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目的建立卷烟中保湿剂(丙二醇、甘油及三甘醇)的气相色谱测定方法。方法卷烟样品在温度(22±1)℃、湿度(60±3)%条件下平衡12 h后称重,用含有2 mg/ml 1,3-丁二醇内标的甲醇溶液振荡提取1 h并过滤后进样,经气相色谱分离后,火焰离子化检测器检测,以保留时间定性,以内标法定量。结果该方法对丙二醇、甘油、三甘醇的检出限分别为0.000 9、0.002 0、0.002 1 mg/ml,测定下限分别为0.003 6、0.008 0、0.008 4 mg/ml,按照4 g烟草样品计算测定范围分别为0.04~10.21、0.10~40.18、0.10~10.18 mg/g。对不同浓度的实际样品测定的日间精密度(以相对标准偏差表示)范围为1.76%~7.05%,高、中、低浓度加标回收率范围为96.7%~110.3%。结论该方法前处理过程简单快捷,测定灵敏、准确,适用于卷烟中保湿剂的测定。
Objective To establish a method for the determination of humectants (propylene glycol, glycerol and triethylene glycol) in cigarettes by gas chromatography. Methods The cigarette samples were weighed and equilibrated for 12 h at temperature (22 ± 1) ℃ and humidity (60 ± 3)%. The cigarette samples were extracted with methanol solution containing 2 mg / ml 1,3-butanediol After filtration, the sample was separated by gas chromatography and detected by flame ionization detector. The retention time was qualitatively determined by internal standard method. Results The detection limits of this method were 0.000 9,0.002 0,0.002 1 mg / ml for propylene glycol, glycerol and triethylene glycol respectively. The lower limits of determination were 0.003 6,0.008 0,0.008 4 mg / ml respectively. According to 4 g tobacco samples The calculated range was 0.04 ~ 10.21,0.10 ~ 40.18,0.10 ~ 10.18 mg / g, respectively. The daytime precision (relative standard deviation) of different concentrations of real samples ranged from 1.76% to 7.05%. The recoveries ranged from 96.7% to 110.3% for high, medium and low concentrations. Conclusion The pretreatment process of the method is simple and quick, sensitive and accurate, and suitable for the determination of humectants in cigarettes.