Application Note Alert

October 2011 Subscribe

Links to technical insights from sponsored Featured Application Notes on Chromatography Online.
Contact Editor
- Janet Kelsey

Featured Application Note:
Targeted Screening of Drugs of Abuse by LC-MS/MS
By C. Gechtman, A. Masarin, S. Scurati, B. Duretz, P. Regulus

Screening of biological samples for drugs of abuse and their metabolites is the work of forensic toxicology laboratories. This note shows a rapid and accurate targeted screening method for 294 compounds in urine utilizing Timed SRMs and a data-dependent scan function that increases product ion sensitivity.

LC/HPLC

Single Column GC/MS Analysis of the 12 Polychlorinated Biphenyls (PCBs) Designated as Toxic by the World Health Organization (WHO)
Carl Sanchez, Sky Countryman, Phenomenex

Simplified GC/MS analysis by providing resolution of all 12 toxic congeners using one column: the Zebron ZB-5ms GC column. The phase utilizes a Si-Arylene bonded polymer that has been demonstrated to provide enhanced resolution of multi-aromatic compounds.

Analysis of Pesticides in Citrus Oil
Hans-Joachim Huebschmann, Charles Lyle, Eric Phillips, Thermo Fisher Scientific

The analysis of citrus oil for pesticide contamination holds specific challenges. Pesticides that are used on the citrus crop are concentrated along with the matrix in this oil. This application describes the analytical methodology for fast multi-residue determination using unique timed selected reaction monitoring (timed-SRM) capabilities.


LC/HPLC
Determination of Sudan Dyes in Chilli Oil
Xu Qun, Dionex Products, now sold under the Thermo Scientific brand

This application note describes an online solid-phase extraction method followed by 2-D HPLC separation to accurately determine Sudan dyes in chili oil. Sudan dyes are prohibited  in foods but are illegally used to color foods and food ingredients such as chilies, chili oil, curry paste, and spices.

Detection of Phthalate compounds by LC-MS/MS
Andre' Schreiber, Fanny Fu, Olivia Yang, Eric Wan, Long Gu, and Yves LeBlanc, AB SCIEX

Phthalates are widely used industrial chemicals, present in products ranging from building materials and adhesives to various household products and food containers.  Leaching of these compounds into food, beverage, and cosmetic products have produced a need for analytical methods that can reliably test for Phthalates with a high level of sensitivity, specificity, and reliability.  Here we present a new and unique method using AB SCIEX QTRAP 5500 MS system to detect 22 phthalate compounds with significant advantages over other techniques (particularly GC) including reduced sample preparation time, shorter analysis times, and better and overall more reliable quantitative results.

Citius LC-HR-TOFMS: xenobiotic metabolite identification
LECO Corporation; Saint Joseph, Michigan USA, LECO

Greater efficiency plus high resolution TOFMS technology for urinary metabolite identification is shown here using LECO’s Citius LC-HRT & ChromaTOF-HRT™ software.  Citius LC-HRT technology delivers qualitative and quantitative data from the same instrument and at the same time.


Sample Prep

Analysis of Engineering Polymers by GPC/SEC
Greg Saunders and Ben MacCreath, Agilent Technologies

Engineering polymers are particularly difficult to analyze – they are generally tough and difficult to dissolve, often requiring aggressive solvents and elevated temperatures. For these applications at high temperature, a high performance integrated GPC system, such as the Agilent PL-GPC 220 Integrated GPC/SEC System, is a necessity. The PL-GPC 220 has the highest temperature range of any system on the market. This application compendium shows the analysis of various types of engineering polymers and illustrates the conditions and equipment required.

Molecular Weight Determination of LMWH SEC/MALS vs. SEC/UV-RI
Wyatt Technology

Low-molecular-weight heparins (LMWHs) are obtained by fractionation or depolymerization of natural heparins. They are defined as having a mass-average molecular weight of less than 8000 and for which at least 60% of the total weight has a molecular mass less than 8000.
Analysis of Low Molecular Weight Resins and Prepolymers by GPC/SEC
Greg Saunders and Ben MacCreath, Agilent Technologies

This application compendium discusses the analysis of low molecular weight resins and highlights those columns best suited for their analysis. A series of example analyses illustrate the quality of data that may be obtained. Agilent produces GPC/SEC columns, standards and instruments that are ideally suited to the analysis of resins and low molecular weight prepolymers.

misc
Automated Solid Phase Extraction and Concentration of PAHs in Water
Phillip Bassignani, FMS, Inc.

Analytically, PAHs present challenges for testing labs. Their volatile nature can make them problematic to extract without loss using manual methods. This is especially true for the evaporation/concentration of sample extracts. The following procedure utilizes the FMS PowerPrep™ SPE extraction system in combination with the PowerVap™ concentrator to extract PAHs from water.

High capacity sample cleaning for pesticide residue analysis
Dr. Elmar Tepper and Dr. Silvia Marten, KNAUER, Germany

In this application note, a stationary phase commonly used for sample cleanup is compared with the new EuroClean GPC material regarding performance and suitability for environmental and food laboratories.

Comparing the MICROLAB600 to volumetric glassware and air displaicement pipettes
Amy Schneck, HAMILTON Bonaduz AG

Most analytical techniques including chromatography require sample dilution to provide accurate mearements, within the detection limits of the chemical detector used. Traditionally samples are preparedusing volumetric glassware and pipettes. In this study we demonstrate that the new MICROLAB 600 semi-automated diluter outperformances the traditional techniques: it saves time, reduces reagent consumption and minimizes user variation. while maintaining high accuracy and precision.
Robust bioanalysis of peptides with SPE/LC/MS/MS
Martin Sibum and Gerard Haak, Spark Holland

The Symbiosis system for SPE/LC/MS/MS has a number of features that make it the perfect tool to meet the analytical challenges of peptide analysis. An assay for a 5900 amu peptides in plasma is presented her as an example. Good validation results are shown for the 0.5-500 ng/ml range.
A Novel Sample Preparation Device for Improved Phospholipid Removal in Bioanalytical Assays
Jessalynn P. Wheaton, Erin E. Chambers, and Diane M. Diehl, Waters Corporation

Matrix effects are residual components of biological matrix that alter mass spectrometry response, decrease method robustness, add to method variability, and lead to poor limits of detection/quantification. A major source of matrix effects in plasma-based bioanalytical assays is residual phospholipids.
A Simple Approach to Fast and Practical Solid Phase Extraction (SPE) Method Development
Michael Rummel, Terrell Matthews, Phenomenex

Solid phase extraction is an effective technique for cleaning up and concentrating samples. In the following application note we outline a simple approach for solid phase extraction method development using Strata® and Strata™-X SPE sorbents.
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