色谱 ›› 2011, Vol. 29 ›› Issue (05): 417-421.DOI: 10.3724/SP.J.1123.2011.00417

• 研究论文 • 上一篇    下一篇

气相色谱-质谱法测定食品接触材料表面印刷油墨中的光引发剂

韩伟1, 于艳军1, 李宁涛1, 王利兵2*   

  1. 1. 天津出入境检验检疫局工业产品安全技术中心, 天津 300042; 2. 湖南出入境检验检疫局技术中心, 食品安全科学技术湖南省重点实验室, 湖南 长沙 410004
  • 收稿日期:2010-12-17 修回日期:2011-02-27 出版日期:2011-05-28 发布日期:2011-05-28
  • 通讯作者: 王利兵,博士,研究员,从事危险品及包装安全检验技术研究

Determination of photoinitiators in printing inks used in food contact materials

HAN Wei1, YU Yanjun1, LI Ningtao1, WANG Libing2*   

  1. 1. Technical Center for Safety of Industrial Products, Tianjin Entry-Exit Inspection and Quarantine Bureau, Tianjin 300042, China; 2. Technical Center for Hunan Entry-Exit Inspection and Quarantine Bureau, Hunan Key Laboratory of Food Safety Science & Technology, Changsha 410004, China
  • Received:2010-12-17 Revised:2011-02-27 Online:2011-05-28 Published:2011-05-28

摘要: 建立了食品接触材料表面印刷油墨中光引发剂(PIs)二苯甲酮(BP)、4-甲基二苯甲酮(MBP)、对二甲氨基苯甲酸乙酯(EDAB)、N,N-二甲氨基苯甲酸异辛酯(EHDAB)和1-羟基环己基苯基甲酮(Irgacure 184)的气相色谱-质谱(GC-MS)分析方法。样品以乙酸乙酯为萃取溶剂进行索氏提取,萃取溶液经净化分离和富集以后,以5%苯基-95%甲基聚硅氧烷为固定相(DB-5MS),采用选择离子扫描(SIM)方式对上述5种PIs进行了定性和定量分析。5种PIs在5.0~200.0 μg/L范围内的线性关系良好(R2>0.9995),在2种浓度的添加水平下,回收率为66.7%~89.4%,相对标准偏差<10%。方法的定量限为0.0017~0.0036 mg/dm2。该方法的样品前处理过程简单,易操作,适用于常规进出口食品接触材料表面印刷油墨中PIs的快速检测。

关键词: 光引发剂, 气相色谱-质谱, 食品接触材料, 印刷油墨

Abstract: A new analytical method based on gas chromatography-mass spectrometry (GC-MS) techniques was developed for the determination of five photoinitiators (PIs), benzophenone (BP), 4-methylbenzophenone (MBP), ethyl-4-dimethylaminobenzoate (EDAB), 2-ethylhexyl-4-dimethylaminobenzoate (EHDAB) and 1-hydroxycyclohexyl phenyl ketone (Irgacure 184), in the printing inks used in food contact materials. The test solutions were extracted from selected food contact materials using Soxhlet extractor with ethyl acetate as the extraction solvent. By adding 50 and 200 μg/L of a standard mixture of photoinitiators into the extracts of the blank packaging materials, the recoveries obtained were in the range of 66.7%~89.4%. The repeatability of the method was assessed by determining the contents of the photoinitiators in five types of food contact materials, and the results were lower than 10%. The instrumental detection limits (IDLs) and method quantification limits (MQLs) were in the range of 2.9~6.0 μg/L and 0.0017~0.0036 mg/dm2, respectively. The method was applied in the analysis of about twenty real samples (yogurt carton, milk carton, fruit juice carton and plastic bags samples). The most significant pollutants were BP and MBP. The concentrations of Irgacure 184, EDAB and EHDAB found in three individual samples were 0.84 mg/dm2, 0.2 mg/dm2 and 1.2 mg/dm2, respectively. The work proposed a new method to analyze the migration level of initiators from the inks.

Key words: food contact materials, gas chromatography-mass spectrometry (GC-MS), photoinitiators, printing ink