tablets are complex formulations with many ingredients. Some vitamins are strongly hydrophilic, so the column needs to operate in 100% aqueous buffer to gain sufficient retention to resolve them from the matrix. The Acclaim® PA can do this reliably whereas a hydrophobic C18 column would likely suffer dewetting. The multiple wavelength capability of the diode array detector provides primary wavelengths for quantitification and alternate wavelengths for confirmation.

Indometacin Suppositories Assay according to the Chinese Pharmacopoeia

2010-02-05T16:00:39.65

This method describes how to assay Indometacin Suppositories according to the Chinese Pharmacopoeia Preparing the Test Solution: Weigh accurately 10 suppositories, cut carefully and mix well. To a quantity, equivalent to about 25 mg of Indometacin, accurately weighed, add a quantity of ethanol to a 50 mL volumetric flask, heat on water bath to dissolve Indometacin, cool to room temperature, and dilute with ethanol to the volume, mix well, and filter. Measure accurately 5 mL of the successive filtrate in a 25 mL volumetric flask, dilute with 50% ethanol solution to the volume, and mix well. Preparing the Reference Solution Weigh accurately 25 mg of Indometacin CRS to a 50 mL volumetric flask, add a quantity of ethanol, shake to dissolve Indometacin, dilute with ethanol to volume, mix well. Measure accurately a quantity and dilute with 50% ethanol solution to produce the reference solution of 0.1 mg/mL.

Nitrophenols

2010-02-17T09:41:11.5

Nitrophenols are highly toxic pollutants. Trinitrophenol, also known as picric acid, is an explosive. These compounds are known for their variable retention and poor peak shape by conventional RP-HPLC. The unique Acclaim Mixed-Mode WAX-1 column gives reliable, sharp peaks.

Fast Separations of Inorganic Anions in Sunnyvale Municipal Drinking Water Samples

2012-01-04T16:54:29.827

Inorganic anions which exist in Sunnyvale municipal environmental water samples are baseline resolved within 4 minutes by using Thermo Scientific Dionex IonPac AS18-Fast analytical column. The “Fast” (150 mm) version of the 2 mm column provides advantages to determination of inorganic anions by providing improved resolution and fast run time and excellent value to customers by high throughput, fast separations and high resolution.

Chiral Analysis of Underivatized Amino Acids at >0.1 w/w% D in L with Charged Aerosol Detection

2011-06-10T06:56:12.517

The use universal detection of non-volatile compounds with the Corona Charged Aerosol Detector (CAD) offers large dynamic range, sensitivity, and uniformity of response which are important in the analysis amino acid chirality. The work outlined in this application uses of the Chirobiotic T (teicoplamin) chiral stationary phase for the analysis of amino acid enantiomers. Using the direct detection of amino acid enantiomers with charged aerosol detection can provide limit of detections of 0.04 w/w% with improved accuracy and precision without derivatization or extensive sample preparation.

Fast Determinations of Inorganic Anions in City B Wastewater Using Carbonate Eluents

2010-10-26T15:20:52.72

AS22 FAST_City B WASTEWATER. This method updates inorganic determinations in wastewater using IonPac AS22 Fast column with carbonate eluents. All seven anions were determined in 5 min.

Fast Inorganic Anions in City A Municipal Wastewater Using Carbonate Eluents

2010-10-26T14:32:08.78

AS22 Fast_City A Wastewater This method updates inorganic anion determinations using the AS22 Fast carbonate column. All seven anions are determined within 5 min.

Rapid Determination of Acetylcholine in Microdialysis Samples

2011-10-10T08:10:58.923

The importance of acetylcholine (ACh) as a neurotransmitter in the nervous system was realized over 80 years ago. Only recently have sensitive methods been developed for sampling and quantifying Ach levels in the central nervous system of awake animals to offer insights about the neurophysiological activity of ACh in a variety of systems. One such approach involves the use of in vivo microdialysis and subsequent quantification of ACh using high-performance liquid chromatography with electrochemical detection (HPLC-ECD). The current method uses a short HPLC column and a post-column solid phase reactor with sensitive electrochemical detection for the separation and measurement of Choline and Acetylcholine at low femtomole levels.

Separation of Fat-Soluble Vitamins on Acclaim RSLC PolarAdvantage II (PA2)

2010-02-19T18:07:35.73

Vitamins D2 and D3 are frequently difficult to separate from each other and from Vitamin E. The Acclaim PolarAdvantage II has an embedded amide group that provides a unique selectivity for some separations. To optimize that selectivity, both the temperature and alcohol content were varied. The Rapid Separation LC (RSLC) format allows fast separations with good resolution, with only a moderate increase in pressure. The diode-array detector confirms the identity and purity of each peak.

Determination of Inorganic Cations in Wine

2011-08-08T16:02:05.063

Inorganic cations in wine are determined by capillary ICS 5000 using IonPac CS16 column.

Lysozyme Protein Digest Separation on Acclaim C18

2010-03-02T09:10:40.09

Mapping tryptic protein digests can produce highly complex chromatograms where every peak counts. The Acclaim 3 μm 2.0 x 100 mm columns yield superior peak capacity and resolution. Using techniques developed for Rapid Separation LC (RSLC) columns, these columns are physically rugged and rated to 800 bar. The 120 C18 chemistry has low silanol activity and high bonding density that produce sharp peaks for small, basic peptides.

Anions in Italian Municipal Wastewater Using a Gradient Separation on IonPac AS19

2010-11-21T19:36:57.39

AS19 Analytical_Italy wastewater. Inorganic anions were determined in an Italian municipal wastewater sample on an ICS-5000 Reagent-Free Ion Chromatography (RFIC) system. The anions were separated on a 2-mm IonPac AS19 anion-exchange column using a gradient KOH eluent electrolytically-generated in line.

Determination of Inorganic Cations in Municipal Drinking Water of City Sunnyvale, CA by IonPac CS12A using Capillary ICS5000

2011-05-04T10:21:38.297

Inorganic cations in municipal drinking water were determined on a capillary ICS-5000 Reagent-Free Ion Chromatography (RFIC) system. The cations were separated on a IonPac CS12A caiton-exchange column using an electrolytically generated MSA eluent.

Analysis of Fluorodeoxyglucose and contaminant Chlorodeoxyglucose

2011-07-20T07:36:56.983

2-Deoxy-2-[18F]fluoro-D-glucose (FDG) is the most widely used radiopharmaceutical for positron emission tomography (PET). It used for the study and diagnosis of a number of disorders. In addition, it is an important tool in neuroscience, and drug research and development. The synthesis of FDG involves nucleophilic displacement and hydrolysis. A contaminant resulting from both processes is 2-Deoxy-2-chloro-D-glucose (ClDG). Limits for ClDG have been set by USP, CMC, and EP and soon by FDA. Measurement of FDG / ClDG uses high performance anion exchange chromatography in combination with pulsed amperometric detection (PAD). Due to the improved sensitivity and selectivity of PAD, sample preparation procedures are not required. HPAC-PAD is well established, sensitive, and selective method for determining carbohydrates. The separation is accomplished on a PA20 column using an alkaline MP (50 mM NaOH).

Simultaneous Separation of Cetirizine and Chloride in Zyrtec® Tablet on Acclaim Trinity P1

2010-02-22T08:54:28.307

Many active pharmaceutical ingredients (APIs) are formulated in salt forms. It is often desired to have mass-balance analysis of the API and its counterion. The Acclaim Trinity P1 is uniquely designed for such applications. This column is based on Nanopolymer Silica Hybrid (NSH) technology and provides anion-exchange, cation-exchange, and reversedphase retention mechanisms at the same time. Zyrtec® is a third-generation antihistamine used to relieve allergic symptoms and is formulated as a hydrogen chloride salt. Usually analysis for the API and its counterion have to be done in two different essays - API by HPLC and counterion by ion chromatography (IC), which require different columns and different instruments. Because neither wide linear range nor low detection limits for chloride are required, an evaporative light scattering detector (ELSD) provides sufficient performance. The Acclaim Trinity P1 column in combination with ELSD provides simultaneous determination of the API (cetirizine) and its counterion (chloride) with excellent retention, resolution, and peak shape, under a simple isocratic condition.

Determination of Inorganic Cations in Vitamin Drink

2011-08-08T15:55:32.97

Inorganic cations in vitamin drinks are determined by capillary ICS 5000 using IonPac CS16 column

Fast Analysis of Diclofenac and its Counterions

2010-02-15T08:06:45.893

This application shows the separation of an active pharmaceutical ingredient (Dicolfenac) with counterions. It uses the Acclaim Trinity P1 column, the UltiMate 3000 RSLC system, and the Corona ultra charged aerosol detector (CAD). This application also shows the results from a UV detector - this demonstrates the inability of UV detectors to measure analytes which do not contain a chromophore, and highlights a key strength of the Corona ultra -it's ability to detect all non-volatile (and many semi-volatile) analytes.

AN198: Determination of Urea and Allantoin in Cosmetics Using the Acclaim Mixed-Mode HILIC Column

2010-02-15T16:19:31.063

In this application note, the chromatographic behavior of highly polar compounds on the Acclaim Mixed-Mode HILIC column is investigated, using allantoin and urea as test compounds. The influence of different sample diluents, and different concentrations and pH values of the buffer in the mobile phases on HILIC, is discussed. After method optimization, the concentrations of allantoin and urea in cosmetic products is determined.

Determinatin of Inorganic Cations in Diet Coke using IonPac CS16 Column

2011-08-08T14:23:40.267

Inorganic cations in diet coke drink is determined by capillary ICS 5000 using Ionpac CS16 column.

Fast Determination of Anions in Fresh Coconut Juice Using Carbonate Eluents

2010-10-26T16:53:30.017

AS22 FAST_Brand A Fresh Coconut Juice. This method demonstrates fast determination of common anions in fresh coconut juice on IonPac AS22 Fast using carbonate eluents within 6 min

Fast Determination of Anions in England Municipal Drinking Water

2011-06-22T10:32:50.157

Inorganic anions in a UK municipal drinking water sample was analyzed by ion chromatography using AS18 Fast column.

Determination of Cations in Drinking Water by Capillary IC

2011-06-22T10:09:05.36

Determination of inorganic cations in drinking water is an important application of ion chromatography. Here is an example of analysis of common cations in a municipal drinking water using capillary IC and IonPac CS16 column.

Determination of Anions in an Artificial Volcanic Gas Condensate Sample on 2 mm IonPac AS25 Column

2011-05-08T17:16:40.11

Determination of Anions in an Artificial Volcanic Gas Condensate Sample on 2 mm IonPac AS25 Column. This sample simulates a volcanic gas condensate sample containing 100 mg/L carbonate, 10 mg/L sulfate and ppb to ppm concentrations of halides, sulfite, thiocyanate, and thiosulfate.

Cation Determinations in Sunnyvale Wastewater by Capillary IC on IonPac CS12A Column

2011-05-08T16:09:35.233

Cation Determinations in Sunnyvale Wastewater by Capillary IC on IonPac CS12A Column. This application demonstrates fast separations of cations in a municipal wastewater sample.

Counter Anion Determinations in Fexofenadine HCl Tablet by Capillary IC

2011-04-14T14:15:15.61

Counter ion determinations in the pharmaceuticals provide important mass balance, contamination, and formulation information during early drug development through to the mature pharmaceutical product. Precise, accurate, and reproducible analytical methods are important to providing a reliable product, as such, IC is the method of choice. In this application, the counter anion, chloride, is determined in a Fexofenadine HCl tablet using anion-exchange chromatography on IonPac AS19 capillary column using an ICS-5000 capillary IC system.

Fast Determination of Common Inorganic Anions in Water

2011-11-30T10:15:49.327

One of the approaches to decrease the analysis time is to increase the flow rate. However, it is limited by the maximum pressure tolerated by the IC system. Sometimes, the fast analysis is achived by sacrificing the resolution. In this work, it is shown that common inorganic anions in water can be separated in less than 3 minutes without compromising the resolution. This achievement is facilitated by using high pressure capillary ICS-5000 system and IonPac AS18 column packed with 4 um particles. These smaller particles greatly enhance the efficiency of the column. At 0.03 mL/min flow rate used in this experiment, about 2800 psi backpressure was generated which was below the pressure limit 5000 psi of high pressure capillary IC system.

Ultrafast Analysis of Fat Soluble Vitamins by Parallel UHPLC

2010-02-12T11:01:24.017

This application separates 6 fat soluble vitamins in less than 4 minutes using an UltiMate 3000 RSLC system that is configured in parallel mode. This configuration can run 2 different applications at the same time for increased throughput and reduced cost of investment. A second application for the analysis of water soluble vitamins by parallel UHPLC can be accessed in the weblinks section

AN 220: Determination of Inorganic Anion Impurities in a Water-Insoluble Pharmaceutical by Ion Chromatography with Suppressed Conductivity Detection

2010-04-23T05:53:14.483

Pharmaceutical impurities are categorized as organic, inorganic, or residual solvents. Inorganic impurities that may be derived from the manufacturing process of bulk drugs include reagents, catalysts, ligands, heavy metals, and other materials. While the presence of many inorganic impurities at low concentrations have few toxicological consequences, significant variation in the impurity levels from batch-to-batch can indicate that the manufacturing process of the drug product is not adequately controlled. In most cases, these impurities should be removed or at least minimized in the final product. Therefore, the identification, quantification, and control of impurities are important during drug development in the pharmaceutical industry. Ion chromatography (IC) with suppressed conductivity detection is a well-established technique for the determination of inorganic and organic ions in pharmaceuticals. For the determination of anions, a hydroxide eluent is commonly used. Hydroxide is suppressed to water, which provides exceptionally low background conductivity and baseline noise and, therefore, very low detection limits. In this Application Note (AN), we demonstrate the development of an IC method for the determination of anionic impurities in a proprietary water-insoluble pharmaceutical.

Indometacin Capsules Assay according to the Chinese Pharmacopoeia

2010-02-05T14:56:28.317

This method describes how to assay Indometacin Capsules according to the Chinese Pharmacopoeia Preparing the Test Solution: Weigh accurately 20 capsules, remove the content. To a quantity, equivalent to about 50 mg of Indometacin, add a quantity of ethanol to a 100 mL volumetric flask, shake to dissolve Indometacin, dilute with ethanol to volume, mix well, and filter. Measure 5 mL of the successive filtrate in a 25 mL volumetric flask, dilute with 50% ethanol solution to volume, and mix well. Preparing the Reference Solution: Weigh accurately 25 mg of Indometacin CRS to a 50 mL volumetric flask, add a quantity of ethanol, shake to dissolve Indometacin, dilute with ethanol to volume, mix well. Measure accurately a quantity and dilute with 50% ethanol solution to produce the reference solution of 0.1 mg/mL.

