分散固相萃取-气相色谱-串联质谱法测定血清中7种多溴联苯醚  

Determination of 7 polybrominated diphenyl ethers in serum by dispersive solid phase extraction combined with gas chromatography-tandem mass spectrometry

作　　者：李晓晶[1] 杨荣[1] 彭荣飞[1] 邓芬芳[1] 刘苗[1] 甘平胜[1] LI Xiao-jing;YANG Rong;PENG Rong-fei;DENG Fen-fang;LIU Miao;GAN Ping-sheng(Guangzhou Municipal Center for Disease Control and Prevention,Gangdong 510440,China)

机构地区：[1]广州市疾病预防控制中心,广东510440

出　　处：《中国卫生检验杂志》2023年第22期2694-2696,2700,共4页Chinese Journal of Health Laboratory Technology

基　　金：广州市卫生健康科技项目(20211A011054);广东省医学科学技术研究基金项目(2020111994146867)。

摘　　要：目的建建立人血清中7种多溴联苯醚的分散固相萃取-气相色谱-串联质谱分析方法。方法取1.0ml血清样品加入1%甲酸乙睛提取,再加人100mg氯化钠,振荡10min,以8000r/min速度冷冻离心5min。提取液加人150mg无水MgSO_(4)和50mgZ-Sep分散剂净化,涡旋振荡5min,取上清液1.00ml于氮气流中吹干,50μl异辛烷复溶。采用气相色谱-三重四级杆-串联质谱测定(GC-MS/MS),DB-5色谱柱分离,电子轰击源(EI)多反应监测模式(MRM)检测,基质匹配标准曲线法定量。结果7种多溴联苯醚分离效果好,在0.1μg/L~50.0μg/L内成现良好的线性关系,相关系数r均>0.999,高、中、低3个浓度水平的平均回收率为88.3%~104.2%,相对标准偏差(RSD)为4.8%~9.2%,方法检出限为0.006ng/ml~0.024ng/ml,方法定量限为0.017ng/ml~0.072ng/ml。结论该分析方法操作简单、灵敏、准确,快速,适用于血清中多种多溴联苯醚的快速测定。Objective This paper aims to develop a method for the analysis of 7 polybrominated diphenyl ethers(PBDEs)in serum by dispersive solid phase extraction(d-SPE)combined with gas chromatography-tandem mass spectrometric(GC-MS/MS).Methods The analytes in serum sample was extracted with 1%acetic acid-acetonitrile,and then 100 mg sodium chloride was added,shaken for 10 min,refrigerated and centrifuged at 8000 r/min for 5 min.The extract was purified by adding 150 mg of anhydrous MgSO_(4) and 50 mg of Z-Sep dispersant and then vortexed for 5 min.1.00 ml of supernatant was dried in a nitrogen stream and redissolved in 50μl of isooctane.The analytes in sample solution were determined by GC-MS/MS,separated with DB-5 column and detected by a mass spectrometer with electron impact ion source(EI)in multiple reac-tions monitoring(MRM)mode.The quantifications were based on matrix-matched calibration curves.Results The separa-tion effect of 7 PBDEs was good,and good linearity was obtained when the concentration of PBDEs was within O.1μg/L-50.0μg/L,with correlation coefficients(r)above 0.999.The average recoveries at low,medium and high spiked levels were in the range of 88.3%-104.2%,with relative standard deviations(RSDs)of 4.8%-9.2%.The detection limits were between 0.006 ng/ml and 0.024 ng/ml,while the quantification limits were between 0.017 ng/ml and 0.072 ng/ml.Conclu-sion This method is simple,sensitive,accurate and fast,which is suitable for the rapid detection of PBDEs in serum.

关 键 词：多溴联苯醚 血清 气相色谱-串联质谱法 分散固相萃取 

分 类 号：O657[理学—分析化学]