食用油中氯丙醇酯的GC-MS/MS测定方法  

GC-MS/MS method for determination of chloropropanol ester in edible oil

作　　者：王冉冉[1] 王庆国[1] 雒婉霞[1] 杨雪丽[1] 马鑫[1] WANG Ran-ran;WANG Qing-guo;LUOWan-xia;YANG Xue-li;MAXin(The Center for Disease Control and Prevention of Xinjiang Uygur Autonomous Region, Urumqi, Xinjiang 830002, China)

机构地区：[1]新疆维吾尔自治区疾病预防控制中心

出　　处：《疾病预防控制通报》2018年第6期79-82,共4页Bulletin of Disease Control & Prevention(China)

摘　　要：目的采用三重四级杆气质联用(GC-MS/MS)技术,建立同时检测食用植物油中一氯丙二醇酯及二氯丙醇酯的方法。方法称取0.1g食用油,加入氯丙醇同位素内标,经甲醇钠/甲醇水解、H2SO4/NaBr溶液中和、正己烷除脂和硅藻土小柱净化后,用GC-MS/MS测定、内标法定量;实验过程中,优化前处理方法各要素,以期得到最优实验参数。结果3-MCPD,2-MCPD,1,3-DCP,2,3-DCP的浓度为10.00~1000ng/ml时,线性关系良好(R2>0.998);3-MCPD,2-MCPD与1,3-DCP,2,3-DCP的检出限分别为50.00ng/g,50.00ng/g,30.00ng/g和30.00ng/g,加标回收率在80.1%~111.8%;待测组分在低、中、高3种浓度水平重复测定的RSD%为1.30%~4.97%。结论该方法简便、准确、安全且高效,适用于检测食用植物油样品中的氯丙醇酯。Objective To establish a method for determination of MCPDE and DCPE in edible vegetable oil simultaneously with GC-MS/MS technology. Methods The internal standards of chloropropanol isotope were added into 0.1 g samples of the oil. After hydrolyzing with sodium methylate-methanol, neutralizing with H2SO4/NaBr and cleaning up with hexane, extracting and purifying with diatomite column, the analytes were detected by GC-MS/MS and quantified with internal standard method. All elements of the pretreatment were optimized to obtain the optimal experimental parameters during the experiment. Results The linearity existed (R2>0.998) when the concentration of MCPD and DCP were 10.00-1 000.00 ng/ml. The limit value of detection for 3-MCPD, 2-MCPD, 1, 3-DCP and 2, 3-DCP was 50.00, 50.00, 30.00 and 30.00 ng/g, respectively, with the recovery of standard addition from 80.1% to 111.8%. The RSD of the repeated determination of the components was 1.30%~4.97% at low, medium and high concentration. Conclusions This method is simple, accurate, safe and efficient, and suitable for the detection of the chloropropanol ester in edible vegetable oil.

关 键 词：一氯丙二醇酯 二氯丙醇酯 方法优化 

分 类 号：TQ646[化学工程—精细化工] TS227[轻工技术与工程—粮食、油脂及植物蛋白工程]