液相色谱-毛细管气相色谱/质谱离线联用分析烟草中的挥发性及半挥发性成分

建立了一种用于烟草样品中挥发性、半挥发性成分分析的液相色谱-毛细管气相色谱/质谱(LC-CGC/MS)离线联用方法。研究了LC-CGC/MS的分离机理。LC分析选用氨基分析柱(250 mm×2.0 mm, 5 μm)作为分析柱,正己烷-二氯甲烷-乙腈(90:6.6:3.4, v/v/v)作为流动相,对挥发性、半挥发性成分进行分离,收集得到5个馏分,并存放在5个氮吹瓶中。多次进样并收集相同时间段的馏分,氮吹浓缩至1 mL,然后分别进行CGC/MS分析,所用的CGC柱为DB-5MS(60 m×0.25 mm×0.25 μm)。结果显示,与直接采用CGC/MS分析相比,采用LC-CGC/MS分析复杂样本的效果更好,定性的可靠性更高。

Analysis of volatile and semi-volatile compounds in tobacco using off-line combination of liquid chromatography and capillary gas chromatography-mass spectrometry

A method of off-line combination of liquid chromatography and capillary gas chromatography-mass spectrometry (LC-CGC/MS) was established for the analysis of volatile and semi-volatile compounds in tobacco. The separation mechanism of volatile and semi-volatile compounds was studied. An LC column of 250 mm×2.0 mm packed with 5 μm amino-bonded silica was used as stationary phase for the separation. n-Hexane/dichloromethane/acetonitrile (90:6.6:3.4, v/v/v) was used as mobile phase. Five fractions from one LC run were collected in five nitrogen-blowing flasks, separately. The same fractions from 10 LC runs were combined together and concentrated to 1 mL by nitrogen blowing, and then were analyzed by CGC/MS. The column of DB-5MS (60 m×0.25 mm×0.25 μm) was used for CGC/MS analysis. Comparing with direct CGC/MS analysis of the same sample, the LC-CGC/MS system is suitable for a complex sample, and has a higher reliability of qualitative analysis.