在更环保(绿色)的溶剂和萃取效率方面,优化了具有三个平行的3.5cm长和100μm宽的互连通道的玻璃液-液萃取(LLE)微芯片。此外,优化后的芯片成功地与纳米液相色谱-紫外和质谱检测(nanoLC-UV-MS)联用,用于在线分析。在这个系统中,样品预处理,分离和检测是一体的,这大大缩短了分析时间,节省劳动力,大大减少溶剂消耗。以士的宁作为模型分析物以确定优化的3相芯片的提取效率。有机溶剂的影响,进料相的pH值,生物碱的类型,和流速进行了调查。结果表明,三相芯片nanoLC-UV/MS联用结合了快速(~25s)和高效(提取效率>90%)的样品制备,自动生物碱分析。该方法适用于实际样品,包括马钱子种子,Cephaelisipecacuanha根,颠茄叶,和Vinca小叶。
A glass liquid-liquid extraction (LLE) microchip with three parallel 3.5 cm long and 100 μm wide interconnecting channels was optimized in terms of more environmentally friendly (greener) solvents and extraction efficiency. In addition, the optimized chip was successfully hyphenated with nano-liquid chromatography with ultraviolet and mass spectrometric detection (nanoLC-UV-MS) for on-line analysis. In this system, sample pretreatment, separation and detection are integrated, which significantly shortens the analysis time, saves labor and drastically reduces solvent consumption. Strychnine was used as model analyte to determine the extraction efficiency of the optimized 3-phase chip. Influence of organic solvent, pH of feed phase, type of alkaloid, and flow rates were investigated. The results demonstrated that the 3-phase chip nanoLC-UV/MS hyphenation combines rapid (~25 s) and efficient (extraction efficiency >90%) sample prep, with automated alkaloid analyses. The method was applied to real samples including Strychnos nux-vomica seeds, Cephaelis ipecacuanha roots, Atropa belladonna leaves, and Vinca minor leaves.