气相色谱-质谱法测定烟草中五种醛类香料的含量

GC-MS Determination of 5 Aldehyde Flavours in Cigarettes

在每支合格卷烟中定量加入5种醛类香料的混合标准溶液,然后分别在4种不同的条件下保存48 h,迅速将每支卷烟的烟丝及过滤嘴取出,用同时蒸馏萃取器分离出其中的5种香料,用二氯甲烷作萃取溶剂。将萃取液蒸发至1 mL,加入乙酸苯乙酯作为内标,供气相色谱-质谱分析。在气相色谱分离中用PE-5MS毛细管柱作为固定相,在质谱测定中采用选择离子检测模式。香料标准与内标峰面积的比值与5种香料均在0.05～1.0 mg·L^(-1)范围内呈线性关系。5种香料的检出限(3S/N)在0.02～0.32 mg·L^(-1)之间。用标准加入法作回收试验,测得回收率在85.5%～91.9%之间,测定值的相对标准偏差(n=5)小于5.5%。

Mixed standard solution of five aldehyde flavours was added to each of the qualified cigarette samples which were then kept under 4 different conditions for 48 h. The cut tobacco and filter tip were taken out from the cigarettes and the 5 flavours were separated by the simultaneous distillation and extraction apparatus using dichloromethan as extraction solvent. The extract was evaporated to 1 mL, which was used for GC-MS analysis after adding phenylethyl acetate as internal standard. The PE-5MS capillary column was used for GC separation and the SIM mode was adopted in MS determination. Linear relationships between values of peak area ratios of the flavour standard to internal standard and mass concentration of each of the flavours obtained were same and in the range from 0. 05 to 1. 0 mg· L^-1. Values of detection limit （3S/N） found were in the range from 0. 02 to 0. 32 mg· L^-1. Recovery was tested by standard addition method, giving values of recovery in the range from 85. 5% to 91.9%, with values of RSD＇s （n=5） less than 5.5%.