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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 |
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DOI: |
中文关键词: 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 |
英文关键词:3-chloro-1,2-propanediol diester refined vegetable oil non-derivatization LC-MS-MS technology |
基金项目:南通市科技项目计划(JC2020109,MS12021027) |
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中文摘要: |
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0.22 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%~1354%,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。 |
英文摘要: |
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 616% -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. |
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