顶空衍生化固相微萃取法测定酱油中3-氯-1,2丙二醇  

Determination of 3-mono-chloropropane-1,2-diol in soy sauce by solid-phase microextraction with headspace derivatization

作　　者：陈朝方[1] 任立峰[1] 罗玉玮[1] 

机构地区：[1]珠海出入境检验检疫局技术中心,珠海519015

出　　处：《分析试验室》2005年第8期1-4,共4页Chinese Journal of Analysis Laboratory

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.

关 键 词：3-氯-1 2丙二醇 衍生化固相微萃取 顶空 酱油 

分 类 号：O658.1[理学—分析化学]