罐装饮料中双酚A-二缩水甘油醚与双酚F-二缩水甘油醚及其衍生物的快速检测

Rapid Determination of Bisphenol A Diglycidyl Ether and Bisphenol F Diglycidyl Ether and Their Derivatives in Canned Beverage by Ultra Performance Liquid Chromatography

建立了固相萃取/超高效液相色谱法测定罐装饮料中9种双酚-二缩水甘油醚,包括双酚A-二缩水甘油醚（BADGE）及其衍生物BADGE·2H2O、BADGE·H2O、BADGE·2HCl、BADGE·HCl、BADGE·H2O·HCl和双酚F-二缩水甘油醚（BFDGE）及其衍生物BFDGE·2H2O、BFDGE·H2O的快速检测方法。采用叔丁基甲醚为提取溶剂,涡旋振荡提取,提取液氮吹至近干后用甲醇-水（2∶3）溶解,采用PLS亲水亲酯柱固相萃取净化。以Shim-pack XR-ODS-Ⅲ为分析柱,乙腈-水为流动相进行梯度洗脱。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,回收率为83.8%~98.7%,RSD为2.3%~5.6%,方法检出限为20μg/kg。该方法操作简单、灵敏度高,可在10 min内对罐装饮料中9种双酚-二缩水甘油醚进行快速检测。

A rapid analytical method based on solid phase extraction and ultra performance liquid chromatography（ UPLC） was developed for the determination of 9 kinds of bisphenol diglycidyl ethers,including bisphenol A diglycidyl ether（ BADGE） and its derivatives： BADGE·2H 2 O,BADGE·H 2 O, BADGE·2HCl,BADGE·HCl,BADGE·H 2 O·HCl,bisphenol F diglycidyl ether（ BFDGE） and its derivatives： BFDGE·2H 2 O and BFDGE·H 2 O. The beverage samples were extracted twice by votex shaking with methyl tert-butyl ether. The extract was dried by a relax flow of nitrogen at 40 ℃. The residue was redissolved with methanol- water（ 2 ∶ 3） followed by cleaning up using PLS solid phase extraction. The target compounds were separated on a Shim- pack XR- ODS- Ⅲ column by gradient elution using acetonitrile- water as mobile phase. Under the optimized conditions,the calibration curves showed good linearity in the range of 0. 05- 10 mg / L. The recoveries at two spiked concentration levels ranged from 83. 8% to 98. 7%,with RSDs of 2. 3%- 5. 6%. The limits of detection（ LODs） for the target compounds were all 20 μg/kg. The method is sensitive and simple,and is suitable for the rapid determination of 9 kinds of bisphenol diglycidyl ethers in 10 min.