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液相色谱与毛细管气相色谱-质谱联用离线分析烟草中的挥发性和半挥发性化合物

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

作者信息

Bai Junchao, Liu Shaofeng, Xie Fuwei, Liu Huimin, Xia Qiaoling

机构信息

Zhengzhou Tobacco Research Institute of China National Tobacco Corporation, Zhengzhou 450001, China.

出版信息

Se Pu. 2010 Jun;28(6):608-14. doi: 10.3724/sp.j.1123.2010.00608.

Abstract

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 x 2.0 mm packed with 5 microm 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 x 0.25 mm x 0.25 microm) 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.

摘要

建立了一种液相色谱与毛细管气相色谱-质谱联用(LC-CGC/MS)的离线分析方法,用于烟草中挥发性和半挥发性化合物的分析。研究了挥发性和半挥发性化合物的分离机理。采用填充有5μm氨基键合硅胶的250mm×2.0mm液相色谱柱作为分离的固定相。以正己烷/二氯甲烷/乙腈(90:6.6:3.4,v/v/v)作为流动相。一次液相色谱运行的五个馏分分别收集在五个氮吹瓶中。将10次液相色谱运行的相同馏分合并在一起,通过氮吹浓缩至1mL,然后进行气相色谱/质谱分析。采用DB-5MS(60m×0.25mm×0.25μm)色谱柱进行气相色谱/质谱分析。与同一样品的直接气相色谱/质谱分析相比,LC-CGC/MS系统适用于复杂样品,且具有更高的定性分析可靠性。

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