Determination of Migration Amounts of 5 Compounds in Food Contact Rubber Liners by High Performance Liquid Chromatography－Tandem Mass Spectrometry

CHEN Yin-qing; LI Zi-cheng; TONG Xing; CHEN Jie; GE Dan-yang; PENG Qi-shan; LI Dan; HU Chang-ying

doi:10.19969/j.fxcsxb.22012503

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Determination of Migration Amounts of 5 Compounds in Food Contact Rubber Liners by High Performance Liquid Chromatography－Tandem Mass Spectrometry

Scientific Papers | 更新时间：2022-06-22

- Determination of Migration Amounts of 5 Compounds in Food Contact Rubber Liners by High Performance Liquid Chromatography－Tandem Mass Spectrometry
- Journal of Instrumental Analysis Vol. 41, Issue 6, Pages: 865-872(2022)
- 作者机构：
  
  1.暨南大学食品科学与工程系，广东广州 510632
  2.广州海关技术中心国家食品接触材料检测重点实验室（广东），广东广州 510623
  3.暨南大学包装工程学院，广东省普通高校产品包装与物流重点实验室，广东珠海 519070
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.22012503
  CLC：
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陈银卿,黎梓城,童星等.高效液相色谱－串联质谱法测定食品接触用橡胶奶衬制品中5种化合物的迁移量[J].分析测试学报,2022,41(06):865-872.

CHEN Yin-qing,LI Zi-cheng,TONG Xing,et al.Determination of Migration Amounts of 5 Compounds in Food Contact Rubber Liners by High Performance Liquid Chromatography－Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2022,41(06):865-872.
陈银卿,黎梓城,童星等.高效液相色谱－串联质谱法测定食品接触用橡胶奶衬制品中5种化合物的迁移量[J].分析测试学报,2022,41(06):865-872. DOI： 10.19969/j.fxcsxb.22012503.

CHEN Yin-qing,LI Zi-cheng,TONG Xing,et al.Determination of Migration Amounts of 5 Compounds in Food Contact Rubber Liners by High Performance Liquid Chromatography－Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2022,41(06):865-872. DOI： 10.19969/j.fxcsxb.22012503.

摘要

建立了食品接触用橡胶奶衬中5种化合物（苯胺、N-甲基苯胺、二苯胍、2-巯基苯并噻唑和苯并噻唑）的高效液相色谱－串联质谱检测方法。采用Agilent Poroshell 120EC－C,18,（3 mm × 50 mm，2.7 μm）色谱柱进行分离，以0.1%（体积分数）甲酸水溶液和乙腈为流动相梯度洗脱分离，在电喷雾离子源的正离子多反应监测（MRM）模式下检测，外标法定量。结果表明，在优化条件下，5种化合物在对应的质量浓度范围内线性关系良好，相关系数（,r,2,）均不小于0.996 6，检出限（LOD，,S,/,N ,= 3）和定量下限（LOQ，,S/N ,= 10）分别为0.8～20 μg/L和3～50 μg/L。在3 ~ 500 μg/L加标水平下的平均回收率为93.4% ~ 112%，相对标准偏差（RSD）为0.70% ~ 4.3%。利用该方法检测市售10种奶衬在3个模拟迁移条件（40 ℃ 10 min，40 ℃ 30 min和40 ℃ 120 min）下5种化合物的迁移量，奶衬中5种化合物均有迁出，二苯胍和2-巯基苯并噻唑的迁移量在限量范围内；苯并噻唑的检出需引起关注；苯胺和N-甲基苯胺的迁移量高于其迁移限量（0.01 mg/kg），有必要改进配方或工艺以控制苯胺和N-甲基苯胺物质的生成。该方法具有操作简单、灵敏度高等优点，可为食品接触用橡胶奶衬制品中5种化合物迁移量的分析提供技术支持。

Abstract

A method was developed for the determination of the migration amounts of 5 compounds，i.e.aniline，N-methylaniline，1，3-diphenylguanidine，2-mercaptobenzothiazole and benzothiazole in food contact rubber liners by high performance liquid chromatography－tandem mass spectrometry（HPLC－MS/MS）．The separation of target compounds was performed with an Agilent Poroshell 120EC－C,18, column（3 mm × 50 mm，2.7 μm），using 0.1%（volume fraction） formic acid and acetonitrile solution as mobile phases by gradient elution．The detection on the analytes was performed with positive electrospray ionization source under multiple reaction monitoring（MRM） mode，and the quantitation was carried out by the external standard method．Under the optimized conditions，the calibration curves were linear in the respective mass concentration ranges，with correlation coefficients（,r,2,） not less than 0.996 6．The limits of detection（LODs，,S,/,N, = 3） and quantitation（LOQs，,S,/,N, = 10） were in the ranges of 0.8－20 μg/L and 3－50 μg/L，respectively．The average recoveries for 5 compounds at the spiked levels of 3－500 μg/L were in the range of 93.4%－112%，with relative standard deviations（RSDs） of 0.70%－4.3%．This method was used to detect the migration amounts of 5 compounds in 10 kinds of food contact rubber liners under the three conditions（40 ℃ for 10 min，40 ℃ for 30 min and 40 ℃ for 120 min）．According to the migration results，5 compounds in all liners were detected，and the migration amounts of 1，3-diphenylguanidine and 2-mercaptobenzothiazole were within the limit range．The detection of benzothiazole needs attention．The migration amounts of aniline and N-methylaniline were higher than its migration limit（0.01 mg/kg），and the generation of aniline and N-methylaniline must be controlled by improving the formulation or the process．This method has the advantages of simple operation and high sensitivity，and it is suitable for the determination of 5 compounds in food contact rubber liners．

关键词

食品接触用橡胶奶衬高效液相色谱－串联质谱法（HPLC－MS/MS）食品模拟物迁移

Keywords

food contact rubber linershigh performance liquid chromatography－tandem mass spectrometry（HPLC－MS/MS）food simulantsmigration

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