鱼肉类罐头中双酚-二环氧甘油醚的固相萃取／HPLC-MS／MS法检测  

Determination of Bisphenol Diglycidyl Ethers in Fish Canned Foodstuffs by Solid-phase Extraction/HPLC-MS/MS

作　　者：张朝晖[1] 罗生亮[2] 吴少林[2] 赵鑫[1] 刘文涛[1] 云环[1] 

机构地区：[1]北京出入境检验检疫局,北京100026 [2]南昌航空大学环境与化学工程学院,江西南昌330063

出　　处：《分析测试学报》2009年第6期714-719,共6页Journal of Instrumental Analysis

基　　金：国家质检总局科技计划资助项目(2006IK119);南昌航空大学研究生创新基金资助项目(YC2007006)

摘　　要：建立了鱼肉类罐头中内分泌干扰物质双酚A二缩水甘油醚（BADGE）及其衍生物BADGE·H2O、BADGE·2H2O、BADGE·2HCl、BADGE·HCl·H2O和双酚F二缩水甘油醚（BFDGE）及其衍生物BFDGE·2H2O、BFDGE·2HCl 8种双酚-二环氧甘油醚的固相萃取／液相色谱-电喷雾串联质谱分析方法。以叔丁基甲醚为提取溶剂，采用超声波辅助溶剂萃取法萃取，萃取液用Waters Oasis HLB固相萃取柱进行净化浓缩。以Thermo Hypersil Gold C18色谱柱为分离柱，在正离子模式下以电喷雾电离串联质谱仪进行测定。考察了流动相组分和流动相添加剂对质谱离子化效率的影响，8种双酚-二环氧甘油醚在1．0～100．0μg／L范围内线性关系良好（r≥0．99）。在2．0、10．0和50．0μg／kg的添加水平下，8种目标化合物的回收率为83％～99％，相对标准偏差小于9．0％，方法的检出限为0．13～0．30μg／kg。方法具有较高的灵敏度和准确度，能够满足鱼肉类罐头食品中双酚-二环氧甘油醚残留量的快速检测。A comprehensive analytical method based on solid-phase extraction/high liquid chromatog- raphy - electrospray ionization tandem mass spectrometry was developed for measuring 8 exogenous endocrine disruptors-bisphenol diglycidyl ethers, including BADGE, BADGE · H2O, BADGE · 2H2O, BADGE· 2HCl, BADGE. HCl·H2O, BFDGE, BFDGE· 2H2O, BFDGE· 2HCl, in fish canned foodstuffs. The samples were extracted with methyl tertiary butyl ether by ultrasonic wave assistant extraction（UAE）. The extracts were cleaned up and concentrated on Waters Oasis HLB column. The targeted compounds were analyzed by HPLC - MS/MS under positive ion mode using Ther- mo Hypersil Gold C18 column as analytical column. Effects of mobile phase and additives on ionization were also discussed. Under the optimal conditions, the calibration curves showed a good linearity in the concentration range of 1.0 - 100.0 μg/L for 8 target compounds. The correlation coefficients （r） were no less than 0. 99. Recoveries of 8 analytes at the spiked level of 2. 0, 10. 0 and 50. 0 μg/kg ranged from 83% to 99% with RSDs less than 9.0% . The detection limits of the method ranged from 0. 13 to 0.30 μg/kg. The method was sensitive and accurate, and was suitable for the rapid determination of exogenous endocrine disruptors-bisphenol diglyeidyl ethers in fish canned food- stuffs.

关 键 词：高效液相色谱-电喷雾质谱/质谱 固相萃取 双酚-二环氧甘油醚 鱼肉类罐头 

分 类 号：O657.63[理学—分析化学] O625.32[理学—化学]