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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
Journal of Chromatography A ( IF 4.1 ) Pub Date : 2018-02-27 , DOI: 10.1016/j.chroma.2018.02.057
Jordan Stubleski , Petr Kukucka , Samira Salihovic , P. Monica Lind , Lars Lind , Anna Kärrman

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 μL 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, providing a suitable high-throughput sample preparation procedure for biomonitoring and epidemiological studies involving large sample size and limited sample volume. GC-HRMS was chosen over GC–MS/MS, however the latter showed promising results, and could be used as an alternative to GC-HRMS analysis for most POPs.



中文翻译:

一种使用96孔板固相萃取分析小剂量血浆和血清样品中的标记持久性有机污染物的方法

这项研究的目的是开发和验证一种96孔板固相萃取方法,用于分析小批量血浆和血清样品中的23种亲脂性持久性有机污染物(POPs),该方法适用于生物监测和流行病学研究。用于内部曝光选定标志物的分析:16和多氯联苯(PCBs),5有机氯农药,八氯代二苯并p通过比较两种SPE吸附剂和GC-HRMS或GC-MS / MS检测对二恶英(OCDD)和多溴二苯醚47(BDE 47)进行了评估。最终方法是在GC-HRMS磁区分析之前,使用每孔含60 mg Oasis HLB吸附剂的96孔提取板从150μL血清和血浆中提取23种POPs。提取方法应用于收集的40份血浆样本,用于流行病学研究。选定的POP的回收率范围为31%至63%(n = 48),PCB的检出限范围为2.2至45 pg / mL,OCP的检出限为4.2至167 pg / mL,OCDD和7.8 pg / mL / mL对于BDE47。此方法显示出良好的精密度,质量控制样品(n = 48)中选定POP浓度的相对标准偏差为11%至25%。用标准参考物质血清(n = 48)确定真实度,其与认证值的偏差范围为1%至27%。在所分析的23种POP中,有43%至100%的血浆样本中有18种被检出用于流行病学研究。该方法显示出良好的鲁棒性,通过十二次96孔板提取确定了低的孔板间差异(11-31%),并且可以在2-3天之内提取96个样品,包括质量控制和程序空白。与GC-MS / MS分析的比较表明,使用GC-APCI-MS / MS可以获得大多数POPs的相似浓度(0.5%到30%之内)。PCB 194的偏差较大(60%),而PCB 194的偏差较大。该方法显示出良好的鲁棒性,通过十二次96孔板提取确定了低的孔板间差异(11-31%),并且可以在2-3天之内提取96个样品,包括质量控制和程序空白。与GC-MS / MS分析的比较表明,使用GC-APCI-MS / MS可以获得大多数POPs的相似浓度(0.5%到30%之内)。PCB 194的偏差较大(60%),而PCB 194的偏差较大。该方法显示出良好的鲁棒性,通过十二次96孔板提取确定了低的孔板间差异(11-31%),并且可以在2-3天之内提取96个样品,包括质量控制和程序空白。与GC-MS / MS分析的比较表明,使用GC-APCI-MS / MS可以获得大多数POPs的相似浓度(0.5%到30%之内)。PCB 194的偏差较大(60%),而PCB 194的偏差较大。反式无氯(43%)。所开发的方法可在血浆和血清中产生低浓度的POPs的准确浓度,为涉及大样本量和有限样本量的生物监测和流行病学研究提供了合适的高通量样本制备程序。选择了GC-HRMS而不是GC-MS / MS,但后者显示出令人鼓舞的结果,可以用作大多数POP的GC-HRMS分析的替代方法。

更新日期:2018-02-27
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