Peptide Map of Beta Casein on Acclaim PolarAdvantage II (PA2)

2010-02-18T13:35:55.97

Mapping tryptic protein digests can produce highly complex chromatograms where every peak counts. The Acclaim 3 μm 3.0 × 250 mm columns yield superior peak capacity and resolution. Using techniques developed for Rapid Separation LC (RSLC) columns, these columns are physically rugged and rated to 800 bar. The PolarAdvantage II chemistry exhibits excellent chemical stability in acidic conditions, and has omplementary selectivity compared to C18. Some peptides, especially phosphopeptides, are sensitive to metal contamination. A small amount of pyrophosphate (0.1 mM) in the mobile phase suppresses metal effects without affecting UV detection.

Analysis of Albumin with Charged Aerosol Detection Demonstrating Consistent Response Independent of MW

2011-10-07T10:50:42.483

Bovine Serum Albumin (BSA) is a serum protein that has a number of practical uses. It is used by biochemists as a cell culture nutrient; to stabilize enzymes used for restriction digests of DNA; in ELISA-based applications; and as a standard for protein quantification assays. It is a well characterized protein with a molecular weight typically ranging from 66,120 and 66,420 Daltons, consisting of 583 amino acid residues. The data presented here show that a) proteins can be measured using the Corona Charged Aerosol Detector (CAD) and b) that the same mass of different analytes gives similar response by CAD, independent of MW. BSA was resolved using a simple acetonitrile/water + 0.1% TFA gradient and a monolith reversed-phase Proswift column. BSA response by traditional UV approaches at 210 and 276 nm was compared to that obtained by CAD. The CAD was able to detect BSA with slightly improved sensitivity over the UV maximum at 276 nm (signal to noise of 920/1 and 840/1 for the CAD and UV @276nm, respectively). The additional benefit with the CAD is that the response of any non-volatile analyte is independent of structure or MW. The attachment shows data comparing the response for BSA (using conditions above) to that of a small MW API, Ketoprofen. Although the same mobile phase gradient and analyte mass (on column) were used, the assay required a different column in order to retain ketoprofen. Results show the universal response of the CAD with a 1.2/1 area difference for the equal mass on column for the API to the protein. The same ratio was ~ 68.7/1 by UV (276nm). This simple monolith / CAD approach has the potential for fast protein characterization and quantification.

Fast Determination of Anions in Bottled Water

2011-07-08T14:17:19.407

Inorganic anions in mg/L concentrations in bottled water sample were seperated using a 2 x 150 mm, IonPac AS18-Fast anion-exchange column designed for fast separation using electrolyticallly generated hydroxide eluents.

Budesonide and Related Substances

2010-02-10T14:01:27.167

Budesonide is a highly effective steroidal antihistamine decongestant, and is available as a mixture of two epimers. The safety of budenoside based pharmaceuticals depends on careful monitoring of impurities associated with the epimers. The related substances are decomposition products and synthetic byproducts. The Acclaim 300 C18 column is a direct replacement for the column in the reference method.

AN 184: Determination of Trace Concentrations of Chlorite, Bromate, and Chlorate in Bottled Natural Mineral Waters

2010-02-22T17:00:04.28

In this application, we compare the IonPac AS19 using an electrolytically generated hydroxide eluent to the IonPac AS23 column using an electrolytically generated carbonate/bicarbonate eluent for the determination of chlorite, bromate, and chlorate in natural mineral waters. We compare the linearity, method detection limits, precisions, and recovery for three mineral waters obtained from three European countries to determine whether these columns have the sensitivity required to meet current EPA and EU requirements.

Anions and Citrate in a Sports Beverage by High Pressure Capillary IC

2011-12-11T19:31:35.203

Anions and Citrate in a Sports Beverage by High Pressure Capillary IC. High Pressure Capillary Reagent-Free™ ion chromatography (RFIC™) is the latest advancement in ion chromatography instrumentation. Typically with an RFIC system, the system pressure is limited to <3000 psi because of the limitations of materials in the RFIC accessories. Now with the upgrade to high pressure, the ICS-5000 IC capillary system can operate at system pressures <5000 psi. This advance in technology allows 2x to 3x the µL/min flow rates with all the same advantages as standard pressure capillary IC, resulting in low consumption of water (30 to 40 mL/d of water) and low waste generation. In capillary IC, the system can remain on without loss in resources, i.e., capillary IC is always on and ready for analysis. These advantages result in: 1. Greater ease-of-use, 2. Longer eluent generator cartridge life, 3. Lower cost of ownership. Additionally, the increase in mass sensitivity, comparable results are achieved as with standard bore system using a sample injection of only 0.4 µL. In this study, inorganic anions and organic acids from a diluted low carbohydrate sports beverage sample are separated by anion-exchange chromatography on a capillary size Thermo Scientific Dionex IonSwift MAX-100 monolith IC column. The IonSwift MAX-100 column is designed with a monolith backbone and optimized with Dionex IonPac AS11 anion-exchange chemistry. This column was selected for these high pressure cap IC experiments because of the high efficiency and high flow rate characteristics.

AN232: Determination of Anthraquinones and Stilbenes in Giant Knotweed Rhizome by HPLC with UV Detection

2010-02-16T14:24:11.303

Giant knotweed rhizome, the dried rhizome and root of Polygonum cuspidatum Sieb. et Zucc. is a common medicinal plant in China. Chinese Pharmacopeia Edition 2005 regulates its use as an herbal medicine. It is used with the belief that it cures angiocardiopathy, skin inflammations, liver diseases, reduces fever, and relieves arthritis pain etc. There are many compounds that are considered active components in giant knotweed rhizome, including anthraquinones. This application note describes an efficient HPLC method that in a single injection determines the eight main active components of giant knotweed rhizome: anthraglycoside A, anthraglycoside B, emodin, physcion, rhein, chrysophanol, resveratrol, and polydatin. Samples were extracted using ultrasonic extraction and the ASE® 200 Accelerated Solvent Extractor respectively, with satisfactory results obtained for both extraction methods.

AN 213: Determination of Polycyclic Aromatic Hydrocarbons (PAHs) in Tap Water Using On-Line Solid-Phase Extraction Followed by HPLC with UV and Fluorescence Detections

2010-02-16T19:07:00.313

This application note details an online SPE method followed by HPLC with fluorescence and UV detections on the UltiMate 3000 ×2 Dual HPLC system for determining the 16 PAHs specified in the US EPA Priority Pollutants List at the concentrations required by world regulatory agencies. Polycyclic aromatic hydrocarbons (PAHs) from water samples are trapped on the Acclaim Polar Advantage II (PA2) column, and then separated on a Supelcosil™ LC-PAH column. This automated method is a cost-effective and accurate way to determine PAHs in drinking water samples.

UHPLC Analysis of Polyaromatic Hydrocarbons using Fluorescence Detection

2010-07-19T08:14:35.843

This application demonstrates the analysis of 17 polyaromatic hydrocarbons (PAHs) in less than 7 minutes. The standard was prepared according to procedures defined by the EPA. This application is ideal for the new UHPLC+ UltiMate 3000 Standard System. The maximum back pressure for the method is less than 540 bar - well within the maximum pressure limit for the system of 620 bar. Finally, the application requires that the excitation and emission wavelengths are switched during the run. The timetable for this can be seen in an attachment for this application.

AN 109: Rapid HPLC Separation of Multiclass Antibiotics in Food and Water

2010-07-30T14:03:23.28

This application brief demonstrates a reproducible Rapid Separation Liquid Chromatography (RSLC) method for the separation of polyketide (tetracycline and oxytetracycline), macrolide (tylosin), phenicol (chloramphenicol), nitrofuran (nitrofurantoin), and sulfonamide (sulfathiazole) classes of antibiotics with an MS-compatible mobile phase.

Fast Anion Determinations in Bottled Water Using Carbonate Eluents

2010-10-26T16:47:30.61

AS22 FAST_Brand A bottled water. This method demonstrates fast determinations of common anions in a bottled water sample within 5 min.

Analysis of OTC Milk Thistle Extract by HPLC-CAD

2011-09-19T11:25:10.063

This example shows how to improve a standard method for determination of silymarins in milk thistle fruit and powdered extracts, Institute for Nutraceutical Advancement (INA) Method 115.00, by employing a higher efficiency Acclaim RSLC 120 C18 2.2 um column in conjunction with a universal detector, the Corona Charged Aerosol Detector (CAD), that provides more uniform response for all nonvolatile analytes than does a UV absorbance detector. A milk thistle plant native to Mediterranean Europe, Silybum marianium, has long been used as an herbal remedy to promote liver health. The seeds, root and milky sap of the milk thistle contain an antioxidant flavonolignan complex known as the silymarin group. Commercial preparations containing an extract from the milk thistle, standardized to contain a stated amount of silymarin, are now widely available as a dietary supplement, or nutraceutical.

Fast Determination of Inorganic Anions in City A Drinking Water Using Carbonate Eluents

2010-10-26T14:56:42.233

AS22 Fast_City A Drinking Water This method updates inorganic anion determinations in drinking water using carbonate eluents. All seven inorganic anions are determined within 5 min.

Counter Cation in a Atoravastatin calcium tablet by Capillary IC on IonPac CS12A Column

2011-05-08T15:37:22.327

Counter Cation in a Atoravastatin calcium tablet by Capillary IC on IonPac CS12A Column. Counter ion determinations are important to the pharmacy drug development, discovery, and production.

Benzalkonium in Spray Disinfectant on the Acclaim Surfactant Column

2010-02-18T16:37:58.087

The Acclaim Surfactant column provides superior performance for the analysis of benzalkonium-type disinfectants. Since the method here uses evaporative light scattering detection, acetonitrile may be replaced by acetone, which is more available, less expensive, and less toxic. Acetone has only slightly higher viscosity than acetonitrile, and similar selectivity for this application. With the use of a 3 mm i.d. column, the mobile phase consumption can be reduced by 55% compared to the 4.6 mm i.d. column format.

Fast Determination of Anions in a Young Coconut Beverage Using Carbonate Eluents

2010-10-28T14:39:32.017

AS22 Fast:Brand A Young Coconut Beverage

Carbohydrate Determinations in a Ketchup Sample Using Capillary HPAE-PAD

2010-11-14T14:23:40.5

Cap IC_PA20_ketchup. Monosaccharides were determined in a ketchup (catsup) sample using capillary HPAE-PAD on a capillary CarboPac PA20 column and ICS-5000 system.

Counter Cation Determinations in Naxproxen sodium by Capillary IC

2011-04-14T14:15:55.22

Counter ion determinations in the pharmaceuticals provide important mass balance, contamination, and formulation information during early drug development through to the mature pharmaceutical product. Precise, accurate, and reproducible analytical methods are important to providing a reliable product, as such, IC is the method of choice. In this application, the counter cation, sodium, is determined in a Naproxen sodium tablet using cation-exchange chromatography on IonPac CS12A capillary column using an ICS-5000 capillary IC system.

Chlorophyll on Acclaim RSLC PolarAdvantage II (PA2)

2010-02-15T15:58:53.537

Chlorophyll is a green pigment found in most plants, algae, and cyanobacteria. Chlorophyll is vital for photosynthesis, which allows plants to obtain energy from light. Chlorophyll a and chlorophyll b are present in plants. Because of their high hydrophobicity, chlorophyll a and chlorophyll b can be analyzed by HPLC using a reversed-phase column under normal-phase condition (high organic solvent). The Acclaim RSLC PA2 stationary phase is based on bonding silyl ligands containing a hydrophobic alkyl chain with a polar amide-embedded group, onto high-purity, spherical, porous, 2.2 micron silica particles. As the result, a 2.1 x 50 mm RSLC PA2 column offers suitable selectivity for high-speed, baseline separation of chlorophylls in spinach leaf. The small amount of buffer ensures good reproducibility and symmetrical peaks. It was observed that in this application, acetonitrile is the weak solvent for the polar pigments, and methanol is the strong solvent.

Fast Analysis of Inorganic Anions in Berkeley Municipal Water Samples

2012-01-04T17:57:37.327

Inorganic anions existing in municipal water samples are baseline resolved within 4 minutes by using Thermo Scientific Dionex IonPac AS18-Fast analytical column. The applications was applied to Berkeley Municipal water samples and five anions in the sample were baseline resolved within 4 min on the “Fast” (150 mm) version of the 2 mm column, emphasizing the fast sample runs possible with these length columns.

AN 195: Determination of Verapamil Hydrochloride Purity Using the Acclaim PA Column

2010-02-18T18:00:17.463

In this application, we describe a new method for the fast determination of verapamil hydrochloride and verapamil-related compounds A, B, and D, using a polar-embedded reversed-phase column, the Acclaim® PolarAdvantage (PA). The new method requires only about half the time of the proposed USP monograph method, provides significant eluent and therefore cost savings, and meets the resolution requirement.

Simultaneous API and Counter Ion from Pain Relief Tablet

2011-04-19T12:39:45.47

In this work, the method development, optimization, and validation of a system looking at the simultaneous analysis of an API and counter-ion in a complex dissolution media are discussed. The system uses a 10 port 2 position valve with tandem C18 trap columns setup with the Trinity P1 column for separation and analysis of sodium by Corona Charged Aerosol Detection (CAD) and Naproxen by UV at 254nm. This optimization is important as it speeds up the method from one hour (to elute the Tween 80 without affecting the buffer solubility and then reconditioning of the column) to only 15 minutes. It also prevents the overloading on both the Trinity column and the CAD. The detailed results and validation of this method can be found in the attached links and documents.

Anions in a diet cola beverage

2011-04-12T17:09:50.703

Inorganic anions in a diet cola beverage were determined on a ICS-5000 capillary Reagent-Free Ion Chromatography (RFIC) system. The anions were separated on a capillary IonPac AS19 anion-exchange column using an electrolytically generated gradient KOH eluent.

