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在线偶合反相液相色谱和气相色谱:TOTAD 接口的新型密封设计。

On-line coupled reversed phase liquid chromatography and gas chromatography: a new sealing design for the TOTAD interface.

机构信息

Instituto de Ciencia y Tecnología de Alimentos y Nutrición (ICTAN), Consejo Superior de Investigaciones Científicas (CSIC), c/Juan de la Cierva 3, 28006 Madrid, Spain.

Instituto de Ciencia y Tecnología de Alimentos y Nutrición (ICTAN), Consejo Superior de Investigaciones Científicas (CSIC), c/Juan de la Cierva 3, 28006 Madrid, Spain.

出版信息

Talanta. 2014 Mar;120:23-9. doi: 10.1016/j.talanta.2013.11.083. Epub 2013 Dec 4.

Abstract

Total elimination of the eluent resulting from the pre-separation step is the critical point when coupling LC to GC. As a helium flow is applied during transfer to eliminate the solvent, the interface used for linking the two chromatographic systems must be properly sealed to prevent gas leaks and to achieve an effective evaporation of the eluent. The aim of this work was to improve the performance of the Through Oven Transfer Adsorption Desorption (TOTAD) interface to remove the eluent coming from LC by modifying the way in which the injector sealing system is held in place. As with the original design, the new approach makes it possible to transfer high volumes at a high rate, but the proposed modification also simplifies the experimental work because the displacement risk of the sealing system is reduced. Analyses of an ester mixture by RPLC-GC were performed to confirm the applicability of the system modification. In this work, volumes of up to 5 ml, at flow rates as high as 2 ml/min, were transferred from LC to GC with almost complete solvent removal even when working in reversed phase mode in the LC step.

摘要

当将 LC 与 GC 耦合时,从预分离步骤中完全消除洗脱液是关键。在转移过程中应用氦气流以去除溶剂时,用于连接两个色谱系统的接口必须正确密封,以防止气体泄漏并实现洗脱液的有效蒸发。本工作的目的是通过改进注射器密封系统的固定方式来提高 Through Oven Transfer Adsorption Desorption(TOTAD)接口从 LC 中去除洗脱液的性能。与原始设计一样,新方法可以实现高速率下的大体积传输,但所提出的改进还简化了实验工作,因为降低了密封系统的置换风险。通过 RPLC-GC 对酯混合物进行分析,以确认系统改进的适用性。在这项工作中,即使在 LC 步骤中处于反相模式下,也可以从 LC 向 GC 转移高达 5 ml 的体积,流速高达 2 ml/min,并且几乎完全去除了溶剂。

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