分散固相萃取-气相色谱串联质谱法快速测定血清中6种新型溴系阻燃剂  

Determination of 6 novel brominated flame retardants in serum by dispersive solid phase extraction combined with gas chromatography tandem mass spectrometry

作　　者：王翼飞[1,2] 陈田[1,2] 张淑华[1,2] 施致雄[1,2] 

机构地区：[1]首都医科大学公共卫生学院,北京100069 [2]首都医科大学环境毒理学北京市重点实验室,北京100069

出　　处：《分析试验室》2017年第2期129-133,共5页Chinese Journal of Analysis Laboratory

基　　金：国家自然科学基金项目(21477083);北京市属高等学校高层次人才引进与培养计划(CIT&TCD201404190);北京市自然科学基金项目(7122022)资助

摘　　要：建立了分散固相萃取-气相色谱串联质谱法快速提取、净化并测定血清中6种新型溴系阻燃剂的分析方法。血清样以正己烷/丙酮混合液提取,Na Cl和无水Mg SO4盐析后,提取液经含有C18和无水Mg SO4的离心管分散净化,采用GC-EI-MS/MS在多反应监测模式下测定五溴甲苯、五溴乙苯、六溴苯、2,3-二溴丙基-2,4,6-三溴苯基醚和1,2-双(2,4,6-三溴苯氧基)乙烷,采用GC-NCI-MS在选择离子监测模式下测定十溴二苯乙烷,同位素内标法定量。除十溴二苯乙烷外其余阻燃剂在1~100μg/L范围内线性关系良好,相关系数均大于0.999。在0.02,0.2和2μg/L三个浓度添加水平下平均回收率范围为89.4%~136.6%,相对标准偏差(RSD)小于18%。除十溴二苯乙烷检出限为350 ng/L外,其余待测物检出限在4.2~32 ng/L。方法适合血清中多种新型溴系阻燃剂的同时前处理与测定。A method for the determination of 6 novel brominated flame retardants（BFRs） was developed using a dispersive solid phase extraction coupled to gas chromatography tandem mass spectrometry（DSPE-GC-MS/MS）.Serum sample was extracted by an acetone/hexane mixture,and then salted-out by adding Na Cl and anhydrous Mg SO4,followed by a dispersive solid-phase extraction（d SPE） step using C18 particles as a sorbent.GC-MS/MS was used for the quantification of the target compounds（including pentabromotoluene, pentabromoethylbenzene,2,3-Dibromopropyl-2,4,6-tribromophenyl ether,hexabromobenzene and 1,2-bis（2,4,6-tribromophenoxy） ethane）.However,GC-NCI-MS was used for the detection of decabromodiphenyl ethane due to its extremely low response in EI-MS/MS.The correlation coefficient was higher than 0.999 with the linear range of 1 - 100 μg/L.The average recoveries were between 89.4% and 136.6% at three spiked levels of 0.02,0.2 and 2 ng/mL with the relative standard deviations lower than 18 % except for decabromodiphenyl ethane.The limits of detection（LOD） ranged from 4.2 to 32 ng/L while LOD of DBDPE was 350 ng/L.This method wasvalidated to be simple,sensitive and selective,and suitable for the routing analysis of BFRs in serum.

关 键 词：血清 新型溴系阻燃剂 分散固相萃取 气相色谱 串联质谱 

分 类 号：TG115.3[金属学及工艺—物理冶金]