摘要
建立了基于液液萃取-固相萃取净化同时测定人血清中43种持久性有机氯污染物(POCPs)的气相色谱-串联质谱(GC-MS/MS)方法,包含18种多氯联苯(PCBs)和25种有机氯农药(OCPs)。取250μL血清样本加入甲醇和酸,使用正己烷和甲基叔丁基醚依次对样品进行萃取,硅胶固相萃取柱对提取液进行净化,洗脱液氮吹浓缩后用甲苯复溶,经TG-5SilMS(30 m×0.25 mm×0.25μm)毛细管色谱柱分离,多反应监测(MRM)模式下进行测定,内标法定量。结果表明,18种PCBs和25种OCPs分别在0.008~1μg/L和0.08~10μg/L范围内线性关系良好,方法检出限为0.005~0.1μg/L,定量下限为0.02~0.3μg/L,基质效应为74.9%~126%;加标回收率为71.6%~129%,日内相对标准偏差(RSD)为1.0%~11%,日间RSD为1.3%~18%。使用标准参考样品评估方法准确度,测定结果与参考值的相对偏差均小于30%。应用该方法测定某地区173份普通人群血清样品,共检出28种POCPs,其中p,p'-DDE和PCB153的检出率超过50%,p,p'-DDE质量浓度的中位数为0.46μg/L,是该地区人群血清中主要的POCPs组分。该方法可有效控制基质效应,提高检测灵敏度,适用于人血清中43种POCPs的检测。
A gas chromatography-tandem mass spectrometric(GC-MS/MS)method was developed for the simultaneous analysis of 43 persistent organochlorine pollutants(POCPs),including 18 poly⁃chlorinated biphenyls(PCBs)and 25 organochlorine pesticides(OCPs)in human serum,based on sol⁃vent extraction coupled with solid-phase extraction cartridge cleanup.Human serum samples were thawed and brought to room temperature before pretreatment.An aliquot of 250μL serum sample was transferred into a 12 mL glass tube.Protein was precipitated using methanol and lipid was removed by acidification to release target analytes.A liquid-liquid extraction was performed using hexane and methyl tert-butyl ether in turn.The extract from both solvent was combined and concentrated.The sample was further purified using silica gel solid-phase extraction cartridges,then concentrated to neardryness under gentle stream of nitrogen and reconstituted with toluene.Subsequently,the chromato⁃graphic separation was performed on a TG-5SilMS(30 m×0.25 mm×0.25μm)column.The target analytes were monitored under multiple reaction monitoring(MRM)mode,and quantified by internal standard method.The results showed that there were good linear relations for the 18 PCBs and 25 OCPs in the ranges of 0.008-1μg/L and 0.08-10μg/L,with the detection limits and the quan⁃titation limits of 0.005-0.1μg/L and 0.02-0.3μg/L,respectively.The matrix effect was in the range of 74.9%-126%.The spiked recoveries ranged from 71.6%to 129%,with intra-day relative standard deviations(RSDs)and inter-day RSDs of 1.0%-11%and 1.3%-18%,respectively.To evaluate method accuracy,standard reference material purchased from the US National Institute of Standards and Technology was used.The relative deviations of tested results were lower than 30%compared to certified values.The developed method was applied to the determination of 173 serum samples collected from general population.A total of 28 POCPs were detected,of which p,p′-DDE and PCB 153 both had a detection frequency over 50%,and the median concentration of p,p′-DDE was found to be 0.46μg/L,making it the primary POCPs in the serum samples of this particular pop⁃ulation.This analytical method is suitable for the detection on 43 POCPs in human serum samples as it could effectively control the matrix effect and improve the analytical sensitivity.
作者
邱天
鲍珊
姜威龙
陆一夫
QIU Tian;BAO Shan;JIANG Wei-long;LU Yi-fu(National Institute of Environmental Health,Chinese Center for Disease Control and Prevention,China CDC Key Laboratory of Environment and Population Health,Beijing 100021,China;School of Public Health,Anhui Medical University,Hefei 230032,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2023年第7期775-783,共9页
Journal of Instrumental Analysis
基金
国家卫生健康委员会公共卫生专项(131031108000160004)
国家自然科学基金项目(82241091)。
关键词
气相色谱-串联质谱
持久性有机氯污染物
液液萃取
固相萃取
人血清
gas chromatography-tandem mass spectrometry
persistent organochlorine pollutants
liquid-liquid extraction
solid-phase extraction
human serum
