同位素稀释气相色谱-质谱法快速测定酱油中3-氯-1,2-丙二醇量  

Rapid Determination of 3-Chloro-1,2-Propanediol in Soy Sauce by Gas Chromatography-Mass Spectrometry with Isotopic Dilution Method

作　　者：王悦宏[1] 闫吉昌[1] 刘俊会[2] 徐锐峰[3] 薛静[1] 王卫华[3] 石金娥[1] 陈大伟[1] 闫福成[1] 

机构地区：[1]东北师范大学城市与环境学院,长春130024 [2]吉林省产品质量监督检验院,长春130022 [3]国家标准物质研究中心,北京100013

出　　处：《分析化学》2007年第11期1657-1660,共4页Chinese Journal of Analytical Chemistry

基　　金：国家计量基标准体系(化学部分)资助共享平台建设(No2005DKA10804);国家科学技术部科技专项基金(No2006BA618A)资助项目

摘　　要：采用同位素稀释气相色谱－质谱联用（GC－MS）法，快速测定酱油中3－氯－1，2-丙二醇（3-MCPD）的含量。试样中加入3－氯－1，2-丙二醇的氘代同位素作为内标，经超声混匀后加入到自行填装的弗罗里硅土柱中，以乙醚洗脱，洗脱液经氮气吹干后在正己烷溶剂中进行衍生化，衍生化试剂采用七氟丁酰咪唑。GC-MS采用选择离子监测（SIM）模式进行定性定量分析。结果表明，本方法的添加回收率为95．0％－101．0％；相对标准偏差为3．2％～4．8％；检出限达到0．010mg／kg。本方法步骤简单，溶剂用量少，定性定量准确可靠。可快速测定酱油等调味品中3－氯－1，2-丙二醇的含量。The method using isotopic dilution and solid phase extraction （SPE） technique was established to determine the concentration of 3-chloro-1,2-propanediol in soy sauce by gas chromatography- mass spectrography （GC-MS）. Internal standard, 3-chloro-l,2-propanediol-d5 was added into soy sauce, after sonication, the mixture was transferred to a Florisil SPE column and eluted with ethyl ether. Evaporate the solution just to dry at room temperature under a stream of N2. 1.0 mL hexane and 0.05 mL heptafluorobutyry-limidazole were added immediately. GC-MS with SIM mode was applied to identify and quantitate. The recoveries ranged from 95.0% - 101.0%. The relative standard deviation was 3.2% - 4.8% with a detection limit of 0. 010 mg/kg.

关 键 词：3-氯-1 2-丙二醇 气相色谱-质谱法 同位素稀释 

分 类 号：TS264.21[轻工技术与工程—发酵工程]