The thermospray liquid chromatography/mass spectrometry (LC/MS) interface has had a major impact on the direct analysis of the metabolic fate of xenobiotics in complex biological media. This paper outlines the rapidity and power of the LC/MS approach, and shows how detailed structural information can be obtained without recourse to individual compound isolation. This provides a great saving in time and effort. The additional specificity of liquid chromatography/tandem mass spectrometry is highlighted in identifying the sites of metabolic transformation. The ability to handle biological samples with little or no clean-up using wide high-performance liquid chromatographic gradients is a key feature of the success of this methodology.
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http://dx.doi.org/10.1002/bms.1200180822 | DOI Listing |
Food Chem
March 2021
Departamento de Química, Universidade Estadual de Londrina (UEL), Rod. Celso Garcia Cid, PR 445 Km 380, Campus Universitário, Londrina, PR CEP 86051-990, Brazil; Instituto Nacional de Ciência e Tecnologia (INCT) de Bioanalítica, Universidade Estadual de Campinas (UNICAMP), Instituto de Química, Departamento de Química Analítica, Cidade Universitária Zeferino Vaz s/n, Campinas, SP CEP 13083-970, Brazil. Electronic address:
This study describes the development of a new analytical method for cadmium determination in flaxseed flour based on ultrasound-assisted extraction combined with supramolecular preconcentration followed by thermospray flame furnace atomic absorption spectrometry. Cadmium from flaxseed flour was extracted by ultrasound-assisted radiation in acid medium (1.5 mol LHNO) followed by liquid-liquid microextraction of the acid extractwith dodecanoic acid/THF supramolecular solvent using diethyl dithiophosphate as a chelating agent.
View Article and Find Full Text PDFAnal Chim Acta
July 2015
Wildlife and Landscape Science Directorate, Science and Technology Branch, Environment Canada, National Wildlife Research Centre, Carleton University, 1125, Colonel By Dr. (Raven Road), Ottawa, ON K1A 0H3, Canada. Electronic address:
A fast, robust and highly sensitive analysis method for determination of trace levels of organophosphate ester (OPE) flame retardants and plasticizers in lipid-rich samples was presently developed, and based on ultra-high performance liquid chromatography-tandem mass spectrometry coupled to a positive atmospheric pressure chemical ionization source (UHPLC-MS/MS-APCI(+)). The target OPEs in the sample were extracted from the biota samples, such as egg and liver, by ultrasonic extraction, and cleaned up further by dispersive solid phase extraction (d-ESP). As a result, background contamination was largely reduced.
View Article and Find Full Text PDFAnal Chem
March 2015
†Arthur Amos Noyes Laboratory of Chemical Physics, California Institute of Technology, Pasadena, California 91125, United States.
The complex chemistry occurring at the interface between liquid and vapor phases contributes significantly to the dynamics and evolution of numerous chemical systems of interest, ranging from damage to the human lung surfactant layer to the aging of atmospheric aerosols. This work presents two methodologies to eject droplets from a liquid water surface and analyze them via mass spectrometry. In bursting bubble ionization (BBI), droplet ejection is achieved via the formation of a jet following bubble rupture at the surface of a liquid to yield 250 μm diameter droplets (10 nL volume).
View Article and Find Full Text PDFBioanalysis
August 2015
DMPK, UCB, 216 Bath Road, Slough, Berks SL1 3WE, UK.
After graduating with an Oceanography degree from Swansea University, Lloyd has spent over 20 years in the field of bioanalysis and metabolite profiling. He started his career in large pharma at Wyeth UK, where he was involved in setting up the first GC and LC-MS/MS systems for both QC and early DMPK assays, employing EI/CI, thermospray, and the then new electrospray ionization techniques. Lloyd then joined Celltech, now UCB, where he is primarily tasked with metabolite profiling by LC-MS and NMR to support both early research projects and late-stage clinical studies.
View Article and Find Full Text PDFJ Anal Toxicol
June 2014
1Department of Forensic and Analytical Science, King's College London, London, UK.
Most antidoping method development in the equine industry has been for plasma and urine, though there has been recent interest in the analysis of synovial fluid for evidence of doping by intra-articular corticosteroid injection. Published methods for corticosteroid analysis in synovial fluid are primarily singleplex methods, do not screen for all corticosteroids of interest and are not adequately sensitive. The purpose of this study is to develop a rapid and sensitive liquid chromatography-tandem mass spectrometry (LC-MS-MS) screening method for the detection of four of the most common intra-articularly administered corticosteroids--betamethasone, methylprednisolone, methylprednisolone acetate and triamcinolone acetonide.
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