超高效合相色谱-串联质谱法定量检测食用植物油中12种长链甘油三酯  

Quantitative Analysis of 12 Kinds of Long-chain Triacylglycerols in Vegetable Oils by Ultra Performance Convergence Chromatography-Tandem Mass Spectrometry

作　　者：杨光勇 郭苍亭 薛光 郭金喜 YANG Guang-yong;GUO Cang-ting;XUE Guang;GUO Jin-xi(Xinjiang Uygur Autonomous Region Product Quality Supervision and Inspection Institute,Urumqi 830011,China;Urumqi Center for Disease Control and Prevention,Urumqi 830026,China)

机构地区：[1]新疆维吾尔自治区产品质量监督检验研究院,新疆乌鲁木齐830011 [2]乌鲁木齐市疾病预防控制中心,新疆乌鲁木齐830026

出　　处：《分析测试学报》2021年第5期699-704,共6页Journal of Instrumental Analysis

摘　　要：建立了超高效合相色谱-串联质谱(UPC 2-MS/MS)测定食用植物油中12种长链甘油三酯(TAGs)含量的方法。样品用正己烷溶解后,以两支串联的HSS C 18 SB色谱柱(100 mm×2.1 mm,1.8μm)为分析柱,超临界CO 2和甲醇(含0.1%甲酸)为流动相梯度洗脱,以97%甲醇水溶液(含0.2%氨水)为补偿液,用配备电喷雾电离源的MS/MS在正离子、多反应监测模式下测定,外标法定量。结果表明:12种TAGs在各自质量浓度范围内线性关系良好(r^(2)≥0.9902),检出限(S/N=3)为1.0~8.0 mg/g,定量下限(S/N=10)为3.0~25 mg/g,平均回收率(n=9)为95.7%~104%,相对标准偏差为1.5%~4.2%,仪器具有良好的精密度。利用该法对实际样品进行检测,并对考察范围以外的部分TAGs进行了分析。该方法基质兼容性强,操作简便,灵敏度高,专属性好,绿色环保,为食用植物油中TAGs的准确定量提供了有效途径。Long-chain triacylglycerols(TAGs)play an important role in maintaining human health and normal development,so it is necessary to establish a rapid and effective method for accurate determination of the contents of TAGs in edible vegetable oils.The polarities and structures of TAGs are very similar,which makes it difficult to separate them by either gas chromatography or liquid chromatography.A method based on ultra performance convergence chromatography-tandem mass spectrometry(UPC 2-MS/MS)was established for the quantitative analysis of 12 kinds of TAGs in vegetable oils.The samples were firstly dissolved and diluted with n-hexane,then separated by gradient elution using an analytical column combining two HSS C 18 SB(100 mm×2.1 mm,1.8μm)columns together,with supercritical carbon dioxide and methanol containing 0.1%formic acid as mobile phases at a flow rate of 1.5 mL/min.The separated compounds were analyzed by MS/MS with an electrospray ionization source in positive ions and multiple reaction monitoring(MRM)modes.Water containing 97%methanol and 0.2%ammonia water was used as the auxiliary pump mobile phase at a flow rate of 0.3 mL/min.The external standard method was used for quantitative analysis of the 12 TAGs in sample solutions.Results showed that there were good linear relationships for the 12 TAGs in the corresponding mass concentration ranges with their correlation coefficients(r 2)not less than 0.9902.The limits of detection(LOD,S/N=3)and limits of quantitation(LOQ,S/N=10)were in the ranges of 1.0-8.0 mg/g and 3.0-25 mg/g,respectively.The average recoveries(n=9)of the method ranged from 95.7%to 104%,with relative standard deviations of 1.5%-4.2%,and good precisions.The developed method was successfully used for the determination of 12 long-chain TAGs in actual samples.Furthermore,some long-chain TAGs outside the scope of the investigation were analyzed.The method is high specific,rapid,simple,reliable,environmentally friendly and compatible for oils matrixes,providing an effective way for determining

关 键 词：超高效合相色谱-串联质谱 长链甘油三酯 食用植物油 

分 类 号：O657.7[理学—分析化学] TS201.6[理学—化学]