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顶空衍生化固相微萃取法测定酱油中3-氯-1,2丙二醇 被引量:5

Determination of 3-mono-chloropropane-1,2-diol in soy sauce by solid-phase microextraction with headspace derivatization
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摘要 建立项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/z 196、201.结果表明,样品中3-MCPD质量浓度为0.01~1 mg/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0.01 mg/kg. 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 (intemal standard) were sampled by headspace dervatiza- tion with phenylboronic acid (PBA)adsorbed onto solid phase microextraction fiber, and analyzed by gas chromatography-mass spectrometry (GC/MS) in selective ion monitoring mode (characteristic ions m/z 196, 201 ), and quantified by an internal standard method. The calibration 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.
出处 《分析试验室》 CAS CSCD 北大核心 2005年第8期1-4,共4页 Chinese Journal of Analysis Laboratory
关键词 3-氯-1 2丙二醇 衍生化固相微萃取 顶空 酱油 3-mono-chloropropane-1,2-diol Derivatization/solid phase microextraction Headspace Soy Sauce
作者简介 陈朝方(1971-),男,工程师
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参考文献11

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