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

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(MTBE)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COSMOSIL C18为分析柱,流动相为0.1%甲酸的5 mmol/L醋酸铵溶液和甲醇。6种双酚-二环氧甘油醚在1.0～100 μg/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0.5～1.5 μg/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。

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

A comprehensive analytical method based on high performance liquid chromatography-tandem 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-2-hydroxypropyl) 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 C18 column as analytical column. Under the optimal conditions, the calibration curves showed a good linearity in the concentration range of 1.0~100.0 μg/L for 6 target compounds. The correlation coefficients (r2) were higher than 0.9991. Recoveries of 6 analytes at three spiked levels ranged from 78.6% to 89.9%, with relative standard deviations (RSDs) less than 10%. The detection limits of the method ranged from 0.5 to 1.5 μg/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.