凝胶渗透色谱-分散固相萃取法同时测定鸡蛋中多溴联苯醚及其衍生物、四溴双酚A和六溴环十二烷  

Determination of Polybrominated Diphenyl Ethers and Derivatives,Tetrabromobisphenol A,Hexabromocyclododecane in Egg Samples by Gel Permeation Chromatography and Dispersive Solid Phase Extraction

作　　者：李敏洁[1] 金芬[1] 杨莉莉[1] 乌日娜[1] 邵华[1] 金茂俊[1] 王静[1] 

机构地区：[1]农业部农产品质量安全重点实验室中国农业科学院农业质量标准与检测技术研究所,北京100081

出　　处：《分析化学》2014年第9期1288-1294,共7页Chinese Journal of Analytical Chemistry

基　　金：国家科技支撑计划资助项目(No.2012BAD29B03)~~

摘　　要：建立了一种同时检测鸡蛋中四溴双酚A（TBBP A）、六溴环十二烷（HBCD）和多溴联苯醚（PBDEs）及其衍生物羟基多溴联苯醚（OH-PBDEs）和甲氧基多溴联苯醚（MeO-PBDEs）的凝胶渗透色谱（GPC）-分散固相萃取（DSPE）-液相色谱-串联质谱（HPLC-MS/MS）和气相色谱-负化学源质谱（GC-NCI/MS）的检测方法。样品经正己烷、二氯甲烷（1∶1,V/V）加速溶剂萃取,凝胶渗透色谱净化后,经100 mg十八烷基键合硅胶（C18）分散固相萃取吸附剂去除杂质,液相色谱-串联质谱和气相色谱-负化学源质谱方法测定,外标法定量。在蛋白和蛋黄样品中添加1.0或5.0μg/kg的目标物,其回收率分别为64.5%~97.2%和65.6%~109.2%（除BDE-85为54.8%,OH-BDE-137为47.4%外）,相对标准偏差小于20.2%,定量限为0.01~0.2μg/kg。A stimulate method for determination of polybrominated diphenyl ethers （PBDEs） and derivatives （OH-PBDEs and MeO-PBDEs）, tetrabromobisphenol A （ TBBPA）, hexabromocyclododecane （HBCD） in egg samples was developed by gel permeation chromatography （ GPC ） and dispersive solid phase extraction （DSPE） combined with liquid chromatography tandem mass spectrometric （HPLC-MS/MS） and gas chroma- tography-negative chemical ionization mass spectrometry （GC-NCI/MS）. The analytes were extracted with mixture of hexane and dichloromethane （1：1, V/V） by accelerated solvent extraction （ASE）, and purified by 100 mg C18 dispersive solid phase extraction （SPE） sorbents followed with gel permeation chromatography （GPC） , and then analyzed by liquid chromatography tandem mass spectrometric （HPLC-MS/MS） and gas chromatography-negative chemical ionization mass spectrometry （GC-NCI/MS）, respectively. The quantitation was carried out external standard method. The recoveries of objects were 64.5% -97.2% and 65.6% - 109.2% （except BDE85 was 54.8%, OH-BDE-137 was 47.4% ） spiked at 1.0 μg/kg or 5.0 p,g/kg in egg white and egg yolk, respectively. The relative standard deviations （RSDs） were less than 20.2%. ,The limits of quantitation （LOQ） for the object were 0.01-0.2 μg/kg.

关 键 词：多溴联苯醚及其衍生物 四溴双酚A 六溴环十二烷 鸡蛋 凝胶渗透色谱 分散固相萃取 

分 类 号：O657.7[理学—分析化学]