液相色谱-串联质谱法同时测定大米中7种香料

Simultaneous determination of 7 spices in rice by liquid chromatography-tandem mass spectrometry

建立一种通过液相色谱-串联质谱法同时测定大米中7种香料(2-乙酰基吡嗪、2-乙酰基吡啶、乙基麦芽酚、香兰素、甲基香兰素、乙基香兰素、香豆素)的方法。大米样品以体积分数0.1%甲酸甲醇-水(体积比7∶3)为提取剂进行前处理,以体积分数0.1%甲酸水-体积分数0.1%甲酸甲醇为流动相进行液相色谱的梯度洗脱,采用正离子扫描多反应监测(+MRM)模式进行质谱检测。结果表明:7种香料在一定的质量浓度范围内线性关系良好,相关系数均大于0.998;方法的检出限为2.0~100.0μg/kg、定量限为5.0~300.0μg/kg、回收率为79.4%~113.0%、相对标准偏差(n=6)为2.3%~10.0%。

A method was established for simultaneous determination of 7 spices(2-acetylpyrazine,2-acetylpyridine,ethyl maltol,vanillin,methyl vanillin,ethyl vanillin,coumarin)in rice by liquid chro-matography-tandem mass spectrometry.The rice samples were pretreated with volume fraction 0.1%for-mic acid methanol-water(volume ratio 7:3)as the extraction agent.Gradient elution was carried out with volume fraction 0.1%formic acid water and volume fraction 0.1%formic acid methanol as mobile phase by liquid chromatography,and the positive ion scanning multi reaction monitoring(+MRM)mode was used for mass spectrometry detection.The results showed that the 7 spices had good linear relation-ships within a certain range of mass concentration,and the correlation coefficients were all greater than 0.998.The detection limit of the method was 2.0-100.0μg/kg,the quantification limit was 5.0-300.0μg/kg,the recovery rate was 79.4%-113.0%,and the relative standard deviation(n=6)was 2.3%-10.0%.