title: Fast determination of hydroxylated polychlorinated biphenyls in human plasma by online solid phase extraction coupled to liquid chromatography-tandem mass spectrometry.
abstract: 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 the determination of OH-PCBs require labor-intensive and long-time consuming sample preparation with several extraction, evaporation and cleanup procedures steps and, in some cases, derivatization prior to the analysis by gas or liquid chromatography-mass spectrometry (GC-MS or LC-MS). The present study developed and validated a novel, sensitive and high throughput online solid phase extraction (SPE) method coupled to LC-tandem mass spectrometry (MS/MS) for the separation and quantitation of relevant congeners of OH-PCBs in human plasma. The developed method presented limits of quantification (LOQ) ranging from 0.02 to 0.5 ng mL(-1) and extraction recoveries from 71 to 134% for all congeners, requiring small amount of sample (only 100 μL) and minimal sample preparation. In order to evaluate the applicability of the method, preliminary tests (N = 93) were conducted in plasma from individuals occupationally exposed to very high levels of PCBs in a German cohort. Penta-through hepta-chlorinated OH-PCBs were the predominant congeners in human plasma with concentrations up to 44.5 ng mL(-1), while lower chlorinated OH-PCBs were occasionally detected. In addition, a new PCB 28 metabolite has been synthesized and identified for the first time in human plasma and associations between OH-PCBs and their parent compounds in the studied cohort were also assessed.
authors: Institute for Occupational and Social Medicine, Medical Faculty, RWTH Aachen University, Pauwelsstrasse 30, 52074 Aachen, Germany. Electronic address: nsoaresquine@ukaachen.de.
authors: Natalia
authors: N
authors: Quinete
authors: Institute for Occupational and Social Medicine, Medical Faculty, RWTH Aachen University, Pauwelsstrasse 30, 52074 Aachen, Germany.
authors: Thomas
authors: T
authors: Kraus
authors: Max Planck Institute for Biophysical Chemistry, Facility for Synthetic Chemistry, Am Fassberg 11, 37077 Göttingen, Germany.
authors: Vladimir N
authors: VN
authors: Belov
authors: Institute for Occupational and Social Medicine, Medical Faculty, RWTH Aachen University, Pauwelsstrasse 30, 52074 Aachen, Germany.
authors: Christina
authors: C
authors: Aretz
authors: Institute for Occupational and Social Medicine, Medical Faculty, RWTH Aachen University, Pauwelsstrasse 30, 52074 Aachen, Germany.
authors: André
authors: A
authors: Esser
authors: Institute for Occupational and Social Medicine, Medical Faculty, RWTH Aachen University, Pauwelsstrasse 30, 52074 Aachen, Germany.
authors: Thomas
authors: T
authors: Schettgen
mesh_terms: D000328:Adult; D000368:Aged; D002853:Chromatography, Liquid / Q000191:economics / Q000379:methods*; D015331:Cohort Studies; D052244:Endocrine Disruptors / Q000097:blood* / Q000378:metabolism; D004785:Environmental Pollutants / Q000097:blood* / Q000378:metabolism; D005260:Female; D008401:Gas Chromatography-Mass Spectrometry / Q000191:economics / Q000379:methods; D006801:Humans; D006900:Hydroxylation; D057230:Limit of Detection; D008297:Male; D008875:Middle Aged; D011078:Polychlorinated Biphenyls / Q000097:blood* / Q000378:metabolism; D052616:Solid Phase Extraction / Q000191:economics / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000191:economics / Q000379:methods*
chemical_list: D052244:Endocrine Disruptors; D004785:Environmental Pollutants; C081766:2,4,4'-trichlorobiphenyl; D011078:Polychlorinated Biphenyls
keywords: Endocrine disruptor; Human plasma; Hydroxylated polychlorinated biphenyls; Liquid chromatography-tandem mass spectrometry; Occupational exposure; Polychlorinated biphenyl metabolism