Drug Fingerprinting via Unique HPLC/MS Salt Forms Method
Thermo Fisher Scientific, Inc announced that it has developed a comprehensive method for the identification, confirmation and quantitation of illicit drugs and their salt forms. This unique method combines high-performance liquid chromatography with mass spectrometry (HPLC/MS) to provide accurate simultaneous separation and detection of cations and anions in illicit drug salt forms. The technique enables drug salt forms to be precisely identified and confirmed by two independent parameters - retention time and mass spectral signature, allowing forensic drug chemists to reliably analyse seized materials. The method also enables pharmaceutical drug QA/QC analysts to determine counterfeit drugs and describe drug efficacy.
The World Drugs Report 2009 states that between 172 and 250 million people worldwide used illicit drugs at least once in 2007, with 18–38 million estimated to be heavy drug users. The illicit drug trade fuels crime and violence and inappropriate and extended use of any of these drugs can lead to devastating health outcomes. Illicit drugs are often encountered in the form of salts and identification of the specific counterion present may provide valuable information about the source of production and the manufacturing pathway. As a result, techniques to accurately screen and identify drugs, drug precursors and new drug derivatives are crucial to law enforcement efforts to curb the black market in controlled substances.
The new Thermo Scientific HPLC/MS method is a powerful alternative to other techniques currently being used to analyse illicit drugs and their salt forms. This method enables simultaneous determination of cations and anions with exceptional sensitivity, detection and accurate identification of a wider range of compounds without requiring derivitisation, which in turn provides simultaneous qualitative and quantitative information on drug salt forms.
In this method, HPLC/MS analysis is performed on a Thermo Scientific Accela UHPLC system coupled to a Thermo Scientific MSQ Plus Mass Detector, a sensitive and fast scanning single quadrupole mass spectrometer. The Accela™ UHPLC system offers the flexibility of performing both conventional and high-speed LC separations on a single platform, while the rapid polarity switching capability of the MSQ™ Plus Mass Detector, together with its operational mass range, enables simultaneous detection of cations and anions in a single analysis.
Circle no. 51
Refurbished MS/LCMS Systems and MS Workstations with Optional Pump Noise Reduction
KRSS is the UK’s fastest growing mass spectrometry service organisation, employing experienced engineers with many years knowledge of mass spec service. The team at KRSS work with customers to offer competitively priced service options which minimise instrument downtime, maximise sample throughput and ensure quality results are delivered on time. Quality spare parts support all LCMS and GCMS service agreements. This provides customers with peace of mind, ensuring results are not compromised. Refurbished LCMS and UHplc MS systems are offered at affordable prices with warranty - each unit is serviced and validated prior to installation.
Custom built LC and MS workstations available with or without inbuilt MS pump noise reduction, along with the new MS-QuietBox II for single or double pump noise reduction.
Comprehensive LCMS and GCMS service support and instrument sales specialist; specialised support for Micromass/Waters, ABI/Sciex, Thermo and Agilent Mass Spectrometers; all inclusive, preventative maintenance, callout paid contracts, IQ/OQ and custom packages available; service and repair of CTC autosamplers, Hplc & GC’s; decommissioning, relocation and installation options; Maldi MS service & laser replacement; and MS workstations with pump noise reduction.
Circle no. 52
Analysis of Perfluorinated Compounds in Human Breast Milk
Thermo Fisher Scientific Inc has developed a new method for sensitive, accurate and reproducible quantitation of low levels of perfluorinated compounds (PFCs) in human breast milk. Using selected reaction monitoring (SRM) and highly selective reaction monitoring (H-SRM) on an integrated ultra high performance liquid chromatography mass spectrometry (UHPLC/MS) platform enables reliable and robust detection of PFCs at ppt concentrations in human breast milk.
Many PFCs are detectable in human serum and breast milk and have been found in the blood of newborns possibly through lactational transfer from mothers. By coupling the Thermo Scientific Accela UHPLC and the PAL autosampler to the Thermo Scientific TSQ Vantage triple-stage quadrupole MS the system was able to provide rapid, accurate and robust analysis and quantitation of six PFCs in
human breast milk using SRM and H-SRM. Elimination of PFC contamination was achieved using a PFC-free Accela pump with a pre-cleaned PFC-free degasser, while also replacing Teflon tubing with PEEK tubing. The excellent sensitivity and selectivity afforded by SRM on the TSQ Vantage system obviated the need for any further modifications of the LC configuration, a distinct advantage over other commercial platforms that require the use of in-line contaminant traps or column-switching methods for PFC analysis.
Using the integrated UHPLC/MS platform, separation of the six PFC analytes in a spiked human breast milk matrix was achieved within nine minutes. As the majority of interferences from matrices elute early at void volume, elution of the first compound at 3.64 minutes ensured a robust quantitation method. Excellent linearity in detector response was observed while H-SRM eliminated matrix interferences without compromising sensitivity.
The Accela system, combined with 1.9 µm particle columns and the industry’s highest pressure quaternary pump, enables fast and efficient chromatographic separations over an expansive range of flow rates and pressures. Delivering up to a tenfold improvement in signal-to-noise ratio compared to existing triple-quadrupole MS systems, The TSQ Vantage facilitates highly sensitive quantitation in matrix-rich samples and enhances analytical precision. The instrument is capable of high resolution selection of precursor ions, enabling H-SRM for greater analytical selectivity and accuracy.
Circle no. 53
Protein Standards for Mass Spectrometry Analysis
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Amsbio has announced a new service whereby it can generate high quality Mass Spectrometry (MS) standards for over 5,000 human proteins. Produced in human HEK293T cells and labelled with [U- 13C6, 15N4]-L-Arginine and [U- 13C6, 15N2]-L-Lysine, the full-length proteins with appropriate post-translational modifications are the best choice for accurate identification and quantification of protein
biomarkers.Amsbio offers stable isotope-labelled full-length protein standards for both matrix-assisted laser desorption/ionisation (MALDI) and electrospray ionisation (ESI) Mass Spectrometers enabling researchers to identify the best SRM and MRM transitions through experimental data.
The MS standards commercialised by Amsbio allow researchers to spike at an early stage of sample processing enabling accurate quantification. Produced in human HEK293T cell line the protein MS standards have authentic post-translational modifications with greater than 90% stable isotope labelling incorporation efficiency. As a consequence researchers are able to gain higher data consistency than by using synthetic peptide internal standards.
Circle no. 54
Mass Spectrometry Focus
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