液相色谱-串联质谱法同时测定食品接触用涂层中13种双酚类缩水甘油醚及其衍生物的迁移量

刘育形; 喻零春; 周瑾艳; 彭绮珊; 梁颖茵; 曾莹; 钟怀宁; 李丹

doi:10.19554/j.cnki.1001-3563.2026.19.011

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包装工程（技术栏目） ›› 2026, Vol. 47 ›› Issue (19) : 103-115. DOI: 10.19554/j.cnki.1001-3563.2026.19.011

农产品保鲜与食品包装

液相色谱-串联质谱法同时测定食品接触用涂层中13种双酚类缩水甘油醚及其衍生物的迁移量

刘育形¹, 喻零春¹, 周瑾艳², 彭绮珊¹, 梁颖茵¹, 曾莹¹, 钟怀宁¹, 李丹^1,*

作者信息 +

Determination of Migration Levels of 13 Bisphenol Diglycidyl Ethers and Their Derivatives in Food Contact Coatings by Liquid Chromatography-Tandem Mass Spectrometry

LIU Yuxing¹, YU Lingchun¹, ZHOU Jinyan², PENG Qishan¹, LIANG Yingyin¹, ZENG Ying¹, ZHONG Huaining¹, LI Dan^1,*

Author information +

文章历史 +

摘要

目的建立可同时测定食品接触用涂层中13种双酚A-二缩水甘油醚和双酚F-二缩水甘油醚及其羟基和氯化衍生物迁移量的液相色谱-串联质谱（Liquid Chromatography-Tandem Mass Spectrometry, LC-MS/MS）法。方法水、酸性,以及酒精类食品模拟物过滤后直接进样,异辛烷和橄榄油模拟物经过乙腈水萃取后进行测试,采用电喷雾离子源（ESI）正离子多反应监测（MRM）进行测试,外标法定量。结果在3.0~100 μg/L 质量浓度范围,样品中13种双酚-二缩水甘油醚类化合物线性关系良好（R²≥0.995）,方法检出限为1.0~3.0 μg/kg,加标回收率在81.5%~116%,相对标准偏差范围为0.2%~7.6%。结论该方法灵敏、操作简便且重现性良好,适用于食品接触涂层中双酚类二缩水甘油醚类物质的定量分析。将该方法应用于64款内壁带环氧涂层的金属罐测试,结果发现BADGE及其衍生物检出率为37.5%,有一款样品的BADGE氯化衍生物特定迁移总量超出限量要求。

Abstract

The work aims to establish a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the simultaneous determination of the migration levels of 13 bisphenol A diglycidyl ethers and bisphenol F diglycidyl ethers, as well as their hydroxyl and chlorinated derivatives in food contact coatings. Aqueous, acidic, and alcoholic simulants were directly injected into LC-MS/MS, whereas isooctane and olive oil simulants were extracted with acetonitrile-water solution prior to analysis. Analysis was conducted in positive ion multiple reaction monitoring (MRM) mode using an electrospray ionization (ESI) source, with quantification performed via the external standard method. Within the mass concentration range of 3.0-100 μg/L, the 13 bisphenol diglycidyl ether compounds in the samples exhibited good linearity (R²≥0.995). The limits of detection of the method were 1.0-3.0 μg/kg, the spiked recoveries ranged from 81.5% to 116%, and the relative standard deviations were between 0.2% and 7.6%. This method is sensitive and simple, and is suitable for the rapid determination of 13 kinds of bisphenol diglycidyl ethers in food contact coatings. This method is applied to the testing of 64 metal cans with epoxy coatings on the inner wall. The results show that the detection rate of BADGE and its derivatives is 37.5%, and the total specific migration of chlorinated BADGE derivatives in one sample exceeds the regulatory limit.

导出引用

刘育形, 喻零春, 周瑾艳, 彭绮珊, 梁颖茵, 曾莹, 钟怀宁, 李丹. 液相色谱-串联质谱法同时测定食品接触用涂层中13种双酚类缩水甘油醚及其衍生物的迁移量[J]. 包装工程. 2026, 47(19): 103-115 https://doi.org/10.19554/j.cnki.1001-3563.2026.19.011

LIU Yuxing, YU Lingchun, ZHOU Jinyan, PENG Qishan, LIANG Yingyin, ZENG Ying, ZHONG Huaining, LI Dan. Determination of Migration Levels of 13 Bisphenol Diglycidyl Ethers and Their Derivatives in Food Contact Coatings by Liquid Chromatography-Tandem Mass Spectrometry[J]. Packaging Engineering. 2026, 47(19): 103-115 https://doi.org/10.19554/j.cnki.1001-3563.2026.19.011

中图分类号： TB486 O657.63

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