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具有快速对映体分离功能的全二维气相色谱法

Comprehensive two-dimensional gas chromatography with fast enantioseparation.

作者信息

Shellie Robert, Marriott Philip J

机构信息

Australian Centre for Research on Separation Science, Department of Applied Chemistry, RMIT University, Melbourne, Victoria.

出版信息

Anal Chem. 2002 Oct 15;74(20):5426-30. doi: 10.1021/ac025803e.

Abstract

The development of fast chiral analysis for use in comprehensive two-dimensional gas chromatography in which a short second dimension enantioselective capillary column provides a route to precise measurement of chiral ratios of enantiomers is described. Retention times as short as 8 s are reported for (+/-)-limonene, with adequate enantioseparation maintained (Rs approximately 1.0) on a 1-m cyclodextrin derivative-coated capillary column. Sufficiently fast elution on the second column was achieved by using GC/ MS in which the subambient pressure (vacuum outlet) conditions promote increased diffusion coefficients and higher component volatility; a 4-fold reduction of second-dimension retention time was observed, as compared with ambient pressure outlet conditions. The enantiomeric distribution of several monoterpene compounds in bergamot essential oil is reported as a demonstration of the method. Total analysis time of the target components was approximately 8.5 min.

摘要

描述了用于全二维气相色谱的快速手性分析方法的发展,其中短的第二维对映体选择性毛细管柱为精确测量对映体的手性比例提供了途径。据报道,(±)-柠檬烯的保留时间短至8秒,在1米的环糊精衍生物涂覆的毛细管柱上保持了足够的对映体分离度(Rs约为1.0)。通过使用气相色谱/质谱联用,在第二根柱上实现了足够快的洗脱,其中低于环境压力(真空出口)条件促进了扩散系数的增加和组分挥发性的提高;与环境压力出口条件相比,观察到第二维保留时间减少了4倍。报道了佛手柑精油中几种单萜化合物的对映体分布,作为该方法的一个实例。目标组分的总分析时间约为8.5分钟。

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