Shrivas Kamlesh, Wu Hui-Fen
Department of Chemistry, National Sun Yat-Sen University, Kaohsiung 804, Taiwan.
J Chromatogr A. 2007 Nov 2;1170(1-2):9-14. doi: 10.1016/j.chroma.2007.09.020. Epub 2007 Sep 14.
A simple and rapid sample cleanup and preconcentration method for the quantitative determination of caffeine in one drop of beverages and foods by gas chromatography/mass spectrometry (GC/MS) has been proposed using drop-to-drop solvent microextraction (DDSME). The best optimum experimental conditions for DDSME were: chloroform as the extraction solvent, 5 min extraction time, 0.5 microL exposure volume of the extraction phase and no salt addition at room temperature. The optimized methodology exhibited good linearity between 0.05 and 5.0 microg/mL with correlation coefficient of 0.980. The relative standard deviation (RSD) and limits of detection (LOD) of the DDSME/GC/MS method were 4.4% and 4.0 ng/mL, respectively. Relative recovery of caffeine in beverages and foods were found to be 96.6-101%, which showing good reliability of this method. This DDSME excludes the major disadvantages of conventional method of caffeine extraction, like large amount of organic solvent and sample consumption and long sample pre-treatment process. So, this approach proves that the DDSME/GC/MS technique can be applied as a simple, fast and feasible diagnosis tool for environmental, food and biological application for extremely small amount of real sample analysis.
提出了一种简单快速的样品净化和预浓缩方法,即采用逐滴溶剂微萃取(DDSME),通过气相色谱/质谱联用(GC/MS)定量测定一滴饮料和食品中的咖啡因。DDSME的最佳实验条件为:氯仿作为萃取溶剂,萃取时间5分钟,萃取相暴露体积0.5微升,室温下不添加盐。优化后的方法在0.05至5.0微克/毫升之间呈现良好的线性,相关系数为0.980。DDSME/GC/MS方法的相对标准偏差(RSD)和检测限(LOD)分别为4.4%和4.0纳克/毫升。饮料和食品中咖啡因的相对回收率为96.6 - 101%,表明该方法具有良好的可靠性。这种DDSME排除了传统咖啡因萃取方法的主要缺点,如大量有机溶剂和样品消耗以及较长的样品预处理过程。因此,该方法证明DDSME/GC/MS技术可作为一种简单、快速且可行的诊断工具,用于环境、食品和生物领域极少量实际样品的分析。