高效液相色谱串联质谱法测定植物油中香兰素、 甲基香兰素和乙基香兰素
高效液相色谱串联质谱法测定植物油中香兰素、 甲基香兰素和乙基香兰素
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。
ObjectiveTo 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). MethodsThe 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). ResultsThe 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. ConclusionThis method is efficient, reliable and sensitive, and suitable for rapid determination of the vanillin, methyl vanillin and ethyl vanillin in vegetable oil.
标题：高效液相色谱串联质谱法测定植物油中香兰素、 甲基香兰素和乙基香兰素
英文标题：Determination of vanillin, methyl vanillin and ethyl vanillin in vegetable oil by high performance liquid chromatography tandem mass spectrometry
作者：
曲宝成 大连市食品检验所
戴学东 大连市食品检验所
张敬波 大连市食品检验所
刘畅 大连市食品检验所
毛希琴 大连市食品检验所
姜俊 大连市食品检验所
庞丽 大连市食品检验所
中文关键词:香兰素,甲基香兰素,乙基香兰素,高效液相色谱串联质谱法,植物油,
英文关键词:vanillin,methyl vanillin,ethyl vanillin,high performance liquid chromatography tandem mass spectrometry,vegetable oil,
发表日期：2017-11-06
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