色谱

色谱 ›› 2012, Vol. 30 ›› Issue (11): 1108-1112.DOI: 10.3724/SP.J.1123.2012.08054

• 专栏 • 上一篇    下一篇

液-液萃取-液相色谱-串联质谱法测定“地沟油”中辣椒碱类化合物及丁香酚

张忠*, 任飞, 张盼   

  1. 重庆市公安局物证鉴定中心, 重庆 400021
  • 收稿日期:2012-08-28 修回日期:2012-10-20 出版日期:2012-11-28 发布日期:2009-02-25
  • 通讯作者: 张忠,主任法医师,主要从事理化检验工作. Tel: (023)63751660, E-mail: zhangzhong5123@126.com.

Determination of capsaicinoids and eugenol in waste-edible-oil by liquid-liquid extraction and liquid chromatography-tandem mass spectrometry

ZHANG Zhong*, REN Fei, ZHANG Pan   

  1. Material Evidence Identification Center of Chongqing Public Security Bureau, Chongqing 400021, China
  • Received:2012-08-28 Revised:2012-10-20 Online:2012-11-28 Published:2009-02-25

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摘要： 建立了“地沟油”中辣椒碱类化合物(包括辣椒素、二氢辣椒素、合成辣椒素)及丁香酚的液-液萃取及液相色谱-串联质谱(LC-MS/MS)检测方法。“地沟油”中辣椒碱类化合物及丁香酚用甲醇萃取,采用SUPEL COSIL ABZ+Plus dC18色谱柱(150 mm×4.6 mm, 5 μm)分离,电喷雾离子源在正、负离子模式下电离,多反应监测(MRM)模式扫描。对辣椒素、二氢辣椒素、合成辣椒素及丁香酚的检出限分别为0.02、0.03、0.03和0.6 μg/L,且在一定的质量浓度范围内线性良好。同一操作人员与不同操作人员间测定的精密度低于5%。该方法专属性强、灵敏、准确,可以作为“地沟油”的判定标准之一。

关键词: 地沟油, 丁香酚, 辣椒碱, 液相色谱-串联质谱

Abstract: A method was developed for the determination of capsaicinoids (capsaicin, dihydrocapsaicin and synthetic capsaicin) and eugenol in waste-edible-oil extracted by liquid-liquid extraction and liquid chromatography-tandem mass spectrometry (LC-MS/MS). The capsaicinoids and eugenol in waste-edible-oil were extracted by methanol, and then separated by a SUPEL COSIL ABZ+Plus dC18 column (150 mm×4.6 mm, 5 μm). The analysis was performed by MS/MS with electrospray ionization in positive and negative ion modes with multiple reaction monitoring (MRM). The limits of detection for capsaicin, dihydrocapsaicin, synthetic capsaicin and eugenol were 0.02, 0.03, 0.03 and 0.6 μg/L, respectively. The good linear relationships were obtained in certain concentration ranges of capsaicinoids and eugenol. The relative standard deviations (RSDs, n=5) of same-worker and different-worker were less than 5%. The method is exclusive, sensitive and accurate, and can be used in waste-edible-oil determination.

Key words: capsaicinoids, eugenol, waste-edible-oils, liquid chromatography-tandem mass spectrometry (LC-MS/MS)