目的 建立高效液相色谱串联质谱同时检测植物油中香兰素、甲基香兰素和乙基香兰素的分析方法.方法 样品经乙腈提取后, 以正己烷除脂净化, 采用 C18色谱柱进行分离, 以0.1%(V/V)甲酸水和甲醇为流动相进行梯度洗脱, 质谱采用电喷雾正离子电离进行多反应监测模式监测(multiple reaction monitoring, MRM).结果 方法加标回收率(n=6)为83.4%~96.8%, 相对标准偏差为3.1%~4.6%, 检出限为23~30 μg/kg, 定量限为76~100 μg/kg.采用该方法对50批次市售植物油进行检测, 只有香兰素被检出, 检出浓度为160~830 μg/kg.结论 该方法操作简便、检测准确、分析速度快, 适合植物油中香兰素、甲基香兰素和乙基香兰素的快速检测.%Objective To establish an analytical method for simultaneous determination of vanillin, methyl vanillin and ethyl vanillin in vegetable oil by high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS). Methods The samples were extracted by acetonitrile, purified by n-hexane, separated by C18 column with 0.1% (V/V) formic acid aqueous solution and methanol as mobile phases, and then analyzed by HPLC-MS/MS. The mass spectrometry was operated in positive electronic spay ionization (ESI+) mode with dynamic multiple reaction monitoring (MRM). Results The spiked recoveries of the method (n=6) were 83.4%~96.8% with the relative standard deviation of 3.1%~4.6%. The limits of detection (LODs) ranged from 23 to 30 μg/kg and the limits of quantification (LOQs) were in the range of 76~100 μg/kg. Fifty batches of commercially available vegetable oil were detected by this method and only vanillin was detected at concentration ranging from 160 to 830 μg/kg. Conclusion This method is efficient, reliable and sensitive, and suitable for rapid determination of the vanillin, methyl vanillin and ethyl vanillin in vegetable oil.
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