Determination of Inorganic Cations in Sports Drink

2011-08-08T15:32:31.673

Inorganic cations are determined in a sports drink by capillary ICS 5000 using IonPac CS16 column

Determination of Lot-Lot Variability of Polysorbate 80 (Tween 80) with Charged Aerosol Detection

2010-10-19T07:06:48.877

The use of polysorbate (Tween) 20, 60, and 80 is widespread through out the food industry as an emulsifier in things such as ice cream and milk as well as in a variety of other foods and commonly used products. The pharmaceutical industry also relies heavily on the use of these compounds to solubilise and stabilise a variety of drugs along with being part of some cleaning procedures. The characterization of polysorbate is challenging because these are polydispered heterogeneous mixtures of non-UV active large molecules. The method shown here along with the additional work in the attached pdf looks at HPLC and UHPLC methods using charged aerosol detection to determine the lot-to-lot variability of these compounds.

AN193: Determination of Additives in Carbonated Beverages using Mixed-mode WAX-1 columns

2010-02-22T18:49:45.443

The soft drink industry is one of the largest in the world, with revenue from sales of carbonated soft drinks totaling billions of dollars annually. While the recipes for these beverages remain proprietary, critical components used as preservatives and sweeteners are subject to analysis for quality control, and must be identified on the beverage’s label. Additives such as benzoate and sorbate function as preservatives. Citrate is used as both a preservative and a flavor agent. Caffeine is an integral part of the overall profile of most colas. Aspartame, acesulfame, and saccharin are three common artificial sweeteners which function as sugar substitutes. Many methods have been developed for determining sweeteners and additives in drink formulations. In this application, we separate caffeine, sorbate, benzoate, citrate, aspartame, acesulfame and saccharin in carbonated drinks in a single run using the Acclaim® Mixed-Mode WAX-1 column. This column features a new mixed mode silica-based packing material that incorporates both hydrophobic and weak anion-exchange properties. Unlike traditional reversed-phase substrates, the new packing features an alkyl long chain with an ionizable terminus. The column demonstrates great potential for separating a wide variety of samples that contain a mixture of anionic and neutral compounds, including food, beverage, pharmaceutical, and chemical samples. The Acclaim column’s mixed-mode capability provides determination of the compounds of interest in many samples in a single injection, rather than two separate injections on two different types of columns.

Determination of Inorganic Anions in Municipal Drinking Water by Capillary ICS-5000

2011-04-25T14:27:47.953

Inorganic anions in municipal drinking water were determined on a ICS-5000 capillary Reagent-Free Ion Chromatography (RFIC) system. The anions were separated on a capillary IonPac AS19 anion-exchange column using an electrolytically generated gradient KOH eluent.

Determination of Inorganic Cations in Bottled Drinking Water by CS12A and Capillary ICS-5000

2011-05-04T09:19:37.937

Inorganic cations in bottled drinking water were separated on IonPac CS12A column using capillary ICS-5000 Reagent-Free Ion Chromatography (RFIC) system. Sample was diluted 2 fold prior to analysis. All cations were eluted within 10 minutes.

Separation of Resveratrol in Red Wine

2010-02-16T15:21:56.537

The composition of wine is highly complex. The superior peak capacity of the Acclaim 3 μm 3.0 × 250 mm column resolves resveratrol and related compounds against a difficult background of flavonoids. The Acclaim PA2 surface chemistry has a unique selectivity for polyphenolic compounds and gives excellent service life under acidic conditions. In this example, methanol provides better separation than acetonitrile, but generates much higher operating pressures. The high pressure rating (800 bar) for the separation column and LC system provide excellent solutions to applications requiring high plate counts (>30,000 plates/column) and high operating pressure (>400 bar). Sample Preparation: • Take 5.0 mL Zinfandel red wine • Fortify to 2 μg/mL resveratrol • Extract with 2 x 1 mL ethyl acetate • Weight of combined extracts approx. 1.5 g

Alternative Solvents for Analysis of Cationic Surfactants on the Acclaim Surfactant Column: Acetone

2010-02-19T15:15:18.69

The Acclaim Surfactant column is a high-efficiency silica column specially designed for separating different types of surfactants, including anionics, cationics, nonionics, and amphoterics. This column exhibits performance far superior to conventional C18 columns, especially for cationic surfactants. Shown here are the baseline separations of a collection of common cationic surfactants on an Acclaim Surfactant, 3 µm column using various organic modifiers. With the use of a 3 mm i.d. column, the mobile phase consumption can be reduced by 55% compared to the 4.6 mm i.d. column format. Acetonitrile is the most popular solvent for HPLC applications, but it is toxic, expensive, and subject to supply shortages. Alcohols are less expensive and less toxic, but have high viscosity, which results in high operating pressure and low peak efficiency. Acetone is a cheaper solvent with low-toxicity, low-viscosity, and selectivity similar to acetonitrile. Thus for applications using evaporative light scattering detection (ELSD), acetone is an excellent alternative to acetonitrile.

Anions in Mature Coconut Water by High Pressure Capillary IC on IonSwift MAX-100 column

2011-05-08T14:26:58.593

Anions in Mature Coconut Water by High Pressure Capillary IC on IonSwift MAX-100 column. Anions and organic acids are separated on anion-exchange monolith column optimized for the separation of organic acids. This application uses the speed advantages of the monolith with the separation characteristics for organic acids at capillary flow rates on a capillary ICS-5000 IC system.

RSLC Method for Determination of Lot-to-Lot Variability of PEG 400 with Charged Aerosol Detection

2010-10-20T08:34:19.983

This application provides a method to baseline resolve the 13 major congeners of polyethylene glycol 400 (PEG 400) in under 3 minutes. The Corona ultra provides range and sensitivity to analyze the compounds over 4 orders of magnitude. The data shown in the attached report clearly illustrates the observed differences between two lots of commercially available material along with other figures of merit for the method. The combination of the small RSLC PA II column, the UltiMate 3000 RSLC system, and CAD detector provide a fast reproducible approach to the analysis of small PEGs.

AN189: Determination of Explosive Compounds in Drinking Water using Parallel-HPLC with UV Detection

2010-02-15T14:06:28.697

Determination of residual explosive materials and their degradation products in the environment has drawn increased attention due to their toxicity, persistence, and increased demand for forensic analysis concerning national security. Gas chromatography has traditionally been used to detect and quantify explosive compounds; however, because some are thermally unstable or nonvolatile, using this method can result in inexact determinations. HPLC with UV detection, however, is ideally suited for low-level determination because it is not subject to these limitations. U.S. EPA Method 8330 describes an HPLC method with UV detection for determination of 14 priority explosives and related substances. The method recommends the use of a C18 reversed-phase column as the primary column for separation, and a secondary column for confirmation. Acclaim® Explosives E1 and E2 columns can provide baseline resolution for 14 compounds with complementary selectivity under identical chromatographic conditions (except mobile phase composition) while reducing analysis time. These columns were used with EPA Method 8330 and the results for column E1 are reported in this application. Analysis was performed by parallel LC using the UltiMate® x2 Dual HPLC system with UV detection. Seven additional related compounds were also determined using this method, two of which can be resolved from the 14 compounds in EPA Method 8330, along with an internal standard (1,2-dinitrobenzene).

Determination of Alkyl Surfactants by RP-HPLC-CAD

2010-12-17T09:23:16.563

Six alkyl surfactants are determined using the Acclaim Surfactant column and reversed-phase gradient elution, using the Corona Charged Aerosol Detector. LODs are approximately 30 ng on column.

AN189: Determination of Explosive Compounds in Drinking Water using Parallel-HPLC with UV Detection

2010-02-15T14:16:57.03

Determination of residual explosive materials and their degradation products in the environment has drawn increased attention due to their toxicity, persistence, and increased demand for forensic analysis concerning national security. Gas chromatography has traditionally been used to detect and quantify explosive compounds; however, because some are thermally unstable or nonvolatile, using this method can result in inexact determinations. HPLC with UV detection, however, is ideally suited for low-level determination because it is not subject to these limitations. U.S. EPA Method 8330 describes an HPLC method with UV detection for determination of 14 priority explosives and related substances. The method recommends the use of a C18 reversed-phase column as the primary column for separation, and a secondary column for confirmation. Acclaim® Explosives E1 and E2 columns can provide baseline resolution for 14 compounds with complementary selectivity under identical chromatographic conditions (except mobile phase composition) while reducing analysis time. These columns were used with EPA Method 8330 and the results for column E2 are reported in this application. Analysis was performed by parallel LC using the UltiMate® x2 Dual HPLC system with UV detection. Seven additional related compounds were also determined using this method, two of which can be resolved from the 14 compounds in EPA Method 8330, along with an internal standard (1,2-dinitrobenzene).

Fast Determination of Inorganic Cations in Sports Drink

2011-11-30T16:34:56.923

One of the important applications of ion chromatography is to determine the inorganic cations in beverages. Here shows an example of separating common inorganic cations in a sports drink using capillary ICS-5000 and capillary IonPac CS16 columns. Scaling down from analytical IC to capillary IC brings many benefits to customers, such as the reduction of eluent consumption, waste, and cost of ownership. By increasing the flow rate to 0.03 mL/min, the analysis of common inorganic cations can be done in less than 7 mins. At this flow rate, about 2100 psi backpressure was generated.

Determination of Inorganic Anions in Municipal Wastewater Using AS25 Column

2011-04-26T15:27:14.22

Inorganic anions in municipal wastewater were determined on a ICS-5000 Reagent-Free Ion Chromatography (RFIC) system. The anions were separated on a IonPac AS25 anion-exchange column using an electrolytically generated KOH eluent. Sample was diluted 10 fold and filtered prior to analysis.

AN 237: Analysis of Benzalkonium Chloride on the Acclaim Surfactant Column by High-Performance Liquid Chromatography

2010-02-22T11:56:45.953

In this application, a complete HPLC methodology for determining benzalkonium chloride homologs in real samples, such as a sterile elastic strip and eye drops, is presented. The HPLC analysis was performed on a specialty column, the Acclaim® Surfactant column, with UV detection. The stationary phase features a unique surface chemistry that effectively deactivates the ionic interaction between the silica surface and cationic surfactants, resulting in excellent peak shapes for cationic surfactants.

AB115: Determination of N-Methylcarbamates

2010-09-20T10:35:43.843

This application brief describes a faster and more sensitive method for determining the carbamates specified in Method 531.2. The separation was performed on an Acclaim® Carbamate column, which is designed for separation of these carbamates, and the detection was performed on the FLD-3400RS fluorescence detector, which provides maximum stray light suppression for higher detection sensitivity.

Brodifacoum in Rodent Bait

2010-02-10T13:04:36.813

Brodifacoum is a powerful second-generation anticoagulant related to warfarin and used as a rodenticide. It is synthesized as a mixture of two diastereomers. Commercial rodent bait formulations typically have about 0.005% active ingredient. The high resolution of the Acclaim® 120 C18 column permits the clean separation of the two isomers from the complex sample background. Sample Preparation: Mutually saturate ethyl acetate and water for use in the next step. Shake 1.0g of finely ground bait with 10.0 mL ethyl acetate, 5.0 mL water and 0.10 mL acetic acid. Centrifuge to separate the emulsion. Evaporate 3.0 mL of ethyl acetate fraction to dryness. Reconstitute in 0.60 mL acetonitrile. Filter.

Efficient Separations of Inorganic Anions in San Jose Municipal Drinking Water

2012-01-05T12:35:10.517

IonPac AS18 high capacity analytical columns provides new ways to achieve with faster separations ad improved resolution of critical pairs. All analysts of interests in San Jose municipal drinking water were baseline resolved at flow rate of 0.40 mL/min. The run time was reduced from 15 min to 8 min. The fast analysis of common anions in municipal waters samples by using 250mm column emphasizes the fast sample runs and higher resolution possible with high capacity column.

Analysis of Irgafos 168 by HPLC and Charged Aerosol Detection

2010-12-17T10:04:48.53

This method was used to determine a number of Hindered Amine Light Stabiliser (HALS) compounds by RP-HPLC and the Corona ultra charged aerosol detector. A post-column acid solvent is added to lower background for CAD. Here, Irgafos 168, is presented. A dynamic range of 1.6 to 12.5 µg o.c and an LOD of 50 ng o.c. was found.

Anions in Brewed Tea Using Capillary IC

2010-11-04T16:14:25.983

Cap AS19 English Breakfast Tea. This method shows anions in a brewed tea sample by capillary IC using a gradient separation on IonPac AS19 capillary anion-exchange column.

Fast Analysis of Inorganic Anions in Perrier Mineral Bottled Drinking Water

2012-01-05T12:13:47.827

All analysts of interests in Perrier mineral bottled drinking water were baseline resolved at flow rate of 0.40 mL/min. The run time was reduced from 15 min to 8 min with good baseline resolution. The fast analysis of common anions in municipal waters samples by using 250mm column emphasizes the fast sample runs and higher resolution possible with high capacity column.

Analysis of Polyethylene Glycols

2010-02-18T09:40:59.603

Polyethylene glycols (PEGs) have a wide variety of uses, including medical formulations, personal care products, and industrial applications. Various PEG products are characterized by their average molecular weights. The Acclaim Mixed-Mode HILIC-1 column offers excellent resolution based on chain length.

Fast determination of inorganic anions in water using IonPac AS18 4um column

2011-11-28T15:35:27.03

It is shown in this chromatogram that when the flow rate is increased to 0.02 mL/min, the common anions can be separated in less than 5 minutes using IonPac AS18 column. The analysis was performed by isocratic eluent, electrolytically generated by capillary ICS-5000 EG. The column utlizes the smaller particle size to provide good resolution. At 0.02mL/min flow rate, about 2000 psi backpressure was generated.

Anions and Organic Acids in Young Coconut water by High Pressure Capillary IC on IonSwift MAX-100

2011-05-08T13:50:28.127

Anions and Organic Acids in Young Coconut water by High Pressure Capillary IC on IonSwift MAX-100. This application uses the advantages of speed of monolith column technology while enjoying the chemistry of IonPac AS11 which is optimized for organic acid separations. While it is not necessary, this application is run on a high pressure capillary ICS-5000 IC system.

Fast Determination of Anions in Sunnyvale Municipal Wastewater

2011-06-21T16:00:13.89

Determination of common inorganic anions is an important application of Ion chromatography in water analysis industry. Here shows the analysis of anions in a municipal wastewater using IonPac AS18 Fast column.

