Citation: CAO Guo-Zhou , CHEN Shao-Hong , XIAO Dao-Qing , ZHU Xiao-Yan , MA Ming , LIU Zai-Mei . Rapid Determination of Bisphenol Diglycidyl Ethers and Its Migration Regulations in Interior Coating of Food Cans. Chinese Journal of Analytical Chemistry, 2014, 42(3): 403-408. doi: 10.3724/SP.J.1096.2014.30796 [复制]
Rapid Determination of Bisphenol Diglycidyl Ethers and Its Migration Regulations in Interior Coating of Food Cans
建立了快速、简便的超高效液相色谱法同时测定食品模拟物中双酚A-二缩水甘油醚（BADGE）、双酚F-二缩水甘油醚（BFDGE）及其衍生物特定迁移量的方法。采用水、3%乙酸、10%乙醇和葵花籽油4种食品模拟物在60℃、10 d的条件下模拟了食品罐内壁涂料中双酚-二缩水甘油醚的迁移。水性食品模拟物直接进样，葵花籽油模拟物采用乙腈提取，提取液经固相萃取净化后进样。迁移到水性食品模拟物中的BADGE、双酚A-（3-氯-2-羟丙基）甘油醚（BADGE·HCl）发生水解，分别转化成双酚A-二（2，3-二羟丙基）醚（BADGE·2H2O）和双酚A-（3-氯-2-羟丙基）（2，3-二羟丙基）醚（BADGE·H2O·HCl）；迁移到油性模拟物中的BADGE和BADGE·HCl则没有发生水解。9种双酚-二缩水甘油醚在0.05~10 mg/L范围内线性关系良好，水性食品模拟物和油性食品模拟物中方法的检出限分别为5 μg/L和20 μg/kg。应用本方法对10种未接触过食品的空罐进行了检测，有5种样品中检出了BADGE及其衍生物，其中1种样品中BADGE·2H2O（或BADGE）和BADGE·H2O·HCl（或BADGE·HCl）在4种食品模拟物中的迁移量均超过了欧盟EC/1895/2005规定的限量。
A rapid and simple ultra performance liquid chromatographic method for determination the specific migration of bisphenol A diglycidyl ether (BADGE), bisphenol F diglycidyl ether (BFDGE) and their derivatives in food simulants was developed. Water, 3% acetic acid, 10% ethanol and sunflower oil were used as food simulants to simulate the specific migration of bisphenol diglycidyl ethers from interior coating of food cans after 10 days storage at 60℃. After the migration period, the aqueous food simulants were directly measured without any further purification, while the sunflower oil simulant was extracted by acetonitrile followed by cleaning up using solid phase extraction. Among the migration process, BADGE and bisphenol A (3-chloro-2-hydroxypropyl)glycidyl ether (BADGE·HCl) migrated into aqueous simulants were hydrolysed into bisphenol A bis (2,3-dihydroxypropyl) ether (BADGE·2H2O) and bisphenol A (3-chloro-2-hydroxypropyl) (2,3-dihydroxypropyl) ether (BADGE·H2O·HCl), respectively. However, BADGE and BADGE·HCl migrated into sunflower oil were not hydrolysed. The calibrating curves showed a good linearity from 0.05 to 10 mg/L for all the 9 target compounds. The detection limits of the method for aqueous food simulants and sunflower oil stimulant were 5 μg/L and 20 μg/kg, respectively. The method was applied to the determination of bisphenol diglycidyl ethers migrated from 10 kinds of food cans which were intended to contact with food. The results indicate that BADGE and its derivatives were detected at 5 of the cans, and the specific migration of BADGE(or BADGE·2H2O)and BADGE·HCl(or BADGE·H2O·HCl)in 1 cans even exceed the responding limitation regulated in EC/1895/2005.