大米中三种香兰素的GC-MS分析方法

GC-MS Analysis of Three Vanillin in Rice

为了解香米中香料的添加情况,建立大米中香兰素、甲基香兰素及乙基香兰素的气相色谱质谱联用的分析方法。大米经乙酸乙酯溶剂萃取后经GC/MS测定,试验对大米中香兰素、甲基香兰素和乙基香兰素的提取条件及气相色谱质谱法分析条件进行了优化。结果:三种香兰素在10~1000μg/L质量浓度范围内线性关系均良好,香兰素的线性方程为y=23.63x-50.01;r^(2)=0.9998。甲基香兰素的线性方程为y=50.05x+605.2;r^(2)=0.9989;乙基香兰素的线性方程为y=44.54x+188.0;r^(2)=0.9999。方法定量限为50μg/kg。样品中分别定量加入20,100和200μg/kg的香兰素、甲基香兰素和乙基香兰素的混合标准溶液,进行6次平行处理和分析检测,回收率在94.3%~99.6%之间,相对标准偏差在0.19%~3.03%(n=6)之间。结论:该方法具有操作简单、准确性好、灵密度高等优点,适用于大批量的日常检测。

A gas chromatography-mass spectrometry(GC-MS)method was established for the determination of vanillin,methyl vanillin and ethyl vanillin in aromatic rice.The rice was extracted with ethyl acetate and determined by GC/MS.The extraction conditions and analysis conditions of vanillin,methyl and ethyl vanillin in rice by gas chromatography-mass spectrometry were optimized.Results:The linear relationship of vanillin was good in the concentration range of 10-1000μg/L.The linear equation of vanillin was y=23.63x-50.01;r^(2)=0.9998,The linear equation of methyl vanillin was y=50.05x+605.2;r^(2)=0.9989.The linear equation of ethyl vanillin was y=44.54x+188.0;r^(2)=0.9999.The limit of quantitation was 50μg/kg.The mixed standard solutions of vanillin,methyl vanillin and ethyl vanillin were quantitatively added into samples at the level of 20,100 and 200μg/kg,respectively,and analyzed for 6 times.The recoveries ranged from 94.3%to 99.6%,and the relative standard deviations(SRSD)ranged from 0.19%to 3.03%(n=6).Conclusion:The method had the advantages of simple operation,good accuracy and high sensitivity,and was suitable for daily detection of large quantities.