Analysis of Shikimic Acid in Wine and Hot Wine Punch

2012-01-17T09:13:22.203

Shikimic Acid is discussed in literature as one potential marker for tracing and identifying the roots of different wine flavors. To date, only few HPLC separations are known, all of them tedious and time-consuming. This UHPLC separation features a high-speed screening method for the rapid analysis of Shikimic Acid in Wines, running on a Hypersil GOLD aQ with 1.9 µm particles, in a run time of 3.5 min with a total cycle time of less than 6 min. Sample preparation is as easy as possible by dilute-and-shoot - just add a four-fold excess of water to the wine sample. With a max. backpressure of 60 MPa, the method can seamlessly be run both on RSLC and SD systems.

Fast Determination of Inorganic Anions in City B Drinking Water Using Carbonate Eluents

2010-10-26T15:06:42.937

AS22 FAST_City B_DRINKING Water This method updates inorganic determinations in drinking water using carbonate eluents. All seven inorganic anions are determined within 5 min.

Fast Determination of Anions in Municipal Drinking Water

2011-07-06T11:07:30.53

Fast Determination of Anions in Municipal Drinking Water using Dionex IonPac AS18-Fast, 2 mm column. Inorganic anions in a drinking water sample were separated in less than 5 min using 23 mM potassium hydroxide electrolytically-generated eluent at 0.45 mL/min.

Trace Anion Standard by Concentration Using Cap IC and ICW-3000 Online Water Purifier

2011-12-12T20:44:58.187

Trace Anion Standard by Concentration Using Cap IC and ICW-3000 Online Water Purifier. Here we show the chromatogram of 200 uL of a ~100 ng/L 7-Anion Standard concentrated on a IonSwift MAC-100 concentrator column. Trace ion determinations in Ultra-Pure Water (UPW) are important analysis for the power industry because ionic contamination at µg/L and ng/L concentrations can cause corrosion of important process equipment resulting in unplanned and costly maintenance. Trace ion determinations have been thoroughly discussed in application documents published from 1996 to 2009. However, detection limits, sample handling, and blank stability have all been improved by recent advances in Dionex ion chromatography (IC) technology, including capillary IC, the Dionex AS-AP autosampler, and the ICW-3000 Online Water Purifier.

AN231: Determination of Melamine in Milk by Ion Chromatography with UV Detection

2010-02-22T19:33:18.81

In 2008, melamine was found as a contaminant of milk and milk-containing products after the discovery of melamine contamination of pet food. These contaminations resulted in infant and pet deaths. Both deliberate contaminations originated in China, with some contaminated products exported to neighboring and more distant countries. Melamine was added to both products to increase their apparent protein content, as it was determined by a nonspecific total nitrogen test and melamine has a large amount of nitrogen per unit mass. This application shows a specific way in which melamine can be determined in milk, powdered milk, and a milk-containing candy by IC using an IonPac® CS17 column and UV detection at 240 nm.

Determination of Cations in Municipal Wastewater by Capillary IC

2011-06-22T09:47:08.5

Determination f inorganic cations in water is an important application of ion chromatography. Here shows an example of the analysis of a municipal wasterwater using capillary IC and IonPac CS16 column.

Fast Analysis of Inorganic Anions in Sunnyvale Municipal Drinking Water

2012-01-05T12:46:16.327

Standard length 250 mm format of IonPac AS18 analytical column has an advantage of allowing larger injections of more concentrated and higher ionic strength matrix samples without dilution. IonPac AS18 high capacity analytical columns also provides new ways to achieve improved resolution of critical pairs with faster separations. All analysts of interests in Sunnyvale municipal drinking water were baseline resolved within 8 min at increased flow rate of 0.40 mL/min. The run time was reduced from 15 min to 8 min with good baseline resolution . The fast analysis of common anions in municipal waters samples by using 250mm column emphasizes the fast sample runs and higher resolution possible with high capacity column.

Clortrimazole in Athlete's Foot Ointment on Accalim 120 C8

2010-02-22T10:15:15.417

Clortrimazole is a popular antifungal agent used to treat athlete's foot and related conditions. Here the Acclaim C8 column is used to determine this active ingredient in topical ointment in under five minutes.

Peptide Map of Bovine Serum Albumin on Acclaim PolarAdvantage II (PA2)

2010-02-18T12:42:43.167

Anion Determinations on 4 mm IonPac AS25 Column for Sulfur Speciation

2011-05-08T16:44:50.563

Anion Determinations on 4 mm IonPac AS25 and IonPac AG 20 Guard Column for Sulfur Speciation. This column is optimized for sulfur speciation and resolution of sulfate from carbonate. This column is ideal for sulfite determinations in environmental samples.

Ultrafast Analysis of Water Soluble Vitamins by Parallel UHPLC

2010-02-23T11:40:54.523

This application separates 7 water soluble vitamins in less than 3 minutes using an UltiMate 3000 RSLC system that is configured in parallel mode. This configuration can run 2 different applications at the same time for increased throughput and reduced cost of investment. A second application for the analysis of fat soluble vitamins by parallel UHPLC can be accessed in the weblinks section

22 Underivatized Amino Acids with Charged Aerosol Detection

2011-05-19T06:58:09.483

The analysis of amino acids (AA) is important across many industries. Finding sensitive and accurate methods often requires the use of derivatization agents which can add time and complexity to the method. Presented here is a simple UHPLC gradient method using the new Acclaim RSLC PAII 2.1 x 250 mm column with Corona Charged Aerosol Detection (CAD). 22 amino acids were well resolved with the exception of glycine and threonine and were measured on the Corona ultra detector at differing levels (100-300 ng on column). The expected limit of detection for all amino acids shown is in the low nanogram level. The diode array data also presented for both 210 and 254 nm shows that only the aromatic amino acids could be detected and with much less sensitivity than the CAD. The fast UHPLC method provides a simple alternative to more time consuming or less sensitive amino acid methods especially for analytes in a simple matrix.

Fast Analysis of Inorganic Cations in Municipal Drinking Water

2011-12-01T15:12:16.907

Ion chromatography is a great technique to determine inorganic cations in water samples. An example of common cation separation using capillary ICS-5000 is shown here. The analysis time was less than 7 mins at 0.03 mL/min flow rate. All the analytes were eluted by isocratic eluent 30 mM MSA generated electrolytically by ICS-5000 EG.

Ethinylestradiol Tablets Assay according to the Chinese Pharmacopoeia

2010-02-26T15:06:01.487

This method describes how to assay Ethinylestradiol Tablets according to the Chinese Pharmacopoeia Preparing the Test Solution: Weigh accurately and powder 20 tablets. To a quantity, weigh accurately, equivalent to about 50 µg of ethinylestradiol in a cube with plug, add 10 ml of mobile phase, sonicate for 30 minutes until ethinylestradiol is dissolved. Shake well and centrifugate, take the supernatant as the test solution. Preparing the Reference Solution: Dissolve a quantity of ethinylestradiol CRS, accurately weighed, in mobile phase and dilute with mobile phase to produce a solution of about 5 µg per ml, repeat the operations of the test solution, calculate the content of C20H24O2 with respect to the peak area obtained in the chromatogram by the external method.

Determination of Inorganic Cations in Munuicipal Drinking Water of City San Francisco, CA by IonPac CS12A using ICS-5000 Capillary System

2011-05-04T09:45:02.843

Inorganic cations in municipal drinking water were determined on a ICS-5000 Reagent-Free Ion Chromatography (RFIC) system. The cations were separated on a IonPac CS12A cation-exchange column using an electrolytically generated MSA eluent.

Rapid Determination of Dopamine and Serotonin in Microdialysis Samples

2011-10-10T09:13:07.72

Significant insights into the working chemistry of the brain have occurred over the past few decades due to the coupling of microdialysis perfusion sampling with HPLC analysis with sensitive electrochemical detection. Neurochemical analysis of the biogenic amines Dopamine and Serotonin using in vivo methods today are pushing toward greater temporal and spatial resolution resulting in samples of lower concentration. The analysis requires both high sensitivity and rapid chromatography. Two approaches have evolved to address these needs: either rapid off line analysis to support very short collection times, or a balancing of collection and chromatographic times for direct on-line analysis. This new method for rapid analysis accommodates both approaches without sacrificing sensitivity. It utilizes a low volume amperometric detection approach to optimize speed, sensitivity and reliability. This application note presents an example of how the method can be used to measure low levels of dopamine (DA) and serotonin (5HT), using rapid separation conditions.

Ultrafast Analysis of Aspirin by UHPLC

2010-02-12T16:38:18.947

This application is a speed-up of the USP method for the assay of Aspirin. The original USP method uses a 4x300 mm column at a flow rate of 2 mL/min. It delivers resolution of 5.7 when used with the Acclaim 120 C18 column. This is an excellent candidate for acceleration with RSLC. Simply recomputing the operating parameters for a 2.1x50 mm column leads to a 10-fold increase in throughput and 96% savings in mobile phase per assay. The accelerated method still gives baseline resolution of the two components.

Analysis of Ethoxylated Lauryl Sulfate

2010-02-17T15:49:08.753

Laureth sulfate surfactants have both C12 and C14 alkyl chains, each with a series of ethoxylate oligomers. The Acclaim Mixed-Mode HILIC-1 column, with acetonitrile in the mobile phase, almost resolves both series. Acetonitrile gives higher selectivity for ethoxylation than does methanol. Detection is by evaporative light scattering (ELS).

Nimodipine Tablets Related Substances according to the Chinese Pharmacopoeia

2010-02-05T13:07:31.89

This method describes how to assess the Related Substances of Nimodipine Tablets according to the Chinese Pharmacopoeia Preparing the Test Solution: Dissolve an accurately weighed quantity of the powder, equivalent to about 10 mg Nimodipine, in the mobile phase in a 50 mL volumetric flask, ultrasonicate for 15 minutes, cool, dilute with the mobile phase to volume, mix well, and centrifuge at 3000 rpm for 10 minutes. The supernatant liquid is the test solution. Preparing the Reference Solution: Dilute the test solution with the mobile phase to produce a solution of 2 µg/mL as reference solution.

Analysis of Hostavin N30 by HPLC and Charged Aerosol Detection

2010-12-17T13:02:36.377

This method was used to determine a number of Hindered Amine Light Stabiliser (HALS) compounds by RP-HPLC and the Corona ultra charged aerosol detector. A post-column acid solvent is added to lower background for CAD. Here, chromatography of a polymeric HALS, Hostavin N30, is presented. A dynamic range of 3 to 50 µg o.c and an LOD of 930 ng o.c. was found.

Counter anion in Metaformin HCl tablet by Capillary IC

2011-04-14T13:39:06.64

Counter ion determinations in the pharmaceuticals provide important mass balance, contamination, and formulation information during early drug development through to the mature pharmaceutical product. Precise, accurate, and reproducible analytical methods are important to providing a reliable product, as such, IC is the method of choice. In this application, the counter anion, chloride, is determined in a Metaformin HCl tablet using anion-exchange chromatography on IonPac AS19 capillary column using an ICS-5000 capillary IC system.

Cation Determinations in Young Coconut Water by Capillary IC on IonPac CS12A Column

2011-05-08T15:54:33.78

Cation Determinations in Young Coconut Water by Capillary IC on IonPac CS12A Column. Young coconut water is a very popular beverage and has shown some medical interest. In this application, cation determinations by capillary IC demonstrate the high concentrations of cationic concentrations.

AN238: Determination of Sulfate and Sulfamate in Topiramate Using a Reagent-Free Ion Chromatography System

2010-07-02T05:32:10.983

In this application note (AN), we demonstrate the use of a Reagent-Free™ Ion Chromatography (IC) system with the IonPac® AS11 column and suppressed conductivity detection for the determination of sulfamate and sulfate in topiramate. The IonPac AS11 column has been successfully used in the pharmaceutical industry and is currently specified in several USP methods, including an assay for citric acid/citrate and phosphate in different pharmaceutical formulations, phosphite in etidronate disodium, and free sulfate in enoxaparin sodium injection. The IonPac AS11 column consists of a 13 μm microporous resin bead with a highly crosslinked core, and a MicroBead® anion-exchange layer that is functionalized with hydrophilic quaternary ammonium groups. The selectivity of the AS11 column is optimized for the separation of a large number of inorganic anions and organic acid anions using a hydroxide eluent gradient. Because the selectivity of sulfamate is similar to low molecular weight organic acids, the AS11 column is ideal for this application. The column enables the resolution of the target analyte from other excipients in a topiramate sample while also allowing the separation of sulfate within a reasonable time. An automated potassium hydroxide eluent generator eliminates the problems typically encountered when manually preparing hydroxide eluents, as described in the current USP method. In addition, no organic solvents are required, which further simplifies this analysis. In this application note, the linearity, detection limits, precision, and recovery of the sulfamate and sulfate degradation products in a topiramate sample are demonstrated.

Cations Determination in a Pharmaceutical Drug Using Capillary IC

2011-06-21T14:46:05.423

Ion chromatography has been widely used to determine counter ions in API and drug product in pharmaceutical industry. Here is an example of analyzing cations in a tablet using capillary IC on IonPac CS16 column.

Accelerated CARB1004 Carbonyl-DNPH Standards on Acclaim Explosives E2

2010-02-17T14:12:24.207

The 3 μm 3 x 150 mm Acclaim Explosives E2 column, with its smaller particle size and 800 bar pressure rating, permits a fourfold speedup of this analysis. CARB 1004 has the most difficult compound list of all the related standard methods for aldehydes and ketones. For less demanding methods, a more aggressive gradient may be used to gain even greater speed.

Anions and Organic Acids in Pomegranet-Grape Juice by Capillary IC Using Standard Flow Rates

2011-12-11T19:09:50.53

Anions and Organic Acids in Pomegranet-Grape Juice by Capillary IC Using Standard Flow Rates. High Pressure Capillary Reagent-Free™ ion chromatography (RFIC™) is the latest advancement in ion chromatography instrumentation. Typically with an RFIC system, the system pressure is limited to <3000 psi because of the limitations of materials in the RFIC accessories. Now with the upgrade to high pressure, the ICS-5000 IC capillary system can operate at system pressures <5000 psi. This advance in technology allows 2x to 3x the µL/min flow rates with all the same advantages as standard pressure capillary IC, resulting in low consumption of water (30 to 40 mL/d of water) and low waste generation. In capillary IC, the system can remain on without loss in resources, i.e., capillary IC is always on and ready for analysis. These advantages result in: 1. Greater ease-of-use, 2. Longer eluent generator cartridge life, 3. Lower cost of ownership. Additionally, the increase in mass sensitivity, comparable results are achieved as with standard bore system using a sample injection of only 0.4 µL. In this study, inorganic anions and organic acids from a diluted pomengranet-grape juice sample are separated by anion-exchange chromatography on a capillary size Thermo Scientific Dionex IonSwift MAX-100 monolith IC column. The IonSwift MAX-100 column is designed with a monolith backbone and optimized with Dionex IonPac AS11 anion-exchange chemistry. This column was selected for these high pressure cap IC experiments because of the high efficiency and high flow rate characteristics.

