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采用微切换和低温调制的靶向多维气相色谱法。

Targeted multidimensional gas chromatography using microswitching and cryogenic modulation.

作者信息

Marriott Philip, Dunn Michael, Shellie Robert, Morrison Paul

机构信息

Australian Centre for Research on Separation Science, Department of Applied Chemistry, RMIT University, GPO Box 2476V, Melbourne 3001, Australia.

出版信息

Anal Chem. 2003 Oct 15;75(20):5532-8. doi: 10.1021/ac034492k.

Abstract

A new method is described that allows fast target analysis in multidimensional gas chromatography by using a microswitching valve between two GC columns, with cryogenic trapping and rapid re-injection of trapped solutes in the second dimension. The essence of the procedure is that heart-cut fractions from the first column (1D) can be selectively transferred to column 2 (2D), where a moveable cryogenic trap first focuses the transferred solute(s) at the head of the second column and then permits their facile rapid analysis on 2D. Since 2D is a short narrow-bore column, which exhibits very fast analysis (on the order of a few seconds elution), peak responses (heights) are significantly enhanced (by up to 40-fold). Additionally, by using a 2D phase of a selectivity different from that used for 1D, it is possible to also separate components that are not resolved on the first column and to increase the resolution for other compounds. The heart-cut valve isolates the section(s) of solutes of interest from the first column separation, and this provides a considerable simplification to the chromatogram-in addition to the separation and sensitivity advantages. By using this method, multidimensional gas chromatography with multiple heart-cuts can be completed within the same time as the primary column separation. Since the described method permits non-heart-cut fractions to be transferred to a monitor detector, normal detection of these fractions is still permitted. By modulation of the cryotrap, it is also possible to achieve comprehensive two-dimensional gas chromatography for the heart-cut fractions; however, only those compounds passed to the second, separation column, which passes through the cryotrap, will be subjected to GC x GC analysis. The technique and the various modes of operation are described in this paper.

摘要

本文描述了一种新方法,该方法通过在两根气相色谱柱之间使用微型切换阀,结合低温捕集和将捕集的溶质快速重新进样到第二维,实现多维气相色谱中的快速目标分析。该方法的核心是,第一根色谱柱(1D)的中心切割馏分可以选择性地转移到色谱柱2(2D),在那里一个可移动的低温捕集器首先将转移的溶质聚焦在第二根色谱柱的柱头,然后对其进行二维快速分析。由于二维是一根短的窄口径色谱柱,具有非常快的分析速度(洗脱时间约为几秒),峰响应(峰高)显著增强(高达40倍)。此外,通过使用与一维不同选择性的二维固定相,还可以分离在第一根色谱柱上未分离的组分,并提高其他化合物的分离度。中心切割阀将感兴趣的溶质部分与第一根色谱柱的分离部分隔离开来,这除了具有分离和灵敏度优势外,还大大简化了色谱图。使用该方法,多次中心切割的多维气相色谱可以在与主色谱柱分离相同的时间内完成。由于所描述的方法允许非中心切割馏分转移到监测检测器,因此仍然可以对这些馏分进行正常检测。通过调节低温捕集器,还可以对中心切割馏分实现全二维气相色谱;然而,只有那些进入第二根分离柱并通过低温捕集器的化合物才会进行全二维气相色谱分析。本文介绍了该技术及各种操作模式。

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