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