Analysis of Tinuvin 770 by HPLC and Charged Aerosol Detection

2010-12-17T12:19:18.983

This method was used to determine a number of Hindered Amine Light Stabiliser (HALS) compounds by RP-HPLC and the Corona ultra charged aerosol detector. A post-column acid solvent is added to lower background for CAD. Here, chromatography of a polymeric HALS, Tinuvin 770, is presented. A dynamic range of 3 to 25 µg o.c and an LOD of 50 ng o.c. was found.

AN 235: Determination of Oversulfated Chondroitin Sulfate and Dermatan Sulfate in Heparin Sodium Using Anion-Exchange Chromatography with UV Detection

2010-03-17T09:44:32.547

This application describes the separation of dermatan sulfate and OSCS from heparin using anion-exchange chromatography (AE) with UV detection according to the USP Stage 2 revision. Dermatan sulfate, OSCS, and heparin sodium are separated on a 2 mm IonPac® AS11 anion-exchange column (USP L61 type column) using a gradient separation, with sodium phosphate monobasic and sodium perchlorate mobile phase solutions at 0.22 mL/min and detected by UV absorbance at 202 nm.

AU151 Sucralose in Peach Citrus Carbonated Beverage

2010-07-26T16:35:06.47

This application update discusses the development of a HPAE-PAD method to determine sucralose in reduced-carbohydrate colas. HPAE-PAD has been used to determine sucralose in other sugar-free beverages, after a 50-fold dilution, and foods. Reduced-carbohydrate cola samples have high concentrations of fructose and sucrose relative to sucralose, making these samples challenging for chromatographic analysis. In this application update, we optimized the sample dilution and the eluent to separate high concentrations of fructose and sucrose from sucralose, while at the same time injecting enough sample to detect the low concentrations of sucralose in beverages.

Determination of Inorganic Anions in Bottled Water by Capillary IC

2011-04-25T15:25:17.453

Inorganic anions in bottled drinking water were determined on a ICS-5000 capillary Reagent-Free Ion Chromatography (RFIC) system. The anions were separated on a capillary IonPac AS19 anion-exchange column using an electrolytically generated gradient KOH eluent.

AN125: Monitoring Protein Deamidation by Cation-Exchange Chromatography

2010-08-17T00:38:52.14

This application note describes the use of the ProPac® WCX-10 column in a bio-inert HPLC system to monitor the products of protein deamidation. The ProPac WCX-10, a weak cation-exchange column, is well suited for the separation of protein variants produced by posttranslational modifications. The packing in this column is a unique pellicular resin with a hydrophilic coating and carboxylate functional groups on grafted linker arms. The physicochemical properties of this support eliminate secondary (nonionic) interactions between the protein analytes and the stationary phase, affording minimal band broadening and high selectivity. The UltiMate® 3000 Titanium System is an HPLC whose flow path ensures that neither solvents nor sample are in contact with stainless steel materials, removing concerns about iron and other transition metals contaminating the column and samples. In the example presented here, deamidated variants of ribonuclease A (RNase A) are separated from the native protein in less than 20 min on a ProPac WCX-10 weak cation-exchange column. This application note also compares the results of using a phosphate-based buffer to that of a 4-morpholineethanesulfonic acid (MES) -based buffer.

Determination of Lipids in Biodiesel by HPLC with CAD Detection

2010-07-23T08:24:30.907

In this application an RSLC biodiesel analysis method is shown that determines acylglycerols in fuels with a 10 min analysis time. This method avoids exceptionally toxic or environmentally damaging solvents, such as propionitrile and dichloromethane, which have previously been used for acylglycerol determination. Acylglycerols are determined in a biodiesel sample by injection of a sample diluted in ethyl acetate.

AN245: Fast HPLC Analysis of Dyes in Foods and Beverages

2010-03-09T00:51:36.203

Dyes have many applications in the food and beverage industries, such as being used to make food more appealing, hide defects, or to strengthen consumer perception of the association between color and flavor. For example, lime flavor is associated with the color green and thus, lime soft drinks are often colored with green food dye. Despite the existence of many dyes, only a few have been approved for use in foods and beverages. Reversed-phase chromatography is an excellent technique for the analysis of dyes. Many dyes are hydrophobic, readily soluble in reversed-phase eluents, and have strong visible and UV absorbance properties. This application note (AN) demonstrates fast separation of 10 dyes in less than 5 min using an Acclaim® PA2 (3 μm) column in a 3 × 75 mm format. The Acclaim PA2 column is ideal for resolving mixtures of compounds with a wide range of hydrophobicities, including very polar compounds. This method was used to determine the quantity of food dyes in six soft drinks and a gelatin dessert. The combination of an UltiMate® 3000 Rapid Separation LC (RSLC) system and an Acclaim PA2 column is suitable for the fast analysis of food and beverage samples that have both approved and illegal dyes.

Analysis of a non-UV Active Anticonvulsant (Gabapentin) by Charged Aerosol Detection (CAD)

2010-11-22T09:21:24.343

This application describes the analysis of several active pharmaceutical ingredients (APIs) including gabapentin which does not have a UV Chromophore. The gradient RSLC method was used to resolve the four compounds of interest in less than 4 minutes which were then analyzed using both the diode array and the Corona ultra detector. The limit of detection for the gabapentin was < 2 ng on column with the CAD.

AN191: Determination of Phenols in Drinking and Bottled Mineral Waters Using Online Solid-Phase Extraction Followed by HPLC with UV Detection

2010-02-16T16:38:58.247

Phenolic compounds are subject to regulation as water pollutants due to their toxicity. This application note details an online SPE method followed by HPLC with UV detection for determining the 11 phenols specified in U.S. EPA Priority Pollutants List at the concentrations required by world regulatory agencies. Phenols from drinking and bottled waters are trapped on an IonPac® NG1, a small polymeric reversed phase column, and then separated on a polar-embedded reversed-phase column, the Acclaim® PA. This automated method is a cost-effective way to determine phenols in drinking and bottled water samples. In the example shown the sample (Spiked Tap Water) is loaded on the SPE Columns using the SPE (left) pump of the dual gradient pump (see Figure 12 from application note 191, link below).

Fast Analysis of Inorganic Cations in Wine by Capillary IC

2011-12-01T15:45:18.953

Ion chromatography is a great technique to determine inorganic cations in beverages. Here shows an example of separating of cations in wine using capillary ICS-5000 IC System and IonPac CS16 column. The analysis time was less than 7 mins at 0.03 mL/min flow rate. The analytes were eluted by isocratic eluent 30 mM MSA, electrolytically generated by ICS-5000 EG.

Anions and Organic Acids in Apple Juice by Capillary IC

2011-12-11T16:03:14.39

Anions and Organic Acids in Apple Juice by Capillary IC. High Pressure Capillary Reagent-Free™ ion chromatography (RFIC™) is the latest advancement in ion chromatography instrumentation. Typically with an RFIC system, the system pressure is limited to <3000 psi because of the limitations of materials in the RFIC accessories. Now with the upgrade to high pressure, the ICS-5000 IC capillary system can operate at system pressures <5000 psi. This advance in technology allows 2x to 3x the µL/min flow rates with all the same advantages as standard pressure capillary IC, resulting in low consumption of water (30 to 40 mL/d of water) and low waste generation. In capillary IC, the system can remain on without loss in resources, i.e., capillary IC is always on and ready for analysis. These advantages result in: 1. Greater ease-of-use, 2. Longer eluent generator cartridge life, 3. Lower cost of ownership. Additionally, the increase in mass sensitivity, comparable results are achieved as with standard bore system using a sample injection of only 0.4 µL. In this study, inorganic anions and organic acids from a diluted apple juice sample are separated by anion-exchange chromatography on a capillary size Thermo Scientific Dionex IonSwift MAX-100 monolith IC column. The IonSwift MAX-100 column is designed with a monolith backbone and optimized with Dionex IonPac AS11 anion-exchange chemistry. This column was selected for these high pressure cap IC experiments because of the high efficiency and high flow rate characteristics. In these experiments, inorganic anions, phosphate, and citrate were separated at the standard flow rate of 12µL/min flow rates using an electrolytically-generated gradient.

Determination of cations in a Cholesterol Drug by Capillary IC

2011-06-21T15:35:52.547

This figure shows an application of IC in analying counter ions in pharmaceutical drugs. Inorganic cations in a cholesterol drug were determined by capilary IC. the separation was carried on IonPac CS16 column.

Indometacin Capsules Related Substances according to the Chinese Pharmacopoeia

2010-02-05T15:19:35.167

Description This method describes how to assess the Related Substances of Indometacin Capsules according to the Chinese Pharmacopoeia Preparing the Test Solution: Weigh accurately 20 capsules, remove the content. To a quantity, equivalent to about 50 mg of Indometacin, add a quantity of ethanol to a 100 mL volumetric flask, shake to dissolve Indometacin, dilute with ethanol to volume, mix well, and filter. Measure 5 mL of the successive filtrate in a 25 mL volumetric flask, dilute with 50% ethanol solution to volume, and mix well. Preparing the Reference Solution: Measure 1 mL of the test solution in a 100 mL volumetric flask and dilute with 50% ethanol solution to volume.

AN236: Determination of Iodide and Iodate in Seawater and Iodized Table Salt by HPLC with UV Detection

2010-02-05T11:23:38.743

In this application, High Performance Liquid Chromatography (HPLC) coupled with photodiode array UV detection is used to determine iodide and iodate in seawater, synthetic sea salt, and table salt. This method is specific, sensitive, and rapid. Iodide and iodate are separated using the Acclaim® Mixed-Mode WAX-1, a silica-based column that incorporates hydrophobic, weak anionexchange, and ion-exclusion properties.

Fast Determination of Inorganic Cations in Municipal Drinking Water

2011-11-30T16:46:20.627

One of the important applications of ion chromatography is to determine inorganic cations in drinking water to ensure the quality of the water and to protect the health publics. Here shows an example of a drinking water sample analysis using capillary ICS-5000 and capillary column IonPac CS16. In this example, the analysis was performed at 0.03 mL/min flow rate and the cations were eluted with 30 mM MSA electrolyticallly generated by capillary ICS-5000 EG. It took less than 7 mins for each analysis.

Dexamethasone Acetate Tablets Assay according to the Chinese Pharmacopoeia

2010-02-22T17:43:48.007

This application describes how to assay Dexamethasone Acetate Tablets according to the Chinese Pharmacopoeia Procedure: Weigh accurately and powder 20 tablets. Weigh accurately about 2.5 mf of dexamethasone acetate in a 50 ml volumetric flask, add a quantity of mobile phase, and apply 30 minutes of ultrasonic treatment until the dexamethasone acetate is dissolved. Dilute with mobile phase to the volume, shake well and filter, and take the filtrate as the test solution.

Determination of Anions in Municipal Wastewater of the City of Sunnyvale, California by ICS 900

2010-12-17T17:18:45.72

Anions in municipal wastewater of the city of Sunnyvale, California is determined by ICS 900 with suppressed conductivity detector using IonPac AS22 and IonPac AG22 columns

Anions in Brand B Bottled Water by Capillary IC on IonPac AS19

2010-10-29T14:58:49.233

Cap AS19 Brand B bottled water. Anions are determined in a bottled water sample using capillary IC on IonPac AS19 capillary column.

Determination of Anions in a Municipal Wastewater Sample on 4 mm IonPac AS25 Column

2011-05-08T17:01:26.343

Determination of Anions in a Municipal Wastewater Sample on IonPac AS25 and IonPac AG20 Columns. This application demonstrates anion determinations on the IonPac AS25 column optimized for sulfur speciation determinations. Additionally, sulfate is well resolved from carbonate. This column is ideal for sulfite determinations in environmental samples.

High-Resolution Triglyceride Profile of Cooking Oils

2010-02-18T10:19:15.553

When comparing oils of similar properties, or trying to get a detailed profile of an oil, a high-resolution analysis is needed. The Acclaim 120 RSLC C18 2.2 µm 2.1, 100 mm column provides excellent efficiency without a speed penalty. Selectivity is improved by using an acetonitrile/ethyl acetate gradient at sub-ambient temperature.

Analysis of Phosphopeptides by Automated IMAC in Gallium Form

2010-02-11T12:59:29.097

Immobilized metal affinity chromatography (IMAC) is a powerful tool for enriching phosphopeptide isolates from protein digests. Gallium and iron are typically used as the immobilizing metals in IMAC. An automation package consisting of the Dionex dual-gradient LC system, ProPac IMAC-10 (for enrichment) and Acclaim 300 analytical column is the perfect solution for this technique. Sample preparation details β-Casein, 2 mg/mL, reduced and carboxymethylated, digestion with immobilized trypsin, diluted 1:1 in 200 mM formic acid.

Omega Free Fatty Acids by RP-HPLC and Charged Aerosol Detector

2011-04-18T07:43:51.14

Natural oils and fats were base hydrolyzed, neutralized and analyzed directly by reversed-phase HPLC using the Corona ultra charged aerosol detector. Samples were not derivatized or processed further. LOD's were less than 15 ng on column for 12 of the 14 analytes in this application, and several samples are shown in the attached poster.

Fast Diisocyanates by OSHA Method 42 on Acclaim RSLC PolarAdvantage II

2010-02-19T12:03:41.65

Diisocyanates TDI and HDI are commonly used in the manufacture of urethane polymers, and are highly toxic by inhalation and carcinogenic. OHSA method 42 is a standard method for testing workplace air for contamination. The Acclaim RSLC PolarAdvantage II (PA2) 2.2 ìm column, a reversed-phase column based on an amide-embedded group, not only provides suitable selectivity for these diisocyanates but also allows an acceleration of about eightfold over the conventional method. The use of elvated temperature improves the resolution of peaks 1 & 2, while reducing the empty space between peaks 2 & 3. It also reduces the backpressure to about 210 bar, well within the range of conventional HPLC pumps. Sample Preparation: Samples are collected by drawing a known volume of air through glass fiber filters coated with 0.1 mg of 1-(2-pyridyl)piperazine (1-2PP) which are contained in open-face cassettes. Samples are extracted with 90/10 (v/v) acetonitrile/dimethyl sulfoxide (ACN/DMSO) and analyzed by high performance liquid chromatography (HPLC) using an ultraviolet or fluorescence detector. (The coated filters used in Method 47 for MDI are also acceptable for this procedure. Those filters are coated with 1 mg instead of 0.1 mg of 1-2PP.)

