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气相色谱-质谱检测法测定人血清中平面和非平面多氯联苯:电子轰击还是电子捕获负离子化?

Determination of coplanar and non-coplanar polychlorinated biphenyls in human serum by gas chromatography with mass spectrometric detection: electron impact or electron-capture negative ionization?

作者信息

Turci Roberta, Bruno Franco, Minoia Claudio

机构信息

Laboratory of Environmental Hygiene and Industrial Toxicology, Salvatore Maugeri Foundation, Via A. Ferrata 8, 27100 Pavia, Italy.

出版信息

Rapid Commun Mass Spectrom. 2003;17(16):1881-8. doi: 10.1002/rcm.1129.

Abstract

A time- and cost-saving method for the congener-specific analysis of polychlorinated biphenyls (PCBs) in human serum has been developed and validated. After two fast extraction and clean-up steps, analyses were performed using gas chromatography coupled with mass spectrometry with single ion monitoring (GC/SIM-MS), either in electron impact (EI) or electron-capture negative ionization (ECNI) mode. For the determination of dioxin-like congeners, an improvement in EI-MS sensitivity is desirable and use of NI is thus preferred. The procedure was validated for 12 dioxin-like congeners by analyzing spiked samples on three different days and using (13)C(12)-labelled analogues as internal standards. When using an NCI source, the limit of quantification was assessed at 0.01 microg/L, except for PCBs #77 and #81, which cannot be reliably detected below 0.05 microg/L. For the lower chlorinated non-dioxin-like congeners, NI offers less selectivity because of limited fragmentation. Electron impact ionization and electron-capture negative ionization mode can therefore be considered to be complementary for the determination of PCB congeners in the general population.

摘要

已开发并验证了一种省时且经济的方法,用于对人血清中的多氯联苯(PCBs)进行同系物特异性分析。经过两步快速提取和净化步骤后,使用气相色谱-单离子监测质谱联用仪(GC/SIM-MS)进行分析,采用电子轰击(EI)或电子捕获负电离(ECNI)模式。对于二噁英类同系物的测定,提高EI-MS灵敏度是可取的,因此优先使用负电离模式。通过在三个不同日期分析加标样品并使用(13)C(12)标记的类似物作为内标,对12种二噁英类同系物的分析方法进行了验证。使用NCI源时,除了PCB #77和#81在低于0.05 μg/L时无法可靠检测外,定量限评估为0.01 μg/L。对于低氯代非二噁英类同系物,由于碎片化有限,负电离模式的选择性较低。因此,电子轰击电离和电子捕获负电离模式可被视为在一般人群中测定PCB同系物的互补方法。

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