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 refined vegetable oil by liquid chromatography tandem mass spectrometry

Abstract

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0.22 μm有机膜，取2 μL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1~1 000 μg/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 NH2 solid phase extraction column and solid phase dispersion extraction clean-up kit（PSA 500 mg， C18 500 mg）. After passing 0.22 μm organic membrane, 2 μL 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 1-1 000 μg/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.

Keywords

• 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
• 3-chloro-1，2-propanediol diester; refined vegetable oil; non-derivatization; lc-ms-ms technology