气相色谱-质谱法测定再造烟叶中甲酰胺

GC-MS Determination of Formamide in Reconstituted Tobacco

再造烟叶样品用甲醇提取5min,取上层清液,经有机相滤膜过滤,采用气相色谱-质谱法测定滤液中甲酰胺的含量。在气相色谱分离中采用DB-Wax毛细管色谱柱(0.32mm×30m,0.25μm),在质谱分析中采用选择离子监测模式。甲酰胺的质量浓度在0.1~5.0mg·L^-1内与其对应的峰面积呈线性关系,检出限(3S/N)为0.01mg·L^-1。加标回收率为92.5%~105%,测定值的日内相对标准偏差(n=6)为2.5%~3.0%,日间相对标准偏差(n=3)为4.4%。

The reconstituted tobacco sample was extracted for 5 min with methanol.The supernatant was taken and filtered with organic phase membrane.GC-MS was applied to the determination of formamide in the filtrate.DB-Wax capillary chromatographic column(0.32 mm×30 m,0.25μm)was used for GC separation and the selected ion monitoring mode was adopted in MS determination.Linear relationship between values of peak area and mass concentration of formamide was kept in the range of 0.1-5.0 mg·L^-1,with detection limit(3 S/N)of0.01 mg·L^-1.Values of recovery found by standard addition method were in the range of 92.5%-105%,and values of intra-day RSDs(n=6)of determined values were in the range of 2.5%-3.0% with inter-day RSD(n=3)of 4.4%.