The Application Notebook-06-01-2010

The Application Notebook

Matrix Elimination — In-line Removal of Chloride using InGuard Ag and Na Cartridges

June 01, 2010

General

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In ion chromatography, the presence of a large amount of matrix ions makes quantification of the target ions difficult. Selective removal of matrix ions - matrix elimination - can be performed by treating a sample with a solid-phase extractant. Halides can be removed by precipitation with silver, which is present as a counterion in a cation-exchange resin. A subsequent treatment with a cation-trapping column removes residual dissolved silver ions.

Fast Analysis of Naproxen Sodium with the Acclaim Trinity P1 Column and Charged Aerosol Detection

June 01, 2010

Pharmaceutical

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The characterization of pharmaceutical salts is critical to the drug development process. Active Pharmaceutical Ingredient (API) salts influence the solubility, stability, and hygroscopicity of pharmaceuticals and affect the final drug formulation.

A Novel, Simplified Methodology for the Analysis of Biodiesel by HPLC

June 01, 2010

Industrial

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Biodiesel is generally produced by the transesterification of vegetable oil or animal fat with methanol. The triglycerides present in the feed oil (vegetable oil or animal fat) are reacted with methanol in the presence of KOH as the catalyst.

Call for Application Notes

June 01, 2010

Articles

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LCGC is planning to publish the next issue of The Application Notebook special supplement in September. The publication will include vendor application notes that describe techniques and applications of all forms of chromatography and capillary electrophoresis that are of immediate interest to users in industry, academia, and government. If your company is interested in participating in these special supplements, contact:

High Resolution Analysis of Compound Danshen (Salvia Miltrorrhiza) Dropping Pills Using Superficially Porous LC Columns

June 01, 2010

Pharmaceutical

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Danshen (Salvia miltiorrhizae) is widely used as a traditional Chinese medicine (TCM) and remedies containing Danshen are traditionally used to treat cardiac and vascular disorders. Danshen Dropping Pills are a compound preparation consisting of Danshen, notoginseng, borneol, and other components.

Alternate Dynamic Headspace GC–MS Method for Automotive Materials Instead of VDA-278 Thermal Desorption

June 01, 2010

Polymer

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Synthetic and natural materials are used in motor vehicles to provide appealing and safe vehicle interiors. The manufacturing process for these materials include volatile (VOC) and semi volatile organic compounds (SVOC), which are released into the interior of vehicles. These compounds produce that new smell, but also create fog on interior glass surfaces of the car and can cause health issues.

Enhancing Phosphotyrosine Proteome Coverage Using a Combined ETD and CID Approach on a LTQ Orbitrap XL ETD

June 01, 2010

Biological

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Collision-induced dissociation (CID) and electron transfer dissociation (ETD) are complementary mass spectrometric fragmentation techniques. We have used CID and ETD in different approaches to analyze tyrosine phosphorylation using a Thermo Scientific LTQ Orbitrap XL equipped with ETD.

Determination of Diethylene Glycol in Sorbitol Solutions Used for Pharmaceutical Formulations

June 01, 2010

Pharmaceutical

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Ingestion of DEG-adulterated glycerin excipients in pharmaceuticals and personal care products, such as toothpaste, mouth wash, and medicinal syrups has caused systemic alcohol intoxication, acidosis, and subsequent multi-organ failure that have led to hundreds of fatalities of children and adults (1). To help prevent future adulterations, the U.S. FDA requested that the U.S. Pharmacopeia (USP) revise the USP 32 NF 26 monograph to identify and quantify EG and DEG in sorbitol solutions at the maximum limit of 0.1%. The revised monograph (USP 33-NF 28) meets these criteria using GC-FID (2).

Effect of Heating on Molecular Weights of Chitosan

June 01, 2010

Pharmaceutical

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Heating is a common and essential requirement in most biopharmaceutical production methods. Chitosan is an amino polysaccharide obtained by alkaline deacetylation of naturally abundant chitin. It is known as a potentially beneficial material in many pharmaceutical applications such as tissue engineering, drug delivery, cell encapsulation, and medical devices.

Analysis of an Expanded Panel of Sympathomimetic Amines in Urine Using Single Quadrupole GC–MS

June 01, 2010

Pharmaceutical

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The United States Substance Abuse and Mental Health Services Administration (SAMHSA) released a revision to the Mandatory Guidelines for Federal Workplace Drug Testing Programs, scheduled to become effective May 1, 2010. As part of the new guidelines, multiple changes were made for the confirmation of amphetamine-class urine analysis.

Improving TOF Mass Resolution by Reducing Ion Detector Time Jitter

June 01, 2010

General

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The resolution of time of flight (TOF) mass spectrometers continues to improve and attributes of the instrument that once were considered inconsequential have risen in importance as the push to higher and higher resolution continues.

Determination of Lactose in Lactose-Free Milk Products

June 01, 2010

Food and Beverage

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Lactose, a major disaccharide found in milk products, is catabolized into glucose and galactose by the enzyme lactase. Lactose-intolerant individuals have a lactase deficiency; therefore lactose is not completely catabolized.

Analyzing Construction Product Emissions Using Novel Micro-Chamber Technology with Thermal Desorption–GC–MS

June 01, 2010

Industrial

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The release of certain chemicals from building products is of increasing concern due to their potential detrimental effect on human health and the environment; therefore, new regulations requiring the production of low emission materials are currently being implemented.

