色谱

色谱 ›› 2013, Vol. 31 ›› Issue (1): 46-52.DOI: 10.3724/SP.J.1123.2012.08055

• 研究论文 • 上一篇    下一篇

气相色谱-质谱法同时测定塑料食品接触材料中25种芳香族伯胺的迁移量

李英1*, 李成发1, 肖道清2, 梁烽1, 陈枝楠1, 陈旭辉1, 孙小颖1, 李泳涛1   

  1. 1. 深圳出入境检验检疫局, 广东 深圳 518045; 2. 宁波出入境检验检疫局, 浙江 宁波 315012
  • 收稿日期:2012-08-30 修回日期:2012-10-19 出版日期:2013-01-28 发布日期:2013-01-21
  • 通讯作者: 李成发
  • 基金资助:
    科技部科技支撑计划项目(2011BAK10B05-03).

Determination of migration of 25 primary aromatic amines from food contact plastic materials by gas chromatography-mass spectrometry

LI Ying1*, LI Chengfa1, XIAO Daoqing2, LIANG Feng1, CHEN Zhinan1, CHEN Xuhui1, SUN Xiaoying1, LI Yongtao1   

  1. 1. Shenzhen Entry-Exit Inspection and Quarantine Bureau, Shenzhen 518045, China; 2. Ningbo Entry-Exit Inspection and Quarantine Bureau, Ningbo 315012, China
  • Received:2012-08-30 Revised:2012-10-19 Online:2013-01-28 Published:2013-01-21

PDF

559

被引次数

35

摘要： 采用固相萃取前处理技术,结合气相色谱-质谱法对食品接触材料中25种芳香族伯胺的迁移量进行了同时测定。样品中25种目标物分别用蒸馏水和30 g/L醋酸浸出后,用氨水调节浸泡液至pH 8～10,经固相萃取小柱富集净化,再用体积比为1:1的叔丁基甲醚和乙醇混合液洗脱定容后用气相色谱-质谱仪测定。不同芳香族伯胺的检出限略有差异,在0.4～2.0 μg/kg的范围内。加标水平在10 μg/kg时,除2,4-二氨基苯甲醚在酸性模拟物中的回收率较低外,其他芳香族伯胺的回收率均在51.6%～118.4%之间,相对标准偏差(n=7)为0.5%～9.8%。同时探讨了不同实验条件如叔丁基甲醚和乙醇的体积比、pH值等条件对25种芳香族伯胺回收率的影响。结果表明,该方法准确、稳定,完全满足欧盟指令No 10/2011对食品接触塑料材料及制品中芳香族伯胺特定迁移量的限量要求,可用于食品接触材料中芳香族伯胺的实际检验。

关键词: 芳香族伯胺, 固相萃取, 气相色谱-质谱法, 食品接触材料, 特定迁移量

Abstract: A solid phase extraction (SPE) combination with gas chromatography-mass spectrometry (GC-MS) was developed for the determination of the migration of 25 primary aromatic amines (PAAs) from food contact plastic materials and articles. The samples were extracted by deionized water and 30 g/L acetic acid, and the pH value of the solution was adjusted to 8-10 with ammonia. The extracts were cleaned up and concentrated on an SPE column, then eluted by equal volume of methyl-tert-butyl ether and ethanol. The analysis of the target compounds was performed by GC-MS. The results indicated that the limits of detection were in the range of 0.4-2.0 μg/kg for different PAAs. The recoveries and relative standard deviations (n=7) of 10 μg/kg PAAs ranged from 51.6%-118.4% and 0.5%-9.8%, respectively, except the 2,4-diaminoanisole in the acid simulant. The effects of different experimental conditions such as the pH value and volume ratio of methyl-tert-butyl ether and ethanol were studied. The results showed that the method is accurate and stable, and could meet the requirement of the European Commission Regulation (EU) No 10/2011 for the determination of primary aromatic amines. It can be applied in the analysis of the primary aromatic amines in real food contact plastic material and article samples.

Key words: food contact materials, primary aromatic amines, solid phase extraction (SPE), specific migration limits, gas chromatography-mass spectrometry (GC-MS)