AN225: Rapid Method for the Estimation of Total Free Monosaccharide Content of Corn Stover Hydrolysate Using HPAE-PAD

2010-02-18T13:54:15.787

Corn stover is the leaf, husk, stalk, and cob remaining in the field after harvest and makes up about half the yield of a crop of corn. Corn stover provides 1.3 billion tons of raw material annually and is a common feedstock for fermentation systems used in biofuel production. Corn stover is acid-hydrolyzed in 0.5 to 1.5% (w/w) sulfuric acid, to release a watersoluble mixture of carbohydrates, typically consisting of arabinose, glucose, galactose, mannose, xylose, fructose, and cellobiose among other noncarbohydrate substances. Pulsed amperometric detection (PAD) has a broad linear range for monosaccharides and most other carbohydrates, and is selective for compounds that can be detected under a given set of electrochemical conditions. High-performance anion-exchange (HPAE) chromatography can separate glucose, galactose, arabinose, xylose, mannose, fructose, cellobiose, and other carbohydrates. The CarboPac® PA1 anion-exchange column rapidly elutes corn stover carbohydrates, resolving the monosacccharides from the unretained and undetected noncarbohydrate components of acid-hydrolyzed corn stover. Under these conditions, disaccharides and trisaccharides are also resolved, with a total elution time less than 10 min.

UHPLC-Fluorescence Detection of Eosin Y in Groundwater Studies

2010-04-23T02:38:09.923

Eosin Y is an important tracer in groundwater studies. Determining water migration paths helps understanding the geography of landscapes and identifying the distribution and fate of environmental pollutants originating from various waste sites. Spectrofluorimetry, HPLC with fluorescence detection, and capillary LC/fluorescence detection are approaches to sensitively detect Eosin Y. HPLC analysis in combination with fluorescence analysis provides a convenient way to separate eosin from humic substances and interfering tracers. Here we demonstrate the separation of an Eosin standard obtained with a binary gradient. The main component Eosin Y is fully resolved from two impurities. A gradient curve is used to reduce the peak broadening for focussing the main compound peak and therefore an improved signal to noise ratio. The mobile phase is buffered at 5.5 to ensure the highest fluorescence intensity. The more acidic the pH, the more fluorescence light emission is significantly quenched. Zero carry-over is assured by wash cycles before and after the injection.

Anions and Organic Acids in Brewed Decaffeinated Coffee by High Pressure Capillary IC on IonSwift MAX-100

2011-05-08T14:46:35.483

Anions and Organic Acids in Brewed Decaffeinated Coffee by High Pressure Capillary IC on IonSwift MAX-100 column. This application demonstrates the separation of many organic acids commonly found in complex samples. The method uses the speed advantages of monoliths with the anion-exchange chemistry to separate many organic acids. Additionally, this is a capillary application on ICS-5000 capillary system.

Melamine and Cyanuric Acid on Acclaim Mixed-Mode WAX-1

2010-03-01T15:39:01.683

Melamine and cyanuric acid have been used as both legal and illegal additives in animal feed. In this method, the Mixed-Mode WAX-1 column is uses a combination of HILIC and anion exchange to retain these polar molecules. Since the buffer is volatile, LC/MS may be used to improve the sensitivity and selectivity of the method.

AN227 Determination of Total Cyanide in Municipal Wastewater

2010-07-23T16:14:40.03

In this Application Note, we describe an ion exclusion chromatography (ICE) method with pulsed amperometric detection (PAD) using a Pt disposable working electrode and an optimized waveform to determine total cyanide in drinking and wastewater samples. The samples are acid distilled, trapped in 1 M NaOH, and diluted to 250 mM NaOH prior to analyses using the EPA-approved MICRO DIST™ sample preparation system. This ICE-PAD method has the advantages of eluting cyanide before sulfide with Rs > 3, and excluding other interferences, such as chloride and sulfate that typically interfere in ion exchange methods resulting in a more sensitive and accurate method. Analytes are also selectively detected by PAD while other compounds remain undetected. This ICE-PAD method provides a fast, reliable, sensitive, and selective method to directly determine µg/L to sub- µg/L concentrations of total cyanide in wastewater. In this Application Note, we demonstrate the linearity, detection limit of 0.27 µg/L, accuracy, and precision for the determination of total cyanide in drinking water and wastewater samples using the MICRO DIST system and ICE-PAD.

Fast Analysis of Inorganic Anions in Evian Bottled Drinking Water

2012-01-05T11:51:16.343

IonPac AS18 high capacity analytical columns provides new ways to achieve improved resolution of critical pairs with faster separations. In this study, all analysts of interests in Evian bottled drinking water were baseline resolved at flow rate of 0.40 mL/min. The run time was reduced from 15 min to 8 min with good baseline resolution. The fast analysis of common anions in waters samples by using 250mm column emphasizes the fast sample runs and higher resolution possible with high capacity column.

Fast Analysis of Fexofenadine and Pseudo-ephedrine

2010-02-17T09:25:35.267

Fexofenadine is a second-generation, nonsedating antihistamine and pseudo-ephedrine is a decongestant. This combination is a popular treatment for relief of allergy symptoms. The analysis is difficult because the two drugs have very different hydrophobicities, but both are strong basic amines with a tendency to tail. Acclaim PolarAdvantage is well suited to this challenge as it delivers good base asymmetry over a wide range of mobile phase compositions. The short 4.6x50 mm format enables this analysis to be completed in less than 3.5 minutes.

AN 188: Determination of Glycols and Alcohols in Fermentation Broths Using Ion-Exclusion Chromatography and Pulsed Amperometric Detection

2010-02-19T10:48:58.35

Fermentation with yeast, bacteria, or other microorganisms has been used for centuries to produce alcoholic beverages, bread, cheese, yogurt, and feed stock for animals. Fermentation broths are complex mixtures of microorganisms and both organic and inorganic compounds. Ionic compounds, carbohydrates, and amino acids are essential for cellular growth and structure. Organic acids, alditols (sugar alcohols), glycols, alcohols, and other compounds are metabolic byproducts. To optimize growth and yields, it is crucial to monitor fermentation broths for both cellular fuel sources as well as metabolic byproducts. For beer and wine, the absence or presence of aldehydes and glycols affects their quality and flavor. Alcohols and glycols have been determined using ion exclusion chromatography with an IonPac® ICE-AS1, using methanesulfonic acid. The waveform and platinum electrode used here allow fast, accurate determinations of alcohols and glycols in fermentation media and alcoholic beverage samples through ion exclusion chromatography with PAD.

Efficient Separations of Inorganic Anions in UK Municipal Drinking Water Samples

2012-01-04T16:11:48.687

Inorganic anions existing in UK municipal drinking water were baseline resolved within 4 min while good resolution was obtained on Thermo Scientific Dionex IonPac AS18-Fast analytical column. The fast analysis of common anions in municipal waters samples emphasizes the fast sample runs and higher resolution possible with “Fast” (150 mm) version of the 2 mm column.

Analysis of 9 Steroids by UHPLC

2011-02-25T00:15:42.877

This applications separates 9 steroids in less than 4 minutes. It was run on an UltiMate 3000 RSLC system, and used an Acclaim RS column.

AN99: Peptide Mapping of Ovalbumin Using Reversed-Phase High-Performance Liquid Chromatography and Prediction of Phosphopeptide Elution

2010-06-11T06:35:21.233

This application note describes a method to reduce, alkylate, and enzymatically digest ovalbumin into peptides using trypsin. These peptides are separated by a reversed-phase HPLC method using an Acclaim® 300, C18 column. The Acclaim 300 column with its 300 Å pore size and 3 μm silica particle size is designed for the rapid analysis of peptide mixtures or proteins. The stable bonding of the Acclaim 300, C18 columns results in predictable reversed-phase separations with minimal secondary interactions and makes them compatible with LC/MS applications. Treating the ovalbumin tryptic digest with alkaline phosphatase removes phosphate from the phosphopeptides. Comparing tryptic maps with and without alkaline phosphatase treatment enables a tentative identificationof the phosphopeptides. The Dionex UltiMate® 3000 HPLC system equipped with an Acclaim 300, C18 column is an excellent solution for routine peptide mapping applications.

Peptide Map of Fetuin on Acclaim PolarAdvantage II (PA2)

2010-02-18T13:01:30.983

Tetracyclines in Pork

2010-02-15T13:33:24.07

Tetracyclines are wide-spectrum antibiotics commonly used for infections in humans and livestock. Animal studies show that tetracycline can cross the placental barrier, and can have toxic effects on developing fetuses. Long term exposure in humans may also lead to the development of antibiotic-resistant strains of bacteria. Tetracycline contaminants in a pork sample are rapidly and easily quantified using a Dionex HPLC system and UV detection. For the determination of tetracycline in pork the gradient program separates four tetracyclines in less than 5 minutes. Sample Preparation: Take 2.0 g pork muscle tissue. Grind with mortar and pestle in sequence with: - 0.1 g of citric acid - 1.0 mL of 3.6 M HNO3 - 4.0 mL of methanol - 1.0 mL of water and then centrifuge the sample.

AN210: Determination of the Phosphate Content of Phosphorylated Proteins

2010-02-22T14:13:53.53

In this Application Note, the determination of phosphate with an RFIC-EG system and suppressed conductivity detection is described. This method directly determines phosphate without any derivatization in 5 min, saving sample and time. This method is used to determine phosphate in six lots of ovalbumin, and single lots of phosvitin and b-casein. The RFIC-EG system delivers fast, accurate, and reproducible determinations of the phosphate contents of phosphorylated proteins.

Automated Method Development for Diuretics

2010-03-03T09:50:21.907

HPLC method development is still considered one of the crucial bottlenecks impeding productivity in analytical laboratories. Usually, due to the variety of available columns, the proper selection of the stationary phase represents the greatest challenge. Despite all efforts in the field of phase characterization and phase property indexing, an unambiguous selection approach is still missing. With the introduction of alkaline stable silica-based stationary phases, a large palette of mobile phase additives and pH values are applicable in reversed phase chromatography. This results in a vast number of parameters which may have to be tackled in method development. In this paper we present a new integrated system that allows automatic and intuitive scouting of columns and eluents. The system includes quaternary gradient capabilities, an autosampler compatible with well plates and standard sample formats, and a powerful diode array detector. Switching valves in the column compartment are used to select between columns. The example shown is method development for diuretics. A diuretic is any drug that elevates the rate of urination and thus provides a means of forced diuresis. There are several categories of diuretics.

Water-Soluble Vitamins on Acclaim RSLC PolarAdvantage II (PA2) with TFA Mobile Phase Additive

2010-02-19T10:22:57.877

Determination of Inorganic Anions in Municipal Drinking Water by Capillary IC

2011-04-25T15:10:35.813

Determination of Inorganic Anions in Municipal Wastewater by Capillary IC

2011-04-25T14:44:52.25

Inorganic anions in municipal wastewater were determined on a ICS-5000 capillary Reagent-Free Ion Chromatography (RFIC) system. The anions were separated on a capillary IonPac AS19 anion-exchange column using an electrolytically generated gradient KOH eluent.

Carbohydrates in Chocolate Syrup Using HPAE-PAD on a Capillary IC System

2010-11-14T11:52:30.937

Cap_PA20_JC_chocolate syrup. Carbohydrates were determined in a chocolate syrup sample using electrolytically-generated eluent on a capillary CarboPac PA20 column and an ICS-5000 capillary system.

Counter Cation in Atorvastatin calcium by Capillary IC

2011-04-14T14:16:24.377

Counter ion determinations in the pharmaceuticals provide important mass balance, contamination, and formulation information during early drug development through to the mature pharmaceutical product. Precise, accurate, and reproducible analytical methods are important to providing a reliable product, as such, IC is the method of choice. In this application, the counter cation, calcium, is determined in a Atorvastatin calcium tablet using cation-exchange chromatography on IonPac CS12A capillary column using an ICS-5000 capillary IC system.

AN 205: Determination of Cefepime and Cefepime-Related Substances Using HPLC with UV Detection

2010-02-12T15:49:51.493

This application maximizes either the speed or the resolution of the United States Pharmacopeia (USP) and the European Pharmacopeia (EP) published monographs, for determining Assay and Related Substances of Cefepime. The Acclaim 120 C18, 3 µm column is used in accordance with L1 column defined by the USP. Cefepime, a fourth generation cephalosporin, is a broad spectrum antibiotic with improved activity against Gram-negative bacteria over other commercially available cephalosporin drugs. Analysis of cefepime purity is particularly challenging due to isomeric and other impurities with similar structures. The chemical instability of the strained ß-lactam ring system and the variable stability of different substituted groups require that analysis of these compounds be rapid. In addition to the need for fast analysis times, superior resolution is necessary to separate synthetic byproducts.

Amoxicilin Capsules Assay according to the Chinese Pharmacopoeia

2010-02-22T11:24:47.847

This method describes how to assay the Amoxicillin Capsules according to the Chinese Pharmacopoeia Preparing the Test Solution: Dissolve an accurately weighed quantity of the mixed contents obtained from the test for weight variation of contents, equivalent to about 0.125 g of amoxicillin, in phosphate buffer (pH 5.0) to produce a solution of 0.5 mg per ml, filter. Preparing the Reference Solution: Dissolve about 25 mg of amoxicillin, accurately weighed, in a 50 ml volumetric flask, dilute with the mobile phase to volume, mix well. Inject 20 µL of the resulting solution onto the column.

Underivatized Ionophoric Antibiotics by HPLC and Charged Aerosol Detector

2011-05-19T10:58:26.36

Ionophoric antibiotics, such as Monensin sodium, Salinomycin, Lasolacid A, and Narasin are used in industrial agriculture to enhance the production rate of poultry and beef. Current HPLC methods require the use of post-column derivatization with methanolic, sulphuric acid vanillin reagent and heating to provide a UV response. Using the Corona ultra, this method provides for the direct determination of these analytes down to 6 ng on column while satisfying the USP system suitability requirements.

