作者: Natalia Quinete , Thomas Kraus , Vladimir N Belov , Christina Aretz , André Esser
DOI: 10.1016/J.ACA.2015.06.041
关键词: Chromatography 、 Derivatization 、 Liquid chromatography–mass spectrometry 、 Solid phase extraction 、 Extraction (chemistry) 、 Tandem mass spectrometry 、 Chemistry 、 Gas chromatography–mass spectrometry 、 Mass spectrometry 、 Sample preparation
摘要: Hydroxylated polychlorinated biphenyls (OH-PCBs) have been shown to be strongly retained in human blood causing endocrine-related toxicity, particularly on the thyroid system. Traditionally, analytical methods for determination of OH-PCBs require labor-intensive and long-time consuming sample preparation with several extraction, evaporation cleanup procedures steps and, some cases, derivatization prior analysis by gas or liquid chromatography-mass spectrometry (GC-MS LC-MS). The present study developed validated a novel, sensitive high throughput online solid phase extraction (SPE) method coupled LC-tandem mass (MS/MS) separation quantitation relevant congeners plasma. presented limits quantification (LOQ) ranging from 0.02 0.5 ng mL(-1) recoveries 71 134% all congeners, requiring small amount (only 100 μL) minimal preparation. In order evaluate applicability method, preliminary tests (N = 93) were conducted plasma individuals occupationally exposed very levels PCBs German cohort. Penta-through hepta-chlorinated predominant concentrations up 44.5 mL(-1), while lower chlorinated occasionally detected. addition, new PCB 28 metabolite has synthesized identified first time associations between their parent compounds studied cohort also assessed.