色谱

色谱

• 研究论文 • 上一篇    下一篇

固相萃取-气相色谱/负化学电离-质谱法测定酸水解植物蛋白及酱油中的3-氯-1,2-丙二醇

陈捷,王志元   

  1. Food Inspection Center, Guangzhou Entry & Exit Inspection and Quarantine Bureau, Guangzhou 510623, China
  • 收稿日期:2005-09-16 修回日期:2006-01-23 出版日期:2006-09-30 发布日期:1986-09-25
  • 通讯作者: 陈捷

Determination of 3-Monochloropropane-1,2-Diol in Hydrolyzed Vegetable Proteins and Soy by Solid Phase Extraction and Gas Chromatography/Negative Chemical Ionization-Mass Spectrometry

CHEN Jie, WANG Zhiyuan   

  1. Food Inspection Center, Guangzhou Entry & Exit Inspection and Quarantine Bureau, Guangzhou 510623, China
  • Received:2005-09-16 Revised:2006-01-23 Online:2006-09-30 Published:1986-09-25
  • Contact: Chen Jie

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710

被引次数

3

摘要： 建立了酸水解植物蛋白及酱油中3-氯-1,2-丙二醇(3-MCPD)的固相萃取-气相色谱/质谱测定方法。样品经Aoisa-HBL固相萃取柱萃取,正己烷-乙酸乙酯净化提取,七氟丁酰咪唑衍生,衍生物经气相色谱/负化学电离-质谱（GC/NCI-MS）选择离子模式(SIM)检测，外标法定量。3-MCPD的定量检测限为0.5 μg/kg,平均回收率为92.2%～97.4%,相对标准偏差为3.6%～10.9%。该方法检测灵敏度高，定性定量准确。

关键词: 3-氯-1,2-丙二醇, 负化学电离源, 固相萃取, 酱油 , 气相色谱/质谱法, 水解植物蛋白, 选择离子扫描

Abstract: Solid phase extraction (SPE) and gas chromatographic/negative chemical ionization-mass spectrometric （GC/NCI-MS） method was developed for the determination of 3-monochloropropane-1,2-diol (3-MCPD) in hydrolyzed vegetable proteins (HVP) and soy. The optimized conditions for the extraction and cleanup of 3-MCPD on an Aoisa-HBL column were investigated. The extract with hexane-ethyl acetate was evaporated to nearly dry by N2 at 40 ℃ and derivatization was performed with 1-(heptafluorobutyryl) imidazole at 70 ℃ for 30 min. The mixture was then injected into a gas chromatograph with a DB-5MS capillary column, detected by a mass spectrometer in negative chemical ionization and selected ion monitoring mode (NCI/SIM) and quantified with external standard calibration. The limit of quantitation (LOQ) for 3-MCPD was 0.5 μg/kg. The average recovery was in a range of 92.2%-97.4% with a relative standard deviation range of 3.6%-10.9%. The results indicated that the method could be used for the sensitive and accurate determination of 3-MCPD in foods and agriculture products.

Key words: 3-monochloropropane-1,2-diol, hydrolyzed vegetable proteins, negative chemical ionization （NCI）, selected ion monitoring （SIM）, solid phase extraction （SPE）, soy , gas chromatography/mass spectrometry （GC/MS）