Gong Aiqin, Zhu Xiashi
College of Chemistry & Chemical Engineering, Yangzhou University, Yangzhou 225002, PR China; Yangzhou Polytechnic Institute, Yangzhou 225127, PR China.
College of Chemistry & Chemical Engineering, Yangzhou University, Yangzhou 225002, PR China.
Spectrochim Acta A Mol Biomol Spectrosc. 2016 Apr 15;159:163-8. doi: 10.1016/j.saa.2016.01.053. Epub 2016 Jan 27.
In this study, for the first time, a coupled 1-mL microsyringe system was utilized to perform a miniaturized ionic liquid dispersive liquid-liquid microextraction (IL-DLLME) method. Danazol was extracted and determined via the developed method followed by micro-volume ultraviolet spectroscopy (UV). The extraction process was carried out by the injection of extraction solvent ionic liquid 1-octyl-3-methylimidazolium hexafluorophosphate [C8mimPF6] into sample solution (syringe A), and then rapid shoot the solution into syringe B. After that the shooting was repeated several times at a rate of 1 cycle/s. The extraction procedure was induced by the formation of cloudy solution, which was composed of fine drops of [C8mimPF6] dispersed entirely into sample solution with the help of shooting without any dispersive solvent, ultrasonication or high temperature. Several important parameters affecting the extraction efficiency were studied and optimized. Under the optimized conditions, the limit of detection (LOD) was 0.055 μg/mL (capsule) or 0.054 μg/mL (serum) at a signal-to-noise ratio of 3. The calibration curve was linear over the range of 0.62-25 μg/mL. The proposed method was successfully applied to danazol capsule and the real mice serum samples and good spiked recoveries in the range of 90.5-103.4% were obtained. The obtained results of this work were in good agreement with the results of HPLC.
在本研究中，首次利用耦合1 mL微注射器系统进行了小型化离子液体分散液液微萃取（IL-DLLME）方法。通过所开发的方法萃取并测定达那唑，随后采用微量紫外光谱法（UV）进行检测。萃取过程是通过将萃取溶剂离子液体1-辛基-3-甲基咪唑六氟磷酸盐[C8mimPF6]注入样品溶液（注射器A），然后迅速将溶液注入注射器B来进行的。之后，以1次循环/秒的速率重复注射几次。萃取过程是由形成浑浊溶液引发的，该浑浊溶液是由[C8mimPF6]的细滴在不借助任何分散溶剂、超声处理或高温的情况下，通过注射完全分散到样品溶液中形成的。研究并优化了几个影响萃取效率的重要参数。在优化条件下，信噪比为3时，检测限（LOD）为0.055 μg/mL（胶囊）或0.054 μg/mL（血清）。校准曲线在0.62 - 25 μg/mL范围内呈线性。所提出的方法成功应用于达那唑胶囊和实际小鼠血清样品，加标回收率良好，在90.5 - 103.4%范围内。本工作获得的结果与高效液相色谱法的结果高度一致。
