超高效液相色谱-电喷雾离子源-串联三重四极杆质谱分析人血中羟基多溴联苯醚  

Determination of Hydroxylated Polylrominated Diphenyl Ethers in Human Serum by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：王英[1] 丁问微[1] 金军[1] 

机构地区：[1]中央民族大学生命与环境科学学院,北京100081

出　　处：《分析化学》2011年第1期22-26,共5页Chinese Journal of Analytical Chemistry

基　　金：高等学校学科创新引智计划"B08044";国家自然科学基金(No.20507023);北京高等学校化学实验教学示范中心建设项目(2008)资助

摘　　要：建立了超高效液相色谱-电喷雾离子源-串联三重四极杆质谱(UPLC-ESI-MS-MS)在负离子模式下测定人血中5种羟基多溴联苯醚(HO-PBDEs)的方法。血清样品中加入替代内标13C12四溴双酚-A(13C12TBBP-A),经萃取、净化、浓缩等预处理过程,多重反应监测(MRM),扫描通道为:m/z555→431,501→81,579→79;内标法定量。方法回收率为(76.2±14)%～(97.8±5.7)%,检出限(LOQ)为1.0～2.0ng/g·脂肪。应用本方法对人血样品进行测定,检出5-HO-BDE-47,6-HO-BDE-47,5'-HO-BDE-99,6'-HO-BDE-99;∑HO-PBDEs浓度范围为未检出至19ng/g(脂肪中),其中6-HO-BDE-47含量最高,占HO-PBDEs总量的48.7%～100%。A new method has been developed for the simultaneous analysis of five hydroxylated polybrominated diphenyl ethers（HO-PBDEs） in human serum using ultra performance liquid chromatography-electrospray ion source tandem mass spectrometry（UPLC-ESI-MS-MS） in negative ion mode.The serum samples were spiked with ^13C12 Tetrabromobisphenol-A（TBBP-A） as surrogate internal standard before extracting,then the samples were further cleaned up and concentrated.Detection was performed by multiple reaction monitoring（MRM） mode in three channels,555→431,501→81 and 579→79.The recovery of spiked ^13C12TBBP-A and five HO-PBDE congeners in blank samples was from（76.2 ± 14） % to（97.8 ± 5.7） %,the limit of qualification（LOQ） were between 1.0 and 2.0 ng/g·lipid.5-HO-2,2＇,4,4＇-tetrabromodiphenyl ether（5HO-BDE-47）,6-HO-2,2＇,4,4＇-tetrabromodiphenyl ether（6-HO-BDE-47）,5＇-HO-2,2＇,4,4＇,5-pentabromodiphenyl ether（5＇-HO-BDE-99）,6＇-HO-2,2＇,4,4＇,5-pentabromodiphenyl ether（6＇-HO-BDE-99） had been detected and the concentration of ∑HO-PBDEs ranged from no detection to 18.9 ng/g·lipid in six serum samples from volunteers living around PBDEs manufactory.6-HO-BDE-47 was the most abundant HO-PBDEs congener accounting for 48.7% to 100.0% of total HO-PBDEs in each sample.The proposed method based on UPLC-MS-MS has been applied to directly determine HO-PBDEs in human serum without derivatization.

关 键 词：超高效液相色谱-三重四极杆质谱 人血 羟基多溴联苯醚 

分 类 号：R446.1[医药卫生—诊断学]