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.
作者
王冉冉
王庆国
雒婉霞
杨雪丽
马鑫
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)
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)
