固相萃取-气相色谱/质谱联用法测定卷烟主流烟气中的香兰素和乙基香兰素

采用固相萃取-气相色谱/质谱联用技术,建立了一种同时测定卷烟主流烟气中香兰素和乙基香兰素的方法。方法优化了萃取条件,考察了萃取溶剂、萃取时间对检测结果的影响。通过硅藻土固相萃取柱净化并浓缩后,选取DB-HeavyWAX毛细管柱进行目标物分离,以香兰素-d3作为内标,对香兰素和乙基香兰素进行定量分析。结果表明,香兰素和乙基香兰素在浓度0.2~20.0 mg/L范围内具有良好的线性关系,其检出限分别为9.1 ng/支和6.5 ng/支,回收率均在96.3%~107.7%之间。

Determination of vanillin and ethyl vanillin in mainstream cigarette smoke by solid phase extraction-gas chromatography/mass spectrometry

Solid phase extraction-gas chromatography/mass spectrometry was applied to the determination of vanillin and ethyl vanillin in mainstream cigarette smoke.The parameters affecting extraction efficiency such as extraction solvent and extraction time were investigated and optimized.The target was first purified and concentrated by diatomite solid phase extraction column,and further separated by the gas chromatography employed DB-HeavyWAX capillary column.Vanillin-d3 was used as internal standard to quantify vanillin and ethyl vanillin.The results showed that the ratio of peak area and the concentrations of vanillin and ethyl vanillin kept a satisfied linear relation ship in the range of 0.2-20.0 mg/L,and the limits of detection for vanillin and ethyl vanillin were 9.1 ng/cig and 6.5 ng/cig,respectively.The recoveries of vanillin and ethyl vanillin ranged from 96.3%to 107.7%.