首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >A method for analysis of marker persistent organic pollutants in low-volume plasma and serum samples using 96-well plate solid phase extraction
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A method for analysis of marker persistent organic pollutants in low-volume plasma and serum samples using 96-well plate solid phase extraction

机译:使用96孔板固相萃取分析低体积血浆和血清样品中标记持续有机污染物的方法

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摘要

The objective of this study was to develop and validate a 96-well plate solid phase extraction method for analysis of 23 lipophilic persistent organic pollutants (POPs) in low-volume plasma and serum samples which is applicable for biomonitoring and epidemiological studies. The analysis of selected markers for internal exposure: 16 polychlorinated biphenyls (PCBs), 5 organochlorine pesticides (OCPs), octachlorinated dibenzo-p-dioxin (OCDD), and polybrominated diphenylether 47 (BDE 47) was evaluated by comparing two SPE sorbents and GC-HRMS or GC-MS/MS detection. The final method extracted 23 POPs from 150 mu L of serum and plasma using a 96-well extraction plate containing 60 mg Oasis HLB sorbent per well prior to GC-HRMS magnetic sector analysis. The extraction method was applied to 40 plasma samples collected for an epidemiological study. The recovery of selected POPs ranged from 31% to 63% (n = 48), and detection limits ranged from 2.2 to 45 pg/mL for PCBs, 4.2 to 167 pg/mL for OCPs, 7.8 pg/mL for OCDD and 6.1 pg/mL for BDE 47. This method showed good precision with relative standard deviations of selected POP concentrations in quality control samples (n = 48) ranging from 11% to 25%. The trueness was determined with standard reference material serum (n = 48) and the deviation from certified values ranged from 1 to 27%. Of the 23 POPs analyzed, 18 were detected in 43% to 100% of plasma samples collected for the epidemiological study. The method showed good robustness with low inter-well plate variation (11-31%) determined by twelve 96-well plate extractions, and can extract 96 samples, including quality controls and procedural blanks in 2-3 days. Comparison with GC-MS/MS analysis showed that similar concentrations (within 0.5% to 30%) of most POPs could be obtained with GC-APCI-MS/MS. Larger deviations were observed for PCB 194 (60%) and trans-nonachlor (43%). The developed method produces accurate concentrations of low-level marker POPs in plasma and serum, prov
机译:本研究的目的是开发和验证96孔板固相提取方法,用于分析低体积血浆和血清样品中的23例亲脂性持续有机污染物(POP),这适用于生物监测和流行病学研究。通过比较两种SPE吸附剂和GC来评估所选内部暴露的选定标志物(PCB),5种有机氯杀虫剂(OCP),八氯丁二苯甲酰基二恶蛋白(OCDD)和聚溴二苯醚47(BDE 47)。 -HRMS或GC-MS / MS检测。在GC-HRMS磁性扇形分析之前,使用含有60mg Oasis HLB吸附剂的96孔提取板提取的最终方法从150μL血清和等离子体中振荡。将提取方法应用于收集的流行病学研究的40个等离子体样品。所选弹出的恢复范围为31%至63%(n = 48),并且PCB的检测限为2.2至45pg / ml,4.2至167pg / ml用于OCDD,7.8 pg / ml和6.1 pg BDE 47.该方法显示出良好的精度,具有所选流行浓度的质量控制样品(n = 48)的相对标准偏差,范围为11%至25%。用标准参考材料血清(n = 48)测定真实性,并且偏离认证值的偏差为1%至27%。在分析的23个流行物中,在收集的流行病学研究中以43%至100%的血浆样品检测18个。该方法表现出良好的稳健性,低井间板变异(11-31%),由12个96孔板萃取确定,可以提取96个样品,包括2-3天内的质量控制和程序坯料。与GC-MS / MS分析的比较表明,通过GC-APCI-MS / MS可以获得大多数POP的相似浓度(0.5%至30%)。针对PCB 194(60%)和反逆转体(43%)观察到较大的偏差。开发方法在血浆和血清中产生精确的低水平标记物污染物,优点

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