Anions and Organic Acids in Apple Juice by High Pressure Capillary IC Using Standard Flow Rates

2011-12-11T17:16:00.72

Anions and Organic Acids in Apple Juice by High Pressure Capillary IC. This application uses standard flow rates and therefore doesn't use the high pressure capabilities. High Pressure Capillary Reagent-Free™ ion chromatography (RFIC™) is the latest advancement in ion chromatography instrumentation. Typically with an RFIC system, the system pressure is limited to <3000 psi because of the limitations of materials in the RFIC accessories. Now with the upgrade to high pressure, the ICS-5000 IC capillary system can operate at system pressures <5000 psi. This advance in technology allows 2x to 3x the µL/min flow rates with all the same advantages as standard pressure capillary IC, resulting in low consumption of water (30 to 40 mL/d of water) and low waste generation. In capillary IC, the system can remain on without loss in resources, i.e., capillary IC is always on and ready for analysis. These advantages result in: 1. Greater ease-of-use, 2. Longer eluent generator cartridge life, 3. Lower cost of ownership. Additionally, the increase in mass sensitivity, comparable results are achieved as with standard bore system using a sample injection of only 0.4 µL. In this study, inorganic anions and organic acids from a diluted apple juice sample are separated by anion-exchange chromatography on a capillary size Thermo Scientific Dionex IonSwift MAX-100 monolith IC column. The IonSwift MAX-100 column is designed with a monolith backbone and optimized with Dionex IonPac AS11 anion-exchange chemistry. This column was selected for these high pressure cap IC experiments because of the high efficiency and high flow rate characteristics.

Anions in Italian Municipal Wastewater Sample by Capillary IC

2010-11-21T19:47:18.077

Cap AS19_Italian Wastewater. Inorganic anions were determined on a ICS-5000 capillary Reagent-Free Ion Chromatography (RFIC) system. The anions were separated on a capillary IonPac AS19 anion-exchange column using an electrolytically-generated gradient KOH eluent.

Fast Determinations of Inorganic Anions in City C Drinking Water Using Carbonate Eluents

2010-10-26T15:42:38.64

AS22 FAST_City C DRINKING Water This method updates previous anion determinations in drinking water using carbonate eluents. All seven inorganic anions are determined on IonPac AS22 Fast within 5 min.

AN239: Determination of Iodide in Seawater and Other Saline Matrices Using a Reagent-Free Ion Chromatography System with Suppressed Conductivity and UV Detections

2010-02-26T16:18:00.173

In this application note (AN), a RFIC-EG™ system with UV detection is used to determine iodide in seawater, synthetic sea salt, and iodized table salt. Iodide is separated from other matrix anions on the IonPac® AS20 column, which is a high-capacity column designed for the separation of polarizable anions. The unique selectivity of this column makes it ideal for separating hydrophobic anions in matrices with high concentrations of chloride, sulfate, and carbonate. The high capacity of the IonPac AS20 column allows the determination of iodide in saline matrices with no sample pretreatment. Furthermore, by detecting iodide by UV absorbance, other anions, such as chloride and carbonate, are not detected and do not interfere with iodide determination. This proposed method is further simplified by using a 2 mm column format and an in-line high-pressure hydroxide eluent generator requiring only the addition of deionized water for continuous operation. In this AN, the linearity, detection limits, precision, and recovery of iodide in saline matrices for the proposed method are demonstrated.

AN202: High Performance Anion-Exchange Chromatography with Pulsed Amperometric Detection (HPAE-PAD) Analysis of Mannose-6-Phosphate

2010-02-19T11:29:34.287

This application note describes a method for determining M-6-P in glycoproteins using HPAE-PAD. Acid-hydrolyzed BSA is used as a generic protein matrix because a commercially available M-6-P-containing protein could not be found. M-6-P added to hydrolyzed BSA was separated on a CarboPac PA200 analytical column using 100 mM sodium hydroxide and 100 mM sodium acetate at 0.5 mL/min for 30 min. M-1-P (3.3 min) and M-6-P (10.7 min) peaks were fully resolved. Peak identification was confirmed by the absence of both peaks after dephosphorylation with alkaline phosphatase, and by determining mannose with a second HPAE-PAD assay. This application note shows that HPAEPAD is a fast, direct (no sample derivatization) method for determining the M-6-P content of a glycoprotein.

Oxyhalides determinations in UK municipal drinking water by High Pressure Cap IC

2011-12-11T19:57:12.313

Oxyhalides determinations in UK municipal drinking water by High Pressure Cap IC High Pressure Capillary Reagent-Free™ ion chromatography (RFIC™) is the latest advancement in ion chromatography instrumentation. Typically with an RFIC system, the system pressure is limited to <3000 psi because of the limitations of materials in the RFIC accessories. Now with the upgrade to high pressure, the ICS-5000 IC capillary system can operate at system pressures <5000 psi. This advance in technology allows 2x to 3x the µL/min flow rates with all the same advantages as standard pressure capillary IC, resulting in low consumption of water (30 to 40 mL/d of water) and low waste generation. In capillary IC, the system can remain on without loss in resources, i.e., capillary IC is always on and ready for analysis. These advantages result in: 1. Greater ease-of-use, 2. Longer eluent generator cartridge life, 3. Lower cost of ownership. Additionally, the increase in mass sensitivity, comparable results are achieved as with standard bore system using a sample injection of only 0.4 µL. In this study, inorganic anions from a municipal drinking water sample are separated by anion-exchange chromatography on a capillary size Thermo Scientific Dionex IonSwift MAX-200 monolith IC column. The IonSwift MAX-200 column is designed with a monolith backbone and optimized with Dionex IonPac AS19 anion-exchange chemistry. This column was selected for these high pressure cap IC experiments because of the high efficiency and high flow rate characteristics.

Separation of Glyceric, Glycolic, Lactic, Acetic, and Levulinic Acids on Acclaim Mixed-Mode WAX-1

2010-02-22T10:22:07.477

This group of very hydrophilic acids are difficult to separate using a reversed-phase column. But on the Acclaim Mixed-Mode WAX-1 column, this task become quite easy. The desirable selectivity results from its unique column chemistry which combines both reversed-phase and anion-exchange properties on the same column. The separation can be optimized by adjusting mobile phase solvent content and/or buffer concentration. In this separation, 5% acetonitrile in the mobile phase keeps the overall run time short and influences the resolution of critical pairs.

Determination of Anions in Municipal Wastewater of the City of San Jose, California by ICS 900

2010-12-17T16:22:19.877

Anions in municipal wastewater of the city of San Jose, California is determined by integrated IC system ICS 900 with suppressed conductivity detector. Sodium carbonate and sodium bicarbonate are used as eluent and IonPac AG22 and IonPac AS22 are used to perform the experiment. Sample is diluted 5 fold by DI water.

Determination of Anions in UK Drinking Water by ICS 900

2010-12-17T17:05:53.437

Anions in UK drinking water is determined by integrated IC system ICS 900 with suppressed conductivity detector using IonPac AG22 and IonPac AS22 columns.

Determinaiton of Anions and Organic Acids in Carbonated Fruit Flavored Beverage by Capillary IC

2011-04-14T17:44:33.64

Anions and organic acids are important part of the flavor experienced by drinking a carbonated beverage. Additionally, some anions are acidulants or preservatives used to maintain the intended flavor and inhibit biological contamination, known commonly as "spoiling". In this application, anions and organic acids in a carbonated fruit-flavored beverage are determined by capillary IC and suppressed conductivity on the ICS-5000 capillary IC system.

AN 196: Determination of Polycyclic Aromatic Hydrocarbons (PAHs) in Edible Oils by Donor-Acceptor Complex Chromatography(DACC)-HPLC with Fluorescence Detection

2010-02-16T20:50:44.433

This application note describes the setup and method for determining PAHs in edible oils on-line using a Dionex UltiMate® 3000 ×2 Dual-Gradient HPLC platform. This solution couples donor-acceptor complex chromatography (DACC) cleanup directly with an analytical HPLC and was performed on an HPLC system equipped with a dual-gradient HPLC pump and two switching valves which was fully automated using Chromeleon CDS. On-line coupling of sample preparation and analysis eliminates the complex manual pretreatment required by traditional methods. This automation reduces unintentional errors and increases reproducibility. The analysis time per sample is approximately 80 min with the dual-gradient HPLC system, compared to 8–10 h with traditional methods. Moreover, this automated system can run 24 h a day, significantly increasing sample throughput and making this complex analysis routine.

Anions in a carbonated fruit beverage by High Pressure Capillary IC

2011-12-11T16:35:30.483

Anions in a carbonated fruit beverage by High Pressure Capillary IC High Pressure Capillary Reagent-Free™ ion chromatography (RFIC™) is the latest advancement in ion chromatography instrumentation. Typically with an RFIC system, the system pressure is limited to <3000 psi because of the limitations of materials in the RFIC accessories. Now with the upgrade to high pressure, the ICS-5000 IC capillary system can operate at system pressures <5000 psi. This advance in technology allows 2x to 3x the µL/min flow rates with all the same advantages as standard pressure capillary IC, resulting in low consumption of water (30 to 40 mL/d of water) and low waste generation. In capillary IC, the system can remain on without loss in resources, i.e., capillary IC is always on and ready for analysis. These advantages result in: 1. Greater ease-of-use, 2. Longer eluent generator cartridge life, 3. Lower cost of ownership. Additionally, the increase in mass sensitivity, comparable results are achieved as with standard bore system using a sample injection of only 0.4 µL. In this study, inorganic anions and organic acids from a diluted fruit-flavored beverage sample are separated by anion-exchange chromatography on a capillary size Thermo Scientific Dionex IonSwift MAX-100 monolith IC column. The IonSwift MAX-100 column is designed with a monolith backbone and optimized with Dionex IonPac AS11 anion-exchange chemistry. This column was selected for these high pressure cap IC experiments because of the high efficiency and high flow rate characteristics.

Water Baseline Injection with ICW-3000 Online Water Purifier Installed

2012-01-06T14:56:56.327

Trace ion determinations in Ultra-Pure Water (UPW) are important analysis for the power industry because ionic contamination at µg/L and ng/L concentrations can cause corrosion of important process equipment resulting in unplanned and costly maintenance. Trace ion determinations have been thoroughly discussed in application documents published from 1996 to 2009. However, detection limits, sample handling, and blank stability have all been improved by recent advances in Dionex ion chromatography (IC) technology, including capillary IC, the Dionex AS-AP autosampler, and the ICW-3000 Online Water Purifier.

Determination of Anions by ICS 5000 using IonPac AS25 Column

2011-05-03T15:31:54.047

IonPac AS25 is a high-capacity, hydroxide-selective, optimized for the separation of multivalent anions, inclusing polarizable anions(perchlorate) and sulfur speciation(sulfite, ulfate, thiocyanate and thiosulfate).

Cation Determinations in San Jose municipal wastewater by Capillary IC on IonPac CS12A

2011-05-08T16:32:03.267

Cation Determinations in San Jose municipal wastewater by Capillary IC on IonPac CS12A. Cations are determined by capillary IC on ICS-5000 capillary IC system.

Anions in A Sports Beverage Using Capillary IC

2010-11-04T15:59:53.127

Cap AS19 Brand A Sports Beverage. Anions are determined in a sports beverage by capillary IC on IonPac AS19 capillary anion exchange column.

Theanine and Amino Acids in Green Tea Separated Using the Acclaim RSLC PolarAdvantage Column

2011-01-26T10:18:13.907

Green tea is a complex beverage with many flavor components and physiologically active substances. Amino acids, especially glutamate, contribute to the savory “umami” flavor. The most abundant amino acid in green tea is theanine, or N’-ethylglutamine. This unusual amino acid is noted for its mild relaxing effect. The amino acids are analyzed by automated precolumn derivatization with o-phthalaldehyde and N,N-dimethylaminoethanethiol. The Acclaim RSLC PolarAdvantage 2.2 μm column is compatible with highly aqueous mobile phases and provides good selectivity to separate the derivatives of amino acids present in green tea. Automated Derivatization Conditions Reagent A: 5 mg/mL o-Phthalaldehyde in 0.5 M potassium borate buffer, pH10.4 Reagent B: 10 mg/mL N,N-Dimethylaminoethanethiol hydrochloride in water Reagent C: 2 M Acetic acid Program: Draw 3 μL air, draw 2.5 μL reagent A, draw 0.5 μL sample, wash needle, draw 2.5 μL reagent B, in-needle mixing six times 16 μL, wait 60 s, wash needle, draw 1.5 μL reagent C, mix three times 16 μL, inject.

Anions and Organic Acids in Orange Juice by High Pressure Capillary IC

2011-12-11T17:24:17.907

Anions and Organic Acids in Orange Juice by High Pressure Capillary IC. High Pressure Capillary Reagent-Free™ ion chromatography (RFIC™) is the latest advancement in ion chromatography instrumentation. Typically with an RFIC system, the system pressure is limited to <3000 psi because of the limitations of materials in the RFIC accessories. Now with the upgrade to high pressure, the ICS-5000 IC capillary system can operate at system pressures <5000 psi. This advance in technology allows 2x to 3x the µL/min flow rates with all the same advantages as standard pressure capillary IC, resulting in low consumption of water (30 to 40 mL/d of water) and low waste generation. In capillary IC, the system can remain on without loss in resources, i.e., capillary IC is always on and ready for analysis. These advantages result in: 1. Greater ease-of-use, 2. Longer eluent generator cartridge life, 3. Lower cost of ownership. Additionally, the increase in mass sensitivity, comparable results are achieved as with standard bore system using a sample injection of only 0.4 µL. In this study, inorganic anions and organic acids from a diluted orange juice sample are separated by anion-exchange chromatography on a capillary size Thermo Scientific Dionex IonSwift MAX-100 monolith IC column. The IonSwift MAX-100 column is designed with a monolith backbone and optimized with Dionex IonPac AS11 anion-exchange chemistry. This column was selected for these high pressure cap IC experiments because of the high efficiency and high flow rate characteristics.

"Green" and Ultrafast Method for Determination of Soft Drink Ingredients on the Acclaim C18 RSLC Column

2010-02-17T08:54:52.567

Soft drinks are beverages consumed widely throughout the world. For quality control, the additive levels in soft drinks must be assayed frequently. This method uses an Acclaim RSLC rapid separation column to improve the throughput to about 20 samples/h (or 2.6 min/sample). To avoid the use of toxic solvents, acetonitrile has been replaced by ethanol. To reduce the solvent viscosity and column pressure, the column is heated to 50 °C. Wavelength switching (changes from 230 nm to 214 nm at 0.3 minutes) suppresses interferences near acesulfame-K. This example shows the separation of 7 components in a standard mixture.

