液相色谱-串联质谱法同时测定 食用植物油中5种香料Simultaneous determination of 5 kinds of spices in edible vegetable oil by liquid chromatography-mass spectrometry

Abstract

为有效提高食用植物油中麦芽酚、乙基麦芽酚、香兰素、甲基香兰素和乙基香兰素的检测效率，建立同时测定食用植物油中麦芽酚、乙基麦芽酚、香兰素、甲基香兰素和乙基香兰素的液相色谱-串联质谱(HPLC-MS/MS)检测方法。样品经乙腈提取，正己烷脱脂后，采用甲醇-0.1%甲酸水溶液作为流动相进行梯度洗脱，质谱电喷雾离子源在正离子模式下进行多反应监测扫描，对5种香料进行定量测定。结果表明，5种香料质量浓度与峰面积线性关系良好,相关系数均大于0998, 方法检出限为2.3~19.5 μg/kg，定量限为7.7~65.0 μg/kg，回收率在85.0%~107.8%之间,相对标准偏差均小于50%。该方法操作简便、定性定量准确、灵敏度高，适用于食用植物油中麦芽酚、乙基麦芽酚、香兰素、甲基香兰素和乙基香兰素的同时测定，可有效提高检测效率。 In order to effectively improve detection efficiency of maltol, ethyl maltol, vanillin, methyl vanillin and ethyl vanillin in edible vegetable oil, a liquid chromatography-mass spectrometry (HPLC-MS/MS) method was established for the simultaneous determination of maltol, ethyl maltol, vanillin, methyl vanillin and ethyl vanillin in edible vegetable oil.The samples were extracted by acetonitrile and defatted by n-hexane,then methanol-0.1% formic acid aqueous solution was used as the mobile phase for gradient elution, electrospray ionization was used to conduct multiple reaction monitoring scanning under positive ion mode, and 5 kinds of spices were quantitatively determined. The results showed that the linear relationships were good between the mass fraction of spices and peak areas, and the correlation coefficients were higher than 0.998,the detection limits were 2.3-19.5 μg/kg, the quantitation limits were 7.7-65.0 μg/kg,the recovery rate were 85.0%-107.8%, and the relative standard deviations were less than 5.0%.The method is simple, accurate and sensitive. It is suitable for the simultaneous determination of maltol, ethyl maltol, vanillin, methyl vanillin and ethyl vanillin in edible vegetable oil, which can improve the detection efficiency effectively.

Keywords

• 液相色谱-串联质谱法；麦芽酚；乙基麦芽酚；香兰素；甲基香兰素；乙基香兰素
• liquid chromatography-mass spectrometry; maltol; ethyl maltol; vanillin; methyl vanillin; ethyl vanillin