气相色谱法测定电子烟烟液及气溶胶中双乙酰和乙酰丙酰

建立气相色谱法氢火焰离子化检测器测定电子烟烟液和气溶胶中双乙酰和乙酰丙酰含量的方法。样品以20 mL乙醇为萃取剂,涡旋振荡萃取10 min,采用气相色谱外标法进行定量分析。双乙酰和乙酰丙酰质量浓度在0.5~50 μg/mL范围内与色谱峰面积呈良好的线性关系,相关系数分别为0.999 6、0.999 4,方法检出限分别为0.044、0.052 μg/mL。烟液中双乙酰和乙酰丙酰测定结果的相对标准偏差为2.5%~4.3%(n=6),样品加标回收率为95.0%~102.5%;气溶胶中双乙酰和乙酰丙酰测定结果的相对标准偏差为3.1%~4.6%(n=6),样品加标回收率为92.7%~102.3%。气溶胶中双乙酰和乙酰丙酰理论浓度与实测浓度具有较强的相关性(对于双乙酰r~2=0.990 1,对于乙酰丙酰r~2=0.994 7),说明双乙酰、乙酰丙酰烟液通过雾化直接转移至气溶胶中。该方法准确度高,重现性好,检出限低,可满足电子烟样品的检测需求。

Determination of diacetyl and acetylpropionyl in e-cigarette liquid and aerosol by gas chromatography

A method for determining diacetyl and acetopropionyl in electronic cigarette liquid and aerosol by gas chromatography with hydrogen flame ionization detector was established.After being extracted with 20 mL ethanol as extractant,the samples were extracted by vortex oscillation for 10 min.The external standard method of gas chromatography was used for quantitative analysis.There was a good linear relationship between the mass concentration of diacetyl and acetopropionyl with chromatographic peak area in the range of 0.5–50μg/mL,the correlation coefficients were 0.9996 and 0.9994,and the detection limits were 0.044 and 0.052μg/mL,respectively.The relative standard deviations of diacetyl and acetopropionyl in cigarette smoke were 2.5%–4.3%(n=6),and the recoveries of spiked samples were 95.0%–102.5%;the relative standard deviations of diacetyl and levulinyl in aerosol were 3.1%–4.6%(n=6),and the recoveries of spiked samples were 92.7%–102.3%.There was a strong correlation between the theoretical concentration of diacetyl and acetylpropionyl in aerosol and the measured concentration(for diacetyl r2=0.9901,for acetylpropionyl r2=0.9947),indicating that diacetyl and levulinyl were directly transferred into aerosol through atomization.The method has the advantages of high accuracy,good reproducibility and low detection limit,which can meet the detection requirements of electronic cigarette samples.