GC-MS/MS法测定烟草中的57种酯类香味成分

Determination of 57 ester aroma components in tobacco by gas chromatography-tandem mass spectrometry

为提高烟草中酯类香味成分的检测水平,建立了酸性条件泡发、乙腈提取、无水MgSO4除水、GC-MS/MS法同时测定烟草中57种关键酯类香味成分的分析方法,优化了质谱参数,考察了提取方式、提取溶剂、泡发液pH、泡发时间、涡旋时间和净化方式对提取效率的影响,并采用本方法检测了15个不同风格的卷烟样品。结果表明:①采用多反应监测模式(dMRM)定量时,57种酯类香味成分标准工作曲线线性关系良好,3个添加水平下,平均回收率在62.5%~128.7%之间,相对标准偏差为0.5%~25.4%,方法的定量限在3~74μg/kg之间。②方法准确度和灵敏度较高、操作简便,可满足烟草中酯类香味成分分析需要。③在卷烟样品中共检出31种酯类香味成分,t检验筛选出8种具有差异性的酯类成分;偏最小二乘法判别分析(PLS-DA)表明筛选出的指标能够区分不同风格的卷烟样品。

To detect the ester aroma components in tobacco more accurately and rapidly,a gas chromatography-tandem mass spectrometry(GC-MS/MS)method was developed on the basis of acidic solution soaking,acetonitrile extraction and anhydrous magnesium sulfate dehydration,and 57 key ester aroma components in tobacco were analyzed simultaneously.The mass spectrometry parameters were optimized,and the effects of extraction type,extraction solvent,pH value of soaking solution,soaking time,vortex time and purification method on extraction efficiency were investigated.The samples of 15 types of cigarettes of different styles were analyzed by the developed method.The results showed that:1)The calibration curve of all the esters presented good linearity when quantitatively analyzing under multiple reaction monitoring mode(dMRM).The average recoveries ranged from 62.5%to 128.7%with the relative standard deviations between 0.5%and 25.4%at three spiked levels.The limits of quantitation(LOQs)were in the range of 3-74μg/kg.2)This method was accurate,sensitive,convenient and met the needs of analysis of ester aroma components in tobacco.3)Thirty-one ester aroma components were detected in cigarette samples,in which 8 components with significant differences were screened out by t test.The results of Partial Least Square Discriminant Analysis(PLS-DA)indicated that the selected indexes could distinguish cigarette samples of different styles.