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基于石墨烯固相萃取,以实际样品为研究对象,建立了食品接触材料中内分泌干扰物双酚A-二缩水甘油醚(BADGE)及其衍生物BADGE·H2O、BADGE·HCl、BADGE·2H2O、BADGE·2HCl、BADGE·H2O·HCl和双酚F-二缩水甘油醚(BFDGE)及其衍生物BFDGE·2HCl、BFDGE·2H2O等9种双酚-二环氧甘油醚迁移量的高效液相色谱-串联质谱(HPLC-MS/MS)检测方法。样品以叔丁基甲醚为提取溶剂,超声提取,提取液经石墨烯固相萃取柱富集、净化。质量分数0.1%乙酸的5 mmol/L醋酸铵溶液和甲醇为流动相,经COSMOSIL C18分析柱分离后,采用电喷雾串联四级杆质谱检测。9种双酚-二环氧甘油醚中2种在0.5~50 ng/m L范围内线性关系良好;2种在5.0~100.0 ng/m L范围内线性关系良好;其他5种在2.0~100.0 ng/m L范围内线性关系良好(r2>0.992 2)。对牛肉、橘片两种罐头食品进行3个水平的添加回收实验,9种目标化合物的回收率分别为:60.0%~97.6%(牛肉)和65.7%~111.3%(橘片),相对标准偏差小于20%。方法的检测低限为0.1~1.0μg/kg。该方法操作简单,灵敏度高,成功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。
Based on the graphene solid-phase extraction, the bioassay of bisphenol A-diglycidyl ether (BADGE) and its derivatives BADGE · H2O, BADGE · HCl, BADGE · 2H2O, High Performance Liquid Chromatography of BDPGE · 2HCl, BADGE · H2O · HCl and Bisphenol F-diglycidyl Ether (BFDGE) and Their Derivatives BFDGE · 2HCl, BFDGE · 2H2O and Other 9 Phenol-Glycidyl Ether Migration - Tandem mass spectrometry (HPLC-MS / MS) detection method. The sample was extracted with tert-butyl methyl ether and extracted by ultrasound. The extract was purified by graphene SPE column. Mass fraction of 0.1% acetic acid in 5 mmol / L ammonium acetate solution and methanol as the mobile phase, the COSMOSIL C18 analytical column separation, the use of electrospray tandem quadrupole mass spectrometry detection. There was a good linear relationship between the two kinds of bisphenol-diglycidyl ethers in the range of 0.5-50 ng / m L, the good linearity was found in the range of 5.0-100.0 ng / m L and the other five were in the range of 2.0-100.0 Linearity was good in the range of ng / m L (r2> 0.992 2). The recoveries of three kinds of canned foods were 60.0% ~ 97.6% (beef) and 65.7% ~ 111.3% (orange slices), respectively. The relative standard deviation Less than 20%. The detection limit of the method is 0.1 ~ 1.0μg / kg. The method is simple in operation and has high sensitivity and is successfully applied to the rapid detection of the migration of bisphenol-diglycidyl ether in food contact materials.