液液萃取-苯硼酸衍生化法快速测定酱油中氯丙二醇  

Liquid-liquid extraction and phenylboronic acid derivatization forrapid determination of 3-monochloropropane-1,2-diol in soy sauce

作　　者：梁秀清 陈倩倩 陈克云 吕邓义 李洁 李霞 王艳丽 刘艳明 LIANG Xiuqing;CHEN Qianqian;CHEN Keyun;LÜDengyi;LI Jie;LI Xia;WANG Yanli;LIU Yanming(Shandong Institute for Food and Drug Control,Industrial Technology Foundation Public Service Platform,Jinan 250101)

机构地区：[1]山东省食品药品检验研究院,产业技术基础公共服务平台,济南250101

出　　处：《中国食品添加剂》2024年第12期209-214,共6页China Food Additives

摘　　要：建立一种快速测定酱油中氯丙二醇含量的分析方法。样品中的氯丙二醇经乙腈提取,苯硼酸衍生化,气相色谱-串联质谱动态多反应离子监测(dMRM)模式测定,内标法定量。方法学评价表明,2种MCPD的检出限、定量限分别为0.0005和0.002 mg/kg,2~400 ng/mL范围内线性关系良好,相关系数大于0.999,空白酱油中4个浓度水平0.002、0.020、0.10、0.40 mg/kg的加标回收率在90.5%~100.7%之间,相对标准偏差为1.8%~4.6%。该方法能满足酱油中氯丙二醇的检测要求。A method of rapid determination of 3-monochloropropane-1,2-diol(MCPD)in soy sauce was established.The MCPD in soy sause samples were extracted by acetonitrile,then derivatized with phenylboronic acid,and quantified using GC-MS/MS in dynamic multiple reaction monitoring(dMRM)mode with internal standard method.The results showed that the limits of detection(LODs)were 0.0005 mg/kg,and the limits of quantitation(LOQs)were 0.002 mg/kg.Two kinds of MCPD had excellent linear relationship between 2 to 400 ng/mL,with the correlation coefficients(R2)greater than 0.999.The spiked recovery rates in blank soy sauce samples were from 90.5%to 100.7%at four levels of 0.002,0.020,0.10,0.40 mg/kg,and the relative standard deviations(RSDs)of method were 1.8%〜4.6%.The developed method met the detection requirements for MCPD in soy sauce.

关 键 词：液液萃取 苯硼酸衍生化法 氯丙二醇 酱油 

分 类 号：TS202.3[轻工技术与工程—食品科学] TS207.3[轻工技术与工程—食品科学与工程]