凝胶渗透色谱-固相萃取结合色谱-质谱法测定乳制品中18种溴系阻燃剂  

Determination of 18 Brominated Flame Retardants in Dairy Product by Gel Permeation Chromatography-Solid Phase Extraction Coupled to Gas Chromatography-Mass Spectrometry and High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：李健[1,2] 王翼飞[1,2] 周显青[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：《分析化学》2016年第11期1742-1747,共6页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金(No.21477083);北京市属高等学校高层次人才引进与培养计划项目(No.CIT&TCD201404190);北京市自然科学基金(No.7122022)资助~~

摘　　要：采用索氏提取、凝胶渗透色谱和固相萃取技术作为前处理方法,建立乳制品中6种新型溴系阻燃剂、8种多溴联苯醚、四溴双酚A和α、β、γ-六溴环十二烷异构体共18种溴系阻燃剂的同时提取与净化方法,并结合气相色谱-负化学源质谱法（GC-NCI/MS）和高效液相色谱-电喷雾电离-串联质谱法（HPLC-ESI-MS/MS）进行检测。奶样经冷冻干燥后以正己烷-丙酮（1∶1,V/V）索氏提取,采用凝胶渗透色谱结合酸化硅胶柱净化,随后以LC-Si固相萃取柱分离气相和液相待测物。以GC-NCI/MS测定6种新型溴系阻燃剂和8种多溴联苯醚,以HPLC-MS/MS检测四溴双酚A和六溴环十二烷异构体,内标法定量。结果表明,以空白牛奶样品为加标基质,多数待测物平均回收率为80.1%-114.7%,方法具有良好的精密度（多数待测物相对标准偏差（RSD）在0.87%-14.9%）和灵敏度（检出限在0.2-119.2 pg/g之间）,可满足乳制品中多种溴系阻燃剂同时提取、净化和检测需求。A novel method was developed for the simultaneous determination of 6 novel brominated flame retardants（NBFRs）,8 polybrominated diphenyl ethers（PBDEs）,tetrabromobisphenolA（TBBPA）and α,β,γ-hexabromocyclododecane（α,β,γ-HBCD）in dairy product. Dairy product samples were extracted using soxhlet extraction with acetone / hexane（1∶ 1,V / V）. The removal of co-extracted materials was achieved by gel permeation chromatography followed by acidified silica treatment. The fractionation of the PBDEs /NBFRs and HBCD / TBBPA was performed using a Supelco LC-Si SPE cartridge. The detection of the PBDEs and NBFRs was then performed by GC-NCI / MS,and that of the HBCDs and the TBBPA was performed using HPLC-MS / MS. A recovery test was performed using a matrix spiking test and for most of the analytes the recoveries ranged from 80. 1% to 114. 7% with RSDs equal to or lower than 14. 9%. The LODs were 0. 2-119. 2 pg / g. This methodology was validated to be accurate and sensitive for the simultaneous pretreatment and analysis of brominated flame retardants in dairy product.

关 键 词：溴系阻燃剂 气相色谱-负化学源质谱 高效液相色谱-串联质谱 乳制品 固相萃取 

分 类 号：TS252.7[轻工技术与工程—农产品加工及贮藏工程]