气相色谱-质谱联用法测定加热卷烟烟草材料中8种凉味剂

Determination of eight cooling agents in tobacco materials for heated tobacco products by gas chromatography-mass spectrometry

为分析加热卷烟用烟草材料中凉味剂的种类及含量(质量分数),通过样品前处理及色谱条件优化,建立了一种基于气相色谱-质谱联用技术测定8种凉味剂的方法,并采用该方法分析了加热卷烟薄片、烟草粉末和烟丝中凉味剂的含量.结果表明:①该方法标准工作曲线在1.0~1000.0μg/mL之间线性良好,相关系数均大于等于0.9996,检出限和定量限分别为0.25~0.54和0.83~1.80μg/g,日内精密度和日间精密度分别为0.29%~2.60%和0.93%~3.35%,低、中、高3个水平下加标回收率分别为85.66%~109.36%、96.08%~105.47%和94.29%~104.12%,相对标准偏差(RSD)≤3.35%.②加热卷烟薄片、烟草粉末和烟丝中凉味剂的含量分别为0.65~29.40、0.15~6.23和0.01~3.94 mg/g(n=3),RSD为0.31%~2.14%.该方法简单、快速,灵敏度和准确度高,稳定性和重复性好,适用于同时检测不同加热卷烟烟草材料中的8种凉味剂.

In order to analyze the types and contents(mass fraction)of cooling agents in tobacco materials for heated tobacco products,a gas chromatography-mass spectrometry(GC-MS)method to quantify eight cooling agents was established by optimizing sample pretreatment and chromatographic conditions.The contents of the cooling agents in reconstituted tobacco,tobacco powder and cut tobacco for heated tobacco products were analyzed.The results showed that:1)The standard curve of this method had a good linear relationship between 1.0 and 1000.0μg/mL with the correlation coefficients of≥0.9996.The detection limits and quantitation limits of the method were 0.25-0.54 and 0.83-1.80μg/g,and intra-day precision and inter-day precision were 0.29%-2.60%and 0.93%-3.35%,respectively.The recoveries were 85.66%-109.36%,96.08%-105.47%and 94.29%-104.12%at low,medium and high levels,respectively.The relative standard deviations(RSD)were≤3.35%.2)The contents of the cooling agents in reconstituted tobacco,tobacco powder and cut tobacco for heated tobacco products were 0.65-29.40,0.15-6.23 and 0.01-3.94 mg/g(n=3)respectively,and RSDs ranged from 0.31%to 2.14%.The method is simple,rapid,sensitive,accurate,stable,reproducible,and suitable for the simultaneous detection of the eight cooling agents in different tobacco materials.