液相色谱串联质谱法测定精炼植物油中的4种3-氯-1,2-丙二醇双酯  

Determination of four 3-chloro-1,2-propanediol diesters in refinedv egetable oil by liquid chromatography tandem mass spectrometry

作　　者：蒋林惠 周楠 周易枚 丁红梅 JIANG Linhui;ZHOU Nan;ZHOU Yimei;DING Hongmei(Nantong Food and Drug Supervision and Inspection Center,Nantong 226006,Jiangsu,China)

机构地区：[1]南通市食品药品监督检验中心,江苏南通226006

出　　处：《中国油脂》2023年第9期93-98,共6页China Oils and Fats

基　　金：南通市科技项目计划(JC2020109,MS12021027)。

摘　　要：为准确、快速测定油脂中3-氯丙醇双酯,建立了一种基于液相色谱串联质谱技术测定精炼植物油中4种3-氯-1,2-丙二醇双酯[3-氯-1,2-丙二醇棕榈酸二酯(3-MCPD-PP)、3-氯-1,2-丙二醇二油酸酯(3-MCPD-OO)、3-氯-1,2-丙二醇硬脂酸二酯(3-MCPD-SS)、3-氯-1,2-丙二醇-1-棕榈酸-2-亚油酸二酯(3-MCPD-PL)]的方法。待测油样加入氘代同位素内标后经NH2固相萃取柱、固相分散萃取净化包(PSA 500 mg, C18 500 mg)联合净化后,过0.22μm有机膜,取2μL样品溶液注入液质联用仪中进行测定。经Accucore VDX色谱柱分离,ESI源离子化,SRM模式,并采用同位素内标法对3-氯-1,2-丙二醇双酯进行定性定量分析。结果表明:4种3-氯-1,2-丙二醇双酯在1~1 000μg/L范围内均呈现良好的线性关系,检出限均为0.010 mg/kg,在精炼植物油中的回收率和相对标准偏差(RSD)分别为3-MCPD-PP 62.3%~94.0%和5.43%~11.67%,3-MCPD-OO 60.1%~91.7%和3.28%~13.54%,3-MCPD-SS 61.6%~92.1%和4.73%~10.46%,3-MCPD-PL 62.3%~92.2%和2.69%~11.37%。该方法简便、高效,可用于精炼植物油中3-氯-1,2-丙二醇双酯的检测。For the accurate and rapid determination of 3-chloropropanol diesters in vegetable oil,a method for the determination of four kinds of 3-chloro-1,2-propanediol diesters,including 3-chloro-1,2-propanediol palmitate diester(3-MCPD-PP),3-chloro-1,2-propanediol dioleate(3-MCPD-OO),3-chloro-1,2-propanediol stearic acid diester(3-MCPD-SS)and 3-chloro-1,2-propanediol-1-palmitate-2-linoleate diester(3-MCPD-PL)in refined vegetable oil by liquid chromatography tandem mass spectrometry(LC-MS-MS)was established.The oil sample was added with deuterium isotope internal standard,then cleaned-up by NH2solid phase extraction column and solid phase dispersion extraction clean-up kit(PSA 500 mg,C18500 mg).After passing 0.22μm organic membrane,2μL sample solution was injected into liquid chromatography-mass spectrometry for determination.After separation by Accucore VDX column,ionization by ESI source,scanning by SRM mode and qualitative and quantitative analysis of 3-chloro-1,2-propanediol diesters by isotope internal standard method.The results showed that there was a good linear relationship when the mass concentration of four 3-chloro-1,2-propanediol diesters was in the range of 1-1000μg/L,and the detection limits of the four 3-chloro-1,2-propanediol diesters were 0.010 mg/kg.The recoveries and relative standard deviations in refined vegetable oil were 3-MCPD-PP 62.3%-94.0%and 5.43%-11.67%,3-MCPD-OO 60.1%-91.7%and 3.28%-13.54%,3-MCPD-SS 61􀆰6%-92.1%and 4.73%-10.46%,3-MCPD-PL 62.3%-92.2%and 2.69%-11.37%,respectively.The method is simple,efficient and can be used for the determination of 3-chloro-1,2-propanediol diesters in refined vegetable oils.

关 键 词：3-氯-1 2-丙二醇双酯 精炼植物油 非衍生化 液相色谱串联质谱技术 

分 类 号：TS227[轻工技术与工程—粮食、油脂及植物蛋白工程] TS221[轻工技术与工程—食品科学与工程]