色谱

色谱 ›› 2011, Vol. 29 ›› Issue (05): 422-425.DOI: 10.3724/SP.J.1123.2011.00422

• 研究论文 • 上一篇    下一篇

气相色谱-质谱法测定蜡笔中的芳香伯胺

康苏媛, 张庆*, 白桦, 王超, 吕庆   

  1. 中国检验检疫科学研究院工业品检验研究所, 北京 100123
  • 收稿日期:2010-12-23 修回日期:2011-02-28 出版日期:2011-05-28 发布日期:2011-05-28
  • 通讯作者: 张庆,博士,副研究员. Tel: (010)85771969,
  • 基金资助:
    国家财政部行业公益性项目(No. 200810953).

Determination of primary aromatic amines in crayons by gas chromatography-mass spectrometry

KANG Suyuan, ZHANG Qing*, BAI Hua, WANG Chao, Lv Qing   

  1. Institute of Industrial Product Inspection, Chinese Academy of Inspection and Quarantine, Beijing 100123, China
  • Received:2010-12-23 Revised:2011-02-28 Online:2011-05-28 Published:2011-05-28

PDF

521

被引次数

18

摘要： 建立了固相萃取-气相色谱-质谱(SPE-GC-MS)检测儿童蜡笔中苯胺等9种芳香伯胺的方法。先用正己烷除去蜡笔中的烷烃类物质,再以甲醇为提取剂在室温下超声提取两次,提取液经过浓缩后与还原剂连二亚硫酸钠在70 ℃下反应30 min,将反应后的溶液通过硅藻土固相萃取柱净化收集,然后采用HP-5M色谱柱分离,并用质谱进行检测。采用该方法成功地实现了9种芳香伯胺的分离检测。对于不同的芳香伯胺的定量限为5 mg/kg,实际样品的平均回收率为86.02%～102.43%。实验结果证明,该方法准确、稳定,可以用于蜡笔中芳香伯胺的实际检验。

关键词: 芳香伯胺, 固相萃取, 蜡笔, 气相色谱-质谱法

Abstract: A method for the determination of nine primary aromatic amines in crayon by solid phase extraction （SPE） and gas chromatography-mass spectrometry （GC-MS） was developed. The alkanes in the sample were removed with n-hexane. Then the sample was extracted twice with ultrasonic extraction by methanol. The extract was evaporated, then the concentrated solution reacted with the reducing agent （sodium hydrosulfite） for 30 min at 70 ℃. After the extraction with a diatomite SPE column, the aromatic amines were collected and separated on an HP-5M column, determined by MS. The nine primary aromatic amines can be separated and determined successfully. Under the optimized conditions, the detection limits were 5 mg/kg and the spiked recoveries of the samples were in the range of 86.02%~102.43%. The method is accurate and stable. It can be applied in the analysis of the primary aromatic amine of real crayon samples.

Key words: gas chromatography-mass spectrometry (GC-MS), primary aromatic amines, crayon, solid phase extraction (SPE)