Peptide Map of Ovalbumin on Acclaim PolarAdvantage II (PA2)

2010-02-18T13:42:56.157

AN221: Rapid Determination of Melamine in Liquid Milk and Milk Powder by HPLC on the Acclaim Mixed-Mode WCX-1 Column with UV Detection

2010-02-16T10:59:08.577

Melamine is a chemical used in some plastics and fertilizer products. Recent investigations of death and health problems of babies in China have revealed that some baby foods (milk powder) have been contaminated by melamine. In this Application Note (AN), a simple HPLC method for rapid analysis of melamine in both liquid milk and milk powder samples is developed. The separation is performed on the Acclaim® Mixed-Mode WCX-1 column7 and UltiMate® 3000 HPLC system with UV detection using an acetate buffer and acetonitrile mobile phase. The sample analysis is completed within 10 min. The Acclaim Mixed-Mode WCX-1 column features a new mixed-mode silica-based packing material that incorporates both hydrophobic and weak cation-exchange properties, and demonstrates great potential for separating samples that contain a mixture of ionic and neutral compounds. Using an Acclaim Mixed Mode WCX-1 column with an UltiMate 3000 system allows a fast analysis of both liquid and powdered milk for melamine.

Ultrafast Analysis of Various Pharmaceutical Compounds by Charged Aerosol Detection (CAD) and an Inverse Gradient

2010-02-15T09:34:19.327

The FDA requires that a cleaning process be documented for all critical equipment used in the development of pharmaceutical products. This process involves defining objectives for the cleaning procedures, determining effectiveness of cleaning techniques, defining sampling techniques, qualifying analytical equipment, establishing acceptable limits, and testing controls. A common technique is HPLC with low wavelength UV detection. However, the shortfall of this technique is that many of the ingredients in cleaning products contain very weak chromophores. This leads to little or no sensitivity for this group of potential contaminants. Another difficulty often encountered using a specific technique like HPLC-UV is the quantification of unknown peaks. The need for fast turnaround time of the cleaned equipment to maintain production schedule does not allow for identification of every peak present. Therefore, quantitation by UV detection is often based solely on peak area. Since the UV response of an aromatic active ingredient would be different than a nonaromatic surfactant, such as dodecylsulfate, this presents a potential source of error. The Corona® CAD detector is mass sensitive and can be added to the traditional HPLC-UV platform. This detector provides the most consistent response, across nonvolatile and some semivolatile analytes, of all HPLC detection techniques. With all aerosol-based detectors, nebulization efficiency is often increased as the organic solvent proportion increases. When running gradients from high aqueous to high organic, CAD response increases. The delivery of a second postcolumn solvent stream, which is inverted in composition relative to the elution gradient, enables a constant proportion of organic solvent to reach the detector and results in more uniform response factors. The focus of this application is to demonstrate an inverse-gradient approach for the analysis of the APIs, potential degradants, byproducts, and residual cleaning products on a single UHPLC platform.

Fast Analysis of Inorganic Cations in Diet Coke with Capillary ICS-5000

2011-11-30T14:44:20.53

One of the important applications of ion chromatography is to determine inorganic cations in beverages. Here shows an example of separating common inorganic cations in diet coke within 7 minutes using capillary ICS-5000 and capillary column IonPac CS16. The flow rate utilized in this application was 0.03 mL/min and the isocratic MSA eluent was generated by ICS-5000 EG. At this flow rate, about 2100 psi backpressure was generated.

Fast Analysis of Inorganic Anions in Richmond Municipal Drinking Water

2012-01-05T12:25:09.61

Standard length 250 mm format of IonPac AS18 analytical column has an advantage of allowing larger injections of more concentrated and higher ionic strength matrix samples without dilution. AS18 high capacity analytical columns also provides new ways to achieve improved resolution of critical pairs with faster separations. All analysts of interests in Richmond municipal drinking water were baseline resolved within 8 min at increased flow rate of 0.40 mL/min. The run time was reduced from 15 min to 8 min with good baseline resolution. The fast analysis of common anions in Richmond municipal waters samples by using 250 mm column emphasizes the fast sample runs and higher resolution possible with high capacity column.

Monosaccharides in Cranberry-Rasberry Juice by Capillary HPAE-PAD

2010-11-21T21:28:18.047

CAP PA20 Cranberry-Rasberry Juice. Fruit juices have characteristic proportions of monosaccharides. These monosaccharide characteristics are used to whether the cranberry-rasberry juice has been adulterated with a lower cost juice. In this application monosaccharides were determined in a diluted cranberry-rasberry juice sample using a capillary ICS-5000 system and high performance anion-exchange chromatography with pulsed amperometric detection (HPAE-PAD). Glucose, fructose, and sucrose were separated on a capillary CarboPac PA20 column using electrolytically generated 50 mM KOH eluent.

Melamine and Cyanuric Acid on Acclaim Mixed-Mode WAX-1

2010-03-01T15:47:38.887

Capillary Scale UHPLC Peptide Mapping of a Monoclonal Antibody (MAb)

2011-04-26T05:39:52.78

Peptide mapping of MAb samples is a mandatory analysis in MAb drug development. The techniques applied are very similar to proteomics; digestion of the protein and analysis of the digest by LC-MS/MS. However, data quality needs to be much higher to get (close to) 100% sequence coverage and mapping of modification sites. Using the NCP-3200RS with a capillary scale UHPLC column will provide maximum separation performance and can be easily interfaced with state-of-the-art mass spectrometry.

Counter Anions in a Metformin HCL tablet by High Pressure Cap IC

2011-12-11T16:44:10.827

Counter Anions in a Metformin HCL tablet by High Pressure Cap IC using the ICS-5000 high pressure capillary system. High Pressure Capillary Reagent-Free™ ion chromatography (RFIC™) is the latest advancement in ion chromatography instrumentation. Typically with an RFIC system, the system pressure is limited to <3000 psi because of the limitations of materials in the RFIC accessories. Now with the upgrade to high pressure, the ICS-5000 IC capillary system can operate at system pressures <5000 psi. This advance in technology allows 2x to 3x the µL/min flow rates with all the same advantages as standard pressure capillary IC, resulting in low consumption of water (30 to 40 mL/d of water) and low waste generation. In capillary IC, the system can remain on without loss in resources, i.e., capillary IC is always on and ready for analysis. These advantages result in: 1. Greater ease-of-use, 2. Longer eluent generator cartridge life, 3. Lower cost of ownership. Additionally, the increase in mass sensitivity, comparable results are achieved as with standard bore system using a sample injection of only 0.4 µL. In this study, inorganic anions from a pharmaceutical tablet sample are separated by anion-exchange chromatography on a capillary size Thermo Scientific Dionex IonSwift MAX-100 monolith IC column. The IonSwift MAX-100 column is designed with a monolith backbone and optimized with Dionex IonPac AS11 anion-exchange chemistry. This column was selected for these high pressure cap IC experiments because of the high efficiency and high flow rate characteristics.

Analysis of Aromatic Hydrocarbons by UHPLC using Phenyl Column

2011-02-25T00:34:10.61

This application separates 5 aromatic hydrocarbons in less than 6 minutes. It was run on an UltiMate 3000 RSLC system and used the Dionex Acclaim Phenyl column.

Analysis of Tinuvin 622 by HPLC and Charged Aerosol Detection

2010-12-17T12:04:52.733

This method was used to determine a number of Hindered Amine Light Stabiliser (HALS) compounds by RP-HPLC and the Corona ultra charged aerosol detector. A post-column acid solvent is added to lower background for CAD. Here, chromatography of a polymeric HALS, Tinuvin 622, is presented. A dynamic range of 3 to 50 µg o.c and an LOD of 650 ng o.c. was found.

Fast Anion Determinations in a UK Drinking Water Sample

2010-11-14T13:45:43.563

AS22 Fast Initial. Anions were determined in an UK drinking water sample within 5 min on IonPac AS22 Fast column using carbonate eluents. An ICS-1100 system was used for the analysis. This application is for customers who prefer using carbonate eluents.

"Green" and Ultrafast Method for Determination of Soft Drink Ingredients on the Acclaim C18 RSLC Column

2010-02-17T09:08:06.467

Anions and Organic Acids in Pomegranet-Grape Juice by High Pressure Capillary IC

2011-12-11T19:21:48.89

Anions and Organic Acids in Pomegranet-Grape Juice by High Pressure Capillary IC High Pressure Capillary Reagent-Free™ ion chromatography (RFIC™) is the latest advancement in ion chromatography instrumentation. Typically with an RFIC system, the system pressure is limited to <3000 psi because of the limitations of materials in the RFIC accessories. Now with the upgrade to high pressure, the ICS-5000 IC capillary system can operate at system pressures <5000 psi. This advance in technology allows 2x to 3x the µL/min flow rates with all the same advantages as standard pressure capillary IC, resulting in low consumption of water (30 to 40 mL/d of water) and low waste generation. In capillary IC, the system can remain on without loss in resources, i.e., capillary IC is always on and ready for analysis. These advantages result in: 1. Greater ease-of-use, 2. Longer eluent generator cartridge life, 3. Lower cost of ownership. Additionally, the increase in mass sensitivity, comparable results are achieved as with standard bore system using a sample injection of only 0.4 µL. In this study, inorganic anions and organic acids from a diluted pomegranet-grape juice sample are separated by anion-exchange chromatography on a capillary size Thermo Scientific Dionex IonSwift MAX-100 monolith IC column. The IonSwift MAX-100 column is designed with a monolith backbone and optimized with Dionex IonPac AS11 anion-exchange chemistry. This column was selected for these high pressure cap IC experiments because of the high efficiency and high flow rate characteristics.

AU172: Determination of Polyphosphates Using Ion Chromatography

2010-06-10T04:57:24.517

This application update briefly compares the performance of the IonPac AS16 column with hydroxide eluents prepared by the eluent generator to manually prepared hydroxide eluents and discusses the value of each approach. The method was applied to the determination of polyphosphates in a sausage sample and in a sodium hexametaphosphate powder. The combination of a high-capacity AS16 column, a hydroxide eluent, and suppressed conductivity detection delivers sensitive high-resolution separations and accurate determination of polyphosphates.

Determination of Anions and Organic acids in a Low Carbohydrate Sports Beverage by Capillary IC

2011-04-14T17:40:46.127

Anions and organic acids are important part of the flavor experienced by drinking a carbonated beverage. Additionally, some anions are acidulants or preservatives used to maintain the intended flavor and inhibit biological contamination, known commonly as "spoiling". In this application, anions and organic acids in a low carbohydrate sports beverage are determined by capillary IC and suppressed conductivity on the ICS-5000 capillary IC system.

Antibiotics in aqueous environmental matrices

2010-03-02T10:03:37.85

The use of antibiotics on livestock, aquaculture, and bee husbandry helps maintain health and provides other benefits such as improved disease resistance, increased production, and in some cases, reduction in foodborne pathogens. However, antibiotic residues in foods can cause undesirable side effects such as idiosyncratic aplastic anemia, production of antibiotic-resistant bacteria,and the reduction of indigenous microbiota found in the human digestive tract. In addition, the wastes of these animals can lead to antibiotics being present in our water. Organizations responsible for food safety perform assays for the presence of allowed and banned antibiotics as part of their surveillance activities. This application is part of a study for the analysis of antibiotics in aqueous environmental matrices on the Acclaim 2.2 µm C18 (2.1 x 100 mm) column.

Fast Determination of Anions in San Jose Municipal Wastewater

2011-06-22T10:26:10.017

Common inorganic anions in San Jose municipal wastewater were analyzed using IonPac AS18 Fast column.

Monosaccharides in Orange Juice by Capillary HPAE-PAD

2010-11-21T20:47:00.017

Cap PA20--Orange Juice. Fruit juices have characteristic proportions of monosaccharides. These monosaccharide characteristics are used to whether the juice has been adulterated with a lower cost juice. In this application monosaccharides were determined in a diluted orange juice sample using a capillary ICS-5000 system and high performance anion-exchange chromatography with pulsed amperometric detection (HPAE-PAD). Glucose, fructose, and sucrose were separated on a capillary CarboPac PA20 column using electrolytically generated 50 mM KOH eluent.

Fast Analysis of Inorganic Cations in Municipal Wastewater by Capillary Ion Chromatography

2011-12-01T14:59:25.377

Ion chromatography is a great technique to determine inorganic cations in water sample. Here show an example of separating common cations in less than 7 minutes using capillary ICS-5000 and IonPac CS16 column. The analytes were eluted with isocratic 30 mM MSA, electrolytically generated by ICS-5000 EG.

Recovery of Nitrofuran Antibiotics from Pet Food on Acclaim® 120 C18 RSLC

2010-02-15T12:58:34.957

Nitrofuran antibiotics are now banned from use in many parts of the world, making it necessary to monitor for illegal or accidental contamination of animal feeds. The Acclaim 120 C18 RSLC column will resolve these four common drugs easily even in a complex feed matrix. The 2 µm RSLC technology now lets this analysis be finished in only 2 minutes.

Oxyhalides determinations in UK municipal drinking water by Cap IC

2011-12-11T19:46:16.953

Oxyhalides determinations in UK municipal drinking water by Cap IC Using Standard Flow Rates High Pressure Capillary Reagent-Free™ ion chromatography (RFIC™) is the latest advancement in ion chromatography instrumentation. Typically with an RFIC system, the system pressure is limited to <3000 psi because of the limitations of materials in the RFIC accessories. Now with the upgrade to high pressure, the ICS-5000 IC capillary system can operate at system pressures <5000 psi. This advance in technology allows 2x to 3x the µL/min flow rates with all the same advantages as standard pressure capillary IC, resulting in low consumption of water (30 to 40 mL/d of water) and low waste generation. In capillary IC, the system can remain on without loss in resources, i.e., capillary IC is always on and ready for analysis. These advantages result in: 1. Greater ease-of-use, 2. Longer eluent generator cartridge life, 3. Lower cost of ownership. Additionally, the increase in mass sensitivity, comparable results are achieved as with standard bore system using a sample injection of only 0.4 µL. In this study, inorganic anions from a municipal drinking water sample are separated by anion-exchange chromatography on a capillary size Thermo Scientific Dionex IonSwift MAX-200 monolith IC column. The IonSwift MAX-200 column is designed with a monolith backbone and optimized with Dionex IonPac AS19 anion-exchange chemistry. This column was selected for these high pressure cap IC experiments because of the high efficiency and high flow rate characteristics.