Gagné Jean-Pierre, Gouteux Bruno, Bertrand Michel J
Laboratoire d'analyses et d'études en géochimie organique (LAEGO), Institut des sciences de la mer de Rimouski, Université du Québec à Rimouski, 310 allée des Ursulines, Rimouski, Québec, Canada G5L 3A1.
J Chromatogr A. 2009 Jan 16;1216(3):442-8. doi: 10.1016/j.chroma.2008.09.083. Epub 2008 Oct 1.
A new type of injector has been developed for gas chromatographic analysis. The injector has high volume and band compression (HVBC) capabilities useful for the analysis of complex samples. The injector consists essentially of a packed liner operated at room temperature while a narrow heated zone is used to axially scan the liner selectively desorbing the compounds of interest. The scanning speed, distance and temperature of the zone are precisely controlled. The liner is connected to an interface which can vent the solvent or any undesirable compounds, and transfer the analytes to an analytical column for separation and quantification. The injector is designed to be compatible with injection volumes from 1 to more than 250microL. At a low sample volume of 1microL, the injector has competitive performances compared to those of the "on-column" and "split/splitless" injectors for the fatty acid methyl esters and toxaphene compounds tested. For higher volumes, the system produces a linear response according to the injected volume. In this explorative study, the maximum volume injected seems to be limited by the saturation of the chromatographic system instead of being defined by the design of the injector. The HVBC injector can also be used to conduct "in situ" pretreatment of the sample before its transfer to the analytical column. For instance, a toxaphene sample was successively fractionated, using the HVBC injector, in six sub-fractions characterized by simpler chromatograms than the chromatogram of the original mixture. Finally, the ability of the HVBC injector to "freeze" the separation in time allowing the analyst to complete the analysis at a later time is also discussed.
已开发出一种用于气相色谱分析的新型进样器。该进样器具有高进样量和谱带压缩(HVBC)能力,对复杂样品的分析很有用。进样器主要由一个在室温下操作的填充衬管组成,同时使用一个狭窄的加热区轴向扫描衬管,选择性地解吸感兴趣的化合物。该区域的扫描速度、距离和温度可精确控制。衬管连接到一个接口,该接口可以排出溶剂或任何不需要的化合物,并将分析物转移到分析柱进行分离和定量。该进样器设计为与1至超过250微升的进样体积兼容。在1微升的低样品体积下,与测试的脂肪酸甲酯和毒杀芬化合物的“柱上进样”和“分流/不分流”进样器相比,该进样器具有竞争力的性能。对于更高的进样体积,系统根据进样体积产生线性响应。在这项探索性研究中,最大进样体积似乎受色谱系统饱和度的限制,而不是由进样器的设计决定。HVBC进样器还可用于在将样品转移到分析柱之前对其进行“原位”预处理。例如,使用HVBC进样器将毒杀芬样品连续分馏成六个子馏分,其色谱图比原始混合物的色谱图更简单。最后,还讨论了HVBC进样器在时间上“冻结”分离从而使分析人员能够在以后完成分析的能力。