气相色谱-质谱法测定蜡笔中的芳香伯胺

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

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。

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.