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一种使用 SPE 和 HRGC/HRMS 快速筛选小量人血浆中《斯德哥尔摩公约》持久性有机污染物的方法。

A rapid method for screening of the Stockholm Convention POPs in small amounts of human plasma using SPE and HRGC/HRMS.

机构信息

MTM Research Centre, School of Science and Technology, Örebro University, SE-701 82 Örebro, Sweden.

出版信息

Chemosphere. 2012 Feb;86(7):747-53. doi: 10.1016/j.chemosphere.2011.11.006. Epub 2011 Dec 5.

DOI:10.1016/j.chemosphere.2011.11.006
PMID:22153485
Abstract

A rapid analytical screening method allowing simultaneous analysis of 23 persistent organic pollutants (POPs) in human plasma was developed. Sample preparation based on solid-phase extraction (SPE) with additional clean-up using small multilayer silica gel columns. SPE was performed using a custom made polystyrene-divinylbenzene sorbent for the extraction of chlorinated and brominated POPs. Special efforts to reduce sample volume and improve speed and efficiency of the analytical procedure were made. Determination of 16 polychlorinated biphenyls (PCBs), 5 organochlorine (OC) pesticides, octachlorinated dibenzo-p-dioxin (OCDD) and polybrominated diphenyl ether (BDE #47) in 0.5 mL human plasma was performed by using high resolution gas chromatography coupled to high resolution mass spectrometry (HRGC/HRMS). Recovery of POPs ranged between 46% and 110%, and reproducibility was below 25% relative standard deviation (RSD) for all target compounds, except for trans-nonachlor and OCDD, which were present only at low levels. Limits of detection (LOD) were for the PCBs between 0.8 and 117.7 pg mL(-1) plasma and for the OC pesticides between 5.9 and 89.1 pg mL(-1) plasma. The LOD for OCDD and BDE #47 were 1.4 pg mL(-1) plasma, and 9.2 pg mL(-1) plasma, respectively. The presented method was successfully applied to 1016 human plasma samples from an epidemiological study on cardiovascular disease.

摘要

建立了一种可同时分析人血浆中 23 种持久性有机污染物(POPs)的快速分析筛选方法。样品制备基于固相萃取(SPE),并用小多层硅胶柱进行额外的净化。SPE 使用一种定制的聚苯乙烯-二乙烯基苯吸附剂进行氯化和溴化 POPs 的萃取。特别努力减少样品体积,提高分析程序的速度和效率。使用高分辨率气相色谱-高分辨率质谱(HRGC/HRMS)测定 0.5 mL 人血浆中的 16 种多氯联苯(PCBs)、5 种有机氯(OC)农药、八氯二苯并对二恶英(OCDD)和多溴联苯醚(BDE #47)。POPs 的回收率在 46%至 110%之间,除了仅在低水平存在的反式-壬烷和 OCDD 外,所有目标化合物的重现性均低于 25%相对标准偏差(RSD)。检出限(LOD)对于 PCBs 在 0.8 至 117.7 pg mL(-1)血浆之间,对于 OC 农药在 5.9 至 89.1 pg mL(-1)血浆之间。OCDD 和 BDE #47 的 LOD 分别为 1.4 pg mL(-1)血浆和 9.2 pg mL(-1)血浆。所提出的方法成功应用于心血管疾病流行病学研究的 1016 个人血浆样本。

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