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Evaluation of Solid-Phase Microextraction Desorption Parameters for Fast GC Analysis of Cocaine in Coca Leaves

机译:固相微萃取解吸参数评估古柯叶中可卡因的快速气相色谱分析

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摘要

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°C and 4 mL/min gas flow rate. The 7-µm polydimethylsiloxane (PDMS) coating is selected for combination with fast GC because the 100- µm 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
机译:固相微萃取(SPME)简便易行,是快速气相色谱(快速GC)中样品引入的有趣替代方法。这种结合取决于影响解吸步骤(即化合物从SPME纤维涂层到GC色谱柱的释放)的众多参数。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脱附过程。此过程之后,通过短毛细管将分流/不分流进样器实时直接耦合到质谱仪。结果表明,以0.75毫米内径进行有效,定量和快速的可卡因(COC)和可卡乙烯(CE)转移。衬里,在280°C和4 mL / min的气体流速下。选择7 µm的聚二甲基硅氧烷(PDMS)涂层与快速GC结合使用,因为100 µm的PDMS纤维存在因纤维渗出引起的某些限制。最后,将开发的SPME-fast GC方法应用于在不到5分钟的时间内完成通过聚焦微波辅助提取从古柯叶中提取的COC的定量分析。每克干物质发现7.6±0.5毫克COC,与先前公布的结果非常吻合

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