Application Note Alert

November 2011 Subscribe

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

Featured Application Note:
Automated Approach for Metabolite Identification Using Fragment Prediction in Combination with Fragment Ion Search (FISh)
By Janine Wank1, Winfried Wagner-Redeker1, Anthony Taylor2, Rose Herbold3, Paul-Gerhard Lassahn1 1Swiss BioAnalytics AG, Basel, Switzerland; 2Thermo Fisher Scientific, Reinach, Switzerland; 3Thermo Fisher Scientific, San Jose, CA, USA

Learn how to evaluate an automated workflow for metabolic profiling and structural elucidation by processing high-resolution, accurate mass data using Fragment Ion Search (FISh) processing tool in Thermo Scientific Mass Frontier 7.0 software.

LC/HPLC
Optimizing the Purification of a Chiral Compound Using an HPLC System
Gilson, Inc

Significant differences in the effectiveness and toxicity of drug enantiomers has led to the need for the separation of chiral drug candidates into their respective enantiomers. Semi-preparative and preparative chromatography has become a common tool for this separation. This application describes the chiral separation of trans-Stilbene oxide using a multi-purpose, benchtop, semi-prep to prep system capable of separating by normal-phase or reverse-phase HPLC at flow rates of up to 100mL/min.

Quantitation and Identification of Pesticides using LC-MS/MS with Scheduled MRM, Fast Polarity Switching, and MS/MS Library Searching
Andre Schreiber and Yun Yun Zou, AB SCIEX

The screening of food samples for a large number of pesticides can sometimes be technically difficult and time-consuming, and the number of compounds tested may often be limited by hardware and software capabilities. Here we present the analysis of a large number of pesticides in food samples using a QuEChERS extraction and HPLC separation using a polar-embedded C18 phase.

New UHPLC based Neurotransmitter Analyzer
H-J. Brouwer, N. Reinhoud, L. van Heerwaarden, Antec

For fast and sensitive Analysis of Neurotransmitters in microdialysates or brain tissue, Antec has developed a new UHPLC based ALEXYS® Analyzer with electrochemical detection (ECD). The system allows for the analysis of all relevant monoamines and metabolites in <5 minutes, GABA and Glu <15 min and Acetylcholine and Choline <10 minutes, with extraordinary detection limits in the sub nmole/L range.
Biomarker Discovery from Tissue using MALDI Imaging
Markus Meyer, Sandra Rauser, Axel Walch, Arnd Ingendoh, Detlev Suckau, Bruker Daltonics and and Institute of Pathology, Helmholtz-Zentrum Munich - German Research Center for Environmental Health, Bruker Daltonics

This study presents an integrated workflow for biomarker discovery and identification in a complete top-down proteomics strategy. The strategy includes tissue screening by MALDI imaging, and is using statistical tools to flag discriminatory proteins. Proteins are identified by ETD/PTR analysis. The breast cancer study presented here reveals a novel putative biomarker which may become relevant for therapeutic decision-making.
Enhancing sensitivities and peak capacities for UHPLC-MS fast gradient analyses when exploiting the properties of 2.6 µm core-shell columns
James Rudge, David Neville, Richard Houghton, Chris Message, and Jeremy Bierman, Phenomenex

When compared to 1.7 μm fully porous materials, the ultra-high efficiency and low backpressures provided by Kinetex core-shell 2.6 μm columns, provides users opportunities to go beyond what is traditionally accepted for UHPLC runs.
User-Defined Autosampler Injection Routines
Evert-Jan Sneekes, Dionex Products, now sold under the Thermo Scientific brand

This technical note describes how to create user-defined programs for three real life injection challenges: maximum injection without sample loss, large volume direct injection for nano LC, and how to incorporate a sample preparation step prior to injection.

LC/HPLC

LECO Pegasus® GC-HR-TOFMS: Characterization of Synthetic Cannabis
LECO Corporation; Saint Joseph, Michigan USA

LECO Pegasus GC-HR-TOFMS enables identification of unknown, new and emerging illegal compounds. Utilizing LECO’s Folded Flight Path™ (FFP™) technology, accurate mass data were acquired and data processed using the LECO ChromaTOF-HRT software.

Identification & Quantification of Wine Impurities by GC/MS
Gauriat-Desroy, Eric Phillips, Stacy Crain, Trisa Robarge, Thermo Fisher Scientific

By identifying maturation tracers and molecules commonly responsible for taste defects in wine, GC/MS augments expert opinion with objective and quantitative information. When using a SPME extraction method, GC/MS has the additional advantages of requiring very small sample sizes, a minimum of sample preparation, and rapid analysis of target molecules.

A comparison of the VOC content of Indian tobacco and UK tobacco by headspace–thermal desorption (HS–TD)
Lara Kelly, Paul Morris, Markes International Ltd

Dynamic headspace sampling using Markes’ HS5-TD™ system, followed by thermal desorption–GC/MS, was used to analyse the headspace profiles of unburnt tobacco originating from India and the UK. Thirty-eight compounds were found in the two samples, with the fragrance compounds added to the Indian tobacco being clearly identified. A key advantage of the system described is that it provides greater sensitivity than conventional static headspace methods, while the ability of Markes’ systems to handle the complexity and dynamic range of the components present in such samples is clearly demonstrated.


Sample Prep
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.

hyphenated
Analysis of Biogenic Amines in Food
Seiji Ito and Fumiya Nakata, Customer Support Center, Tosoh Corporation, Kanagawa, Japan, Tosoh Bioscience

Biogenic amines are present in protein-rich food such as fish, meat or milk. Their concentration increases during food decomposition. This application note demonstrates the analysis of six biogenic amines in 15 minutes under HILIC conditions using a TSKgel Amide-80 column without the need for a complex and time-consuming derivatization procedure.
API Purification Using LC with UV and MS Detection
Luke Roenneburg, Tim Hegeman, and Toni Hofhine, Gilson, Inc

Purification of active pharmaceutical ingredients (APIs) often yields high numbers of fractions, leading to a bottleneck of fractions to dry-down and subsequently analyze. UV-based fraction collection based on slope or threshold values offers some specificity and reduction in the number of fractions collected compared to basic time- or volume-based collection.

sampleprep
Automated Solid Phase Extraction and Concentration of Semi-Volatile Organic Compounds in Water
Phil Bassignani, FMS, Inc.

The following note was developed to demonstrate the benefits of automating EPA Method 525.2 using SPE cartridges, the FMS PowerPrep™ SPE and the FMS PowerVap™ Direct-to-Vial Concentration system. This one step method delivers rapid, consistent and reproducible extraction and concentration of semi volatile organic compounds in water samples for analysis by GC/MS.
Simplified Extraction and Rapid LC/MS/MS Analysis of Synthetic Cannabinoids from Urine using Strata™-X-Drug N Solid Phase Extraction (SPE) and Kinetex 2.6 µm PFP Core-Shell HPLC/UHPLC Columns
Michael Rummel, Matthew Trass Shahana Huq, jeff Layne, Sky Countryman, Phenomenex

The goal of this study was to develop a LC/MS/MS method for urinary synthetic cannabinoids for use in confirmational analysis. Because of the affinity of the Strata-X-Drug N SPE sorbent for synthetic cannabinoids, a rapid extraction procedure featuring a very strong wash was developed. The method also incorporates mass spectrometry polarity switching to achieve detection of the six synthetic cannabinoids. The Kinetex PFP core-shell HPLC/UHPLC column selectivity complimented the scheduled polarity switching by eluting the six compounds in the correct windows of polarity.

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