多壁碳纳米管固相萃取-高效液相色谱-串联质谱法测定食品接触材料中双酚-二环氧甘油醚的迁移量

Determination of the migration of bisphenol diglycidyl ethers from food contact materials by high performance chromatographytandem mass spectrometry coupled with multi-walled carbon nanotubes solid phase extraction

建立了测定食品接触材料中6种双酚-二环氧甘油醚(双酚A二缩水甘油醚(BADGE)及其衍生物双酚A(2,3-二羟丙基)甘油醚(BADGE·H2O)、双酚A(3-氯-2-羟丙基)甘油醚(BADGE·HCl)、双酚A(3-氯-2-羟丙基)(2,3-二羟丙基)醚(BADGE·H2O·HCl)和双酚F二缩水甘油醚(BFDGE)及其衍生物双酚F双(3-氯-2-羟丙基)甘油醚(BFDGE·2HCl))迁移到食品中的迁移量的高效液相色谱-串联质谱法(HPLC-MS/MS)。样品以叔丁基甲醚(MT-BE)为提取溶剂,超声提取,提取液经多壁碳纳米管(MWCNTs)固相萃取(SPE)柱富集、净化。以COSMOSILC18为分析柱,流动相为0.1%甲酸的5mmol/L醋酸铵溶液和甲醇。6种双酚-二环氧甘油醚在1.0～100μg/L范围内线性关系良好(r2>0.9991)。在3个添加水平下,6种目标化合物的回收率范围为78.6%～89.9%,相对标准偏差小于10%。方法检出限范围为0.5～1.5μg/L。该方法操作简单,灵敏度高,可应用于食品接触材料中双酚-二环氧甘油醚迁移量的快速检测。

A comprehensive analytical method based on high performance liquid chromatographytandem mass spectrometry（HPLC-MS/MS）was developed for measuring 6 exogenous endocrine disruptors bisphenol diglycidyl ethers,including bisphenol A diglycidyl ether（BADGE）,bisphenol A glycidyl（2,3-dihydroxypropyl）ether（BADGE·H2O）,bisphenol A glycidyl（3-chloro-2hydroxypropyl）ether（BADGE· HCl）,bisphenol A（3-chloro-2-hydroxypropyl）（2,3-dihydroxypropyl）ether（BADGE·H2O·HCl）,bisphenol F diglycidyl ether（BFDGE）and bisphenol F bis（3-chloro-2-hydroxypropyl）ether（BFDGE·2HCl）.The samples were extracted with methyl tert-butyl ether（MTBE）by ultrasonic wave assistant extraction.The extracts were cleaned up and concentrated on multi-walled carbon nanotubes（MWCNTs）.The target compounds were analyzed by HPLC-MS/MS under positive ion mode using a COSMOSIL C18column as analytical column.Under the optimal conditions,the calibration curves showed a good linearity in the concentration range of 1.0-100.0μg/L for 6 target compounds.The correlation coefficients（r2）were higher than 0.999 1.Recoveries of 6 analytes at three spiked levels ranged from78.6%to 89.9%,with relative standard deviations（RSDs）less than 10%.The detection limits of the method ranged from0.5 to 1.5μg/L.The method is sensitive and simple,and is suitable for the rapid determination of the migration of bisphenol diglycidyl ethers from food contact materials.