Analysis of Small Molecules with amaZon: Enhanced Sensitivity, Speed, and Dynamic Range

June 01, 2010

General

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The amaZon series is the next step in Bruker Daltonics' family of ion trap mass spectrometers. Incorporating a number of new innovations to Bruker's highly successful ion trap technology platforms, the amaZon series is a true leap forward in performance and reliability.

High Temperature Simulated Distillation: ASTM D 7169

June 01, 2010

Industrial

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Robust hardware and automated software are critical to method ASTM D7169. The Shimadzu GC-2010, equipped with an advanced flow controller, has proven to be reproducible and effective, and Shimadzu distillation GC software has achieved automation by integrating calibration, integration, calculation, and report functions.

Faster Analysis of Naproxen Tablets — Improvements on the USP Method

June 01, 2010

Pharmaceutical

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The costs associated with pharmaceutical testing are considerable and many lab managers are seeking ways to reduce costs by reducing solvent usage and improving productivity while still using the LC instruments in their lab.

Evaluation of the Gas-Liquid Separator in the Mass-Directed SFC Prep System with Open-Bed Collection

June 01, 2010

Pharmaceutical

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With many "blockbuster" drugs losing patent protection, there has been mounting pressure across the pharmaceutical industry to shorten the time to bring new chemical entities (NCEs) to market and reduce the overall cost. This requires concerted productivity improvement in many aspects of drug discovery and development by continuously adopting new enabling technologies.

Development of a High-Throughput LC–MS-MS Assay for 13 Commonly Prescribed Pain Management Drugs from Urine with Cleanup Using Solid Phase Extraction (SPE)

June 01, 2010

Pharmaceutical

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In pain management analysis, urine is often used as it is a copiously available bodily fluid that can be collected easily and used for analysis. Urine, however, can cause difficulties in analysis due to the variances in the endogenous nature of the urine matrix, which can impact the chromatographic separation and quantitation.

U.S. EPA Method 524.3 for Analysis of Volatile Organic Compounds (VOCs) in Finished Drinking Water

June 01, 2010

Environmental

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The U.S. EPA Office of Groundwater and Drinking Water released Method 524.3, "Measurement of Purgeable Organic Compounds in Water by Capillary Column Gas Chromatography/Mass Spectrometry, Version 1.0," in the Federal Register on August 3rd, 2009 (1, 2). This new method contains an updated list of 76 VOCs that includes fuel oxygenates and two emerging contaminants of interest.

Simultaneous UHPLC–MS Analyses of Explosive Compounds

June 01, 2010

General

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Explosive compounds are widely used in warfare, mining industries, terrorist attacks, and civil constructions. Explosive contaminated soils are mostly found on firing points, impact areas, and training ranges. The explosive contaminates in soil are possible sources for surface and ground water contaminations, posing environmental and public health risks due to the compounds' toxicity, carcinogenicity, and mutagenicity.

EDTA by Anion Exchange HPLC

June 01, 2010

Pharmaceutical

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Hamilton Company is best known for manufacturing precision fluid measuring products, including syringes for HPLC and GC. For the last 30 years Hamilton Company has manufactured HPLC resins and columns while developing separations for customers. Two of the separations are highlighted below.

High Resolution UHPLC Analysis of Naringin in Grapefruit Juice

June 01, 2010

Food and Beverage

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Grapefruit juice was analyzed by gradient UHPLC for naringin - a flavanoid that gives it its bitter taste. A ZORBAX Rapid Resolution HD (RRHD) StableBond-C18 2.1 x 150 mm, 1.8 µm column resolved over 60 peaks including naringin in 7 min, and was re-equilibrated in just 3 min by operating at a high flow rate (0.8 mL/min).

Identification and Quantification of Illegal Drugs and Benzodiazepines in Human Plasma by LC–MS-MS After Solid Phase Extraction (SPE)

June 01, 2010

Pharmaceutical

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The identification and quantification of drugs of abuse in blood (plasma, serum, whole blood) has become very common in the forensic medicine laboratory. Liquid-liquid extraction (LLE) has been traditionally used at a basic pH (pH = 9) for the extraction of amphetamines, cocaine and its metabolites, and opiates from blood.

Identifying Unexpected Environmental Contaminants with High-Resolution, Accurate Mass LC–MS-MS

June 01, 2010

Environmental

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This paper describes the use of the AB SCIEX TripleTOF 5600 LC–MS-MS system for the screening and identification of unexpected contaminants in lake water, demonstrating the value of high-resolution, accurate-mass data, and retrospective data processing for the identification of nontargeted compounds.

Extend UHPLC Column Lifetime with KrudKatcher Ultra In-Line Filters

June 01, 2010

General

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For many years, the use of guard columns has been advocated by column manufacturers and other experts to protect and extend column lifetime and performance of analytical columns from potential damage caused by the presence of chemical contaminants and microparticulates in the sample and mobile phase.

Planning a Busy Summer at LCGC

June 01, 2010

From the Publisher

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Traditionally, summer is a time when the worlds of lab research and business slow down to a large extent. If you work in academia, chances are many of your students have returned home for the summer and the teaching load has been reduce, while those of you working in private industry and research labs may see coworkers taking long-anticipated (and well-deserved) vacations.

Heparin Characterization

June 01, 2010

Pharmaceutical

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Heparin is well-known as an anticoagulant, antithrombotic drug. Chemically, it is a linear polysaccharide that is derived from animal tissues. For some time it has been known that heparin is not a homogeneous substance; rather, it is a heterogeneous mixture of molecules ranging in molar mass from less than 5,000 to more than 30,000 Daltons.