Ilias Yara, Bieri Stefan, Christen Philippe, Veuthey Jean-Luc
Laboratory of Pharmaceutical Analytical Chemistry, School of Pharmaceutical Sciences EPGL, University of Geneva, University of Lausanne, 20, Bd. d'Yvoy, 1211 Geneva 4, Switzerland.
J Chromatogr Sci. 2006 Aug;44(7):394-8. doi: 10.1093/chromsci/44.7.394.
By its simplicity and rapidity, solid-phase microextraction (SPME) appears as an interesting alternative for sample introduction in fast gas chromatography (fast GC). This combination depends on numerous parameters affecting the desorption step (i.e., the release of compounds from the SPME fiber coating to the GC column). In this study, different liner diameters, injection temperatures, and gas flow rates are evaluated to accelerate the thermal desorption process in the injection port. This process is followed with real-time direct coupling a split/splitless injector to a mass spectrometer by means of a short capillary. It is shown that an effective, quantitative, and rapid transfer of cocaine (COC) and cocaethylene (CE) is performed with a 0.75-mm i.d. liner, at 280 degrees C and 4 mL/min gas flow rate. The 7-microm polydimethylsiloxane (PDMS) coating is selected for combination with fast GC because the 100-microm PDMS fiber presents some limitations caused by fiber bleeding. Finally, the developed SPME-fast GC method is applied to perform in less than 5 min, the quantitation of COC extracted from coca leaves by focused microwave-assisted extraction. An amount of 7.6 +/- 0.5 mg of COC per gram of dry mass is found, which is in good agreement with previously published results.
固相微萃取(SPME)因其简单性和快速性,似乎是快速气相色谱法(快速GC)中进样的一种有趣替代方法。这种组合取决于许多影响解吸步骤的参数(即化合物从SPME纤维涂层释放到GC柱中)。在本研究中,评估了不同的衬管直径、进样温度和气体流速,以加速进样口中的热解吸过程。通过一根短毛细管将分流/不分流进样器与质谱仪实时直接耦合来跟踪这个过程。结果表明,使用内径为0.75毫米的衬管,在280℃和4毫升/分钟的气体流速下,可实现可卡因(COC)和可口卡因(CE)的有效、定量和快速转移。选择7微米的聚二甲基硅氧烷(PDMS)涂层与快速GC联用,因为100微米的PDMS纤维存在一些因纤维流失导致的局限性。最后,所开发的SPME-快速GC方法用于在不到5分钟的时间内对通过聚焦微波辅助萃取从古柯叶中提取的COC进行定量。发现每克干物质中含有7.6±0.5毫克的COC,这与先前发表的结果高度一致。