气相色谱质谱法测定6种加香目标物质的含量及对烟丝加香均匀性的评价

建立了一种运用气相色谱-质谱联用技术(GC-MS)同时测定卷烟烟丝中呋喃酮、异戊酸异戊酯、麦芽酚、薄荷醇、乙基麦芽酚和茴香脑6种烟用加香目标物的检测方法。试样用二氯甲烷溶液振荡提取,旋转蒸发仪浓缩,气相色谱-质谱联用仪检测分析。分别对样品量、萃取溶剂和萃取时间等前处理条件进行了优化。该方法的线性相关系数r均在0.998以上,采用SIM法定量分析,其平均加标回收率为86%～92%,相对标准偏差(RSD,n=6)为4.7%～7.1%,检出限(S/N=3)和定量下限(S/N=10)分别为0.014 7～0.0746μg/g和0.048 9～0.248 8μg/g。结果表明,该方法简便、灵敏度高、线性关系好,能满足同时测定烟丝中此6种加香目标物质的要求。方法还通过测定烟丝样品中加香目标物的含量及其含量的RSD值对卷烟制丝工艺加香的均匀性进行了评价。

Determination of Six Flavoring Characteristic Compounds by GC-MS and Its Evaluation on the Flavoring Uniformity in Cigarette

A gas chromatography-mass spectrometric(GC-MS) method was established for the simultaneous determination of 6 kinds of characteristic compounds,including furaneol,isoamyl isovalerate,maltol,menthol,ethyl maltol and anethole in cigarette.The sample was extracted with dichloromethane solution,concentrated with the rotary evaporation instrument,and analyzed by GC-MS.The conditions for sample preparation(e.g.sample volume,extraction solvent and extraction time) were optimized.Under the optimal conditions,the correlation coefficients of 6 analytes were higher than 0.998.The average spiked recoveries were in the range of 86%-92% with relative standard deviations(RSDs,n=6)of 4.7%-7.1%.The detection limits(S/N=3)and quantitation limits(S/N=10) were in the range of 0.014 7-0.074 6 μg/g and 0.048 9-0.248 8 μg/g,respectively.The method showed good extraction efficiency,high sensitivity and good reproducibility,and was suitable for the simultaneous detection of 6 compounds in cigarette flavoring.The results also indicated that the method could be used for the evaluation of the uniformity of cigarette flavoring on the processing line through determination of the characteristic compound contents in samples.