| 顶空衍生化固相微萃取法测定酱油中3-氯-1,2丙二醇 |
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| 引用本文： | 陈朝方,任立峰,罗玉玮.顶空衍生化固相微萃取法测定酱油中3-氯-1,2丙二醇[J].分析试验室,2005,24(8):1-4. |
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| 作者姓名： | 陈朝方 任立峰 罗玉玮 |
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| 作者单位： | 珠海出入境检验检疫局技术中心,珠海,519015;珠海出入境检验检疫局技术中心,珠海,519015;珠海出入境检验检疫局技术中心,珠海,519015 |
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| 摘 要： | 建立顶空衍生化固相微萃取测定酱油中3-氯-1,2丙二醇(3-MCPD)的方法。聚乙二醇-二乙烯基苯(CW-DVB)萃取纤维先顶空吸附苯基硼酸,然后同时萃取和衍生化样品顶空气体中的3-MCPD和内标物d5-3-MCPD,衍生化产物在进样口热解吸,GC-MS检测,内标法定量,特征离子为m/z196、201。结果表明,样品中3-MCPD质量浓度为0.01~1mg/kg时,工作曲线的线性良好(r=0.9994),添加回收率为89%~104%,检出限为0.01mg/kg。
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| 关 键 词： | 3-氯-1 2丙二醇 衍生化固相微萃取 顶空 酱油 |
| 文章编号： | 1000-0720（2005）08-0001-04 |
| 收稿时间： | 2004-09-20 |
| 修稿时间： | 2004-12-01 |
Determination of 3-mono-chloropropane-1, 2-diol in soy sauce by solid-phase microextraction with headspace derivatization |
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| Chen Chao-fang,REN Li-feng,Luo Yu-wei.Determination of 3-mono-chloropropane-1, 2-diol in soy sauce by solid-phase microextraction with headspace derivatization[J].Chinese Journal of Analysis Laboratory,2005,24(8):1-4. |
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| Authors: | Chen Chao-fang REN Li-feng Luo Yu-wei |
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| Abstract: | A novel method for the determination of 3- mono-chloropropane-1, 2-diol (3-MCPD) in soy sauce was developed. Gaseous 3-MCPD and d5-3-MCPD (in- ternal standard) were sampled by headspace dervatiza- tion with phenylboronic acid (PBA) adsorbed onto solid phase microextraction fiber, and analyzed by gas chro- matography-mass spectrometry (GC/MS) in selective ion monitoring mode (characteristic ions m/z 196, 201), and quantified by an internal standard method. The cali- bration curve was linear over the range of 0. 01 ~ 1. 0 mg/kg. The recoveries of spiked samples were 89%~ 104%. The detection limit was 0.01 mg/kg. |
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| Keywords: | 3-mono-chloropropane-1 2-diol Derivatiza- tion/solid phase microextraction Headspace Soy Sauce |
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