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October 2012 Subscribe

Links to technical insights from sponsored Featured Application Notes on Chromatography Online.
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- Kate Mosford

Featured Application Note:
Plasma Free Metanephrines Quantitation with Automated Online Sample Preparation and Liquid Chromatography—Tandem Mass Spectrometry
Xiang He and Marta Kozak, Thermo Fisher Scientific

The development of an automated method to quantitate plasma free metanephrines is described. The method employs online sample preparation with the Thermo Scientific Transcend TLX-1 system to reduce analysis time while maintaining analytical performance comparable to the original offline SPE method.



Sample prep
Totally Automated Sample Extraction, Cleanup and Direct to Vial Concentration of PBDEs in Soil
Phil Bassignani, FMS, Inc.

PBDEs have been used in a wide array of products, including building materials, electronics, furnishings, motor vehicles, airplanes, plastics, polyurethane foams, and textiles. The health hazards of these chemicals have attracted increasing scrutiny, and they have been shown to reduce fertility and linked to other toxicities in humans. The sample prep process for PBDEs has been shown to be particularly difficult when done manually due to outside contamination. This note shows how a totally automated closed system for sample extraction, cleanup, and concentration can lower the possibilities of sample contamination. For more information.
Method 523: Determination of Triazine Pesticides and their Degradates in Drinking Water by Gas Chromatography/Mass Spectrometry (GC/MS) Version 1.0
Don Shelly and Craig A Perman, UCT, Inc

Method 523 is rapidly completed using UCT EC523506 graphitized carbon cartridges. Samples are pH adjusted, dechlorinated with ammonium acetate then protected from microbial degradation with 2-chloroacetamide during collection. Analytes are extracted from a 250 mL sample using the 250 mg cartridges.
Extraction of a range of opiates and metabolites from human urine using ISOLUTE® SLE+ columns prior to GC-MS analysis
Rhys Jones, Dr. Lee Williams and Adam Senior, Biotage AB, Sweden

This application note demonstrates an effective, efficient and quick sample preparation protocol using ISOLUTE SLE+ For the clean-up and concentration of a wide range of opiates and metabolites from urine, prior to quantitative GC-MS analysis. Average recoveries of 70-99% were achieved with RSD’s less than 5 for all analytes.

HPLC

LC–MS-MS Analysis of Water Using Microflow HPLC Coupled to Mass Spectrometry
Jason Causon, AB SCIEX

Water testing is fundamental for ensuring both safety in our water supply for consumption and also for monitoring environmental safety. Ultimately, water testing requires ultra-sensitive instrumentation that can target very low levels of assorted compounds and contaminants. Microflow LC is an exciting new approach that improves both analysis sensitivity and sample throughput for water analysis using LC–MS-MS. This article outlines a study showing how microflow LC–MS-MS can be applied to quantify low level pesticides in water samples.

Hydrophilic Interaction Chromatography (HILIC) Using Agilent Poroshell 120 HILIC
William Long and Anne E. Mack, Agilent Technologies

Hydrophilic interaction chromatography (HILIC) has been gaining popularity in liquid chromatography particularly for its ability to retain and separate small polar analytes, an area where common reversed-phase chromatography methods often fail. Poroshell 120 is now available in HILIC, combining the time savings and high resolution advantages of Poroshell 120 with the advantages of HILIC mode. This note explores the technical aspects of Poroshell 120 HILIC and demonstrates results for several applications.

Targeted Proteomics using Skyline
Stephanie Kaspar, Pierre-Olivier Schmitt, Wolfgang Jabs, Carsten Baessmann, Brendan MacLean, Mike MacCoss, Bruker Daltonics GmbH

Mass spectrometry-based quantitative proteomics is a popular tool for protein biomarker candidate discovery and subsequent validation. With the maXis impact different targeted proteomics strategies can be followed of which the high resolution extracted ion chromatogram (HR-XIC) approach is described. Data processing was done using Skyline – a freely available software tool for targeted proteomics developed by the MacCoss lab (University of Washington).

Fast Simulation of Drug Metabolism Using Electrochemistry-MS
A. Kraj, H-J. Brouwer, M. Eysberg, and J-P. Chervet, Antec

For faster, better, and superior simulation of drug metabolism, Antec has developed a dedicated electrochemistry system, called ROXY™ EC. The system is used up-front MS and allows for the generation and screening of potential metabolites, mimicking P450 enzymatic reactions in a few seconds without any biological interferences.

Agilent 1290 Infinity LC — Which Applications Require the Ultra Low Dispersion Kit?
Sonja Schneider, Agilent Technologies

Improvements regarding peak width, peak capacity, and plate number were evaluated using the ULD Capillary Kit and the ULD Flow Cell for the Agilent 1290 Infinity LC.

Trace-level aliphatic amines in pharmaceutical ingredients
N. Harihara Subramanian, P. Manigandan, R. Ganeshjeevan, Ganga Radhakrishnan and A. Wille, Metrohm AG

The determination of low-molecular-weight aliphatic amines in interfering matrices is a challenging task because the protonated amines are often poorly retained on the column. This problem is met by applying coupled-column matrix elimination.

Analysis of Common Sweeteners and Additives in Beverages
Njies Pedjie, PerkinElmer ®, Inc.

The use of artificial sweeteners is regulated in most countries. In the U.S., artificial sweeteners are part of the generally recognized as safe (GRAS) ingredients. However, the FDA has established an acceptable daily intake (ADI) for all sweeteners. Therefore, manufacturers are required to list the type and amount of sweeteners on a food label. This application note presents a fast and robust liquid chromatography method to test widely used artificial sweeteners such as acesulfame potassium, saccharine, and aspartame.


GPC
Antibody Drug Conjugate Analysis
Wyatt Technology

There has been a significant resurgence in the development of antibody-drug conjugates (ADC) as target-directed therapeutic agents for cancer treatment. Among the factors critical to effective ADC design is the drug antibody ratio (DAR). The DAR describes the degree of drug addition, which directly impacts both potency and potential toxicity of the therapeutic, and can have significant effects on properties such as stability and aggregation. Determination of DAR is, therefore, of critical importance in the development of novel ADC therapeutics and this note shows how multiangle light scattering can help determine the DAR.

GC
Agilent J&W DB-624 Ultra Inert Capillary Column's Utility in Screening Distilled Spirits by GC/MS Static Headspace
Ken Lynam, Agilent Technologies

Small batch distillation of spirits is becoming an increasingly popular means of producing premium spirits that are finding a ready market for consumers with discriminating tastes. The inertness and selectivity of Agilent J&W DB-624UI make distilled spirit profiling by static headspace GC straightforward, with clear differences in fusel oils and related fermentation products between orange-flavored cognac and bourbon samples.

general
Chiesi and Waters Implement a Lean, Paperless Lab
Waters Corporation

Chiesi Ltd. selected a complete Waters Informatics solution, including NuGenesis SDMS, NuGenesis ELN, and Empower 3 Software, to implement a paperless lab that facilitates innovation and interpretation of data.
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