Letcher R J, Li H X, Chu S G
Great Lakes Institute for Environmental Research, University of Windsor, Windsor, Ontario, Canada N9B 3P4.
J Anal Toxicol. 2005 May-Jun;29(4):209-16. doi: 10.1093/jat/29.4.209.
Hydroxylated metabolites of polychlorinated biphenyls (HO-PCBs) and pentachlorophenol (PCP) are halogenated phenolic compounds, and they are increasingly common as environmental contaminants mainly in the blood of wildlife and humans. A methodology based on high-performance liquid chromatography (reversed-phase)-electrospray (negative) ionization-tandem quadrupole mass spectrometry (LC-ESI(-)-MS-MS) in the select ion monitoring or multiple reaction monitoring modes was developed for HO-PCB and PCP determination in blood plasma and serum. Among 11 environmentally relevant HO-PCB congeners and PCP spiked to fetal calf serum, quantitative assessments, including matrix effects on ESI(-) suppression/ enhancement, showed process (recovery) efficiencies of 73% to 89% without internal standard (IS) correction, and 88% to 103% with IS correction, and method limits of quantification ranging from 1 to 50 pg/g (wet weight). Using the developed LC-ESI(-)-MS methodology in comparison with GC-MS and GC-ECD based approaches, similar results were found for HO-PCB identification and quantification in the plasma of polar bear (Ursus maritimus) from the Canadian arctic. LC-ESI(-)-MS identified four HO-PCB congeners [4'-HO-2,2',4,6,6'-pentachlorobiphenyl (4'-HO-CB104), 4-HO-2,3,3',4',5-pentachlorobiphenyl (4-HO-CB107), 4-HO-2,3,3',5,5',6-hexachlorobiphenyl (4-HO-CB165) and 3'-HO-2,2',3,4,4',5,5'-heptachlorobiphenyl (3'-HO-CB180)], and 14 additional tetra- to hepta-chlorinated HO-PCBs isomers in the polar bear plasma.
多氯联苯(HO-PCBs)和五氯苯酚(PCP)的羟基化代谢产物是卤代酚类化合物,作为环境污染物,它们在野生动物和人类血液中越来越常见。本文建立了一种基于高效液相色谱(反相)-电喷雾(负离子)电离-串联四极杆质谱(LC-ESI(-)-MS-MS)的方法,用于在选择离子监测或多反应监测模式下测定血浆和血清中的HO-PCBs和PCP。在添加到胎牛血清中的11种与环境相关的HO-PCB同系物和PCP中,定量评估(包括基质对ESI(-)抑制/增强的影响)显示,在无内标(IS)校正的情况下,方法回收率为73%至89%,在有IS校正的情况下,回收率为88%至103%,方法定量限为1至50 pg/g(湿重)。将所建立的LC-ESI(-)-MS方法与基于GC-MS和GC-ECD的方法进行比较,在加拿大北极地区北极熊(Ursus maritimus)血浆中HO-PCB的鉴定和定量方面得到了相似的结果。LC-ESI(-)-MS鉴定出北极熊血浆中的4种HO-PCB同系物[4'-羟基-2,2',4,6,6'-五氯联苯(4'-HO-CB104)、4-羟基-2,3,3',4',5-五氯联苯(4-HO-CB107)、4-羟基-2,3,3',5,5',6-六氯联苯(4-HO-CB165)和3'-羟基-2,2',3,4,4',5,5'-七氯联苯(3'-HO-CB180)],以及另外14种四至七氯代HO-PCB异构体。