Wang Xiaozhong, Li Xuwen, Li Lanjie, Li Min, Liu Ying, Wu Qian, Li Peng, Jin Yongri
College of Chemistry, Jilin University, Changchun, China.
School of Chemistry and Chemical Engineering, Ningxia University, Yinchuan, China.
J Sep Sci. 2016 May;39(10):1971-8. doi: 10.1002/jssc.201600118. Epub 2016 May 3.
A simple and sensitive method for determination of three aconitum alkaloids and their metabolites in human plasma was developed using matrix solid-phase dispersion combined with vortex-assisted dispersive liquid-liquid microextraction and high-performance liquid chromatography with diode array detection. The plasma sample was directly purified by matrix solid-phase dispersion and the eluate obtained was concentrated and further clarified by vortex-assisted dispersive liquid-liquid microextraction. Some important parameters affecting the extraction efficiency, such as type and amount of dispersing sorbent, type and volume of elution solvent, type and volume of extraction solvent, salt concentration as well as sample solution pH, were investigated in detail. Under optimal conditions, the proposed method has good repeatability and reproducibility with intraday and interday relative standard deviations lower than 5.44 and 5.75%, respectively. The recoveries of the aconitum alkaloids ranged from 73.81 to 101.82%, and the detection limits were achieved within the range of 1.6-2.1 ng/mL. The proposed method offered the advantages of good applicability, sensitivity, simplicity, and feasibility, which makes it suitable for the determination of trace amounts of aconitum alkaloids in human plasma samples.
建立了一种简单灵敏的方法，采用基质固相分散结合涡旋辅助分散液液微萃取和二极管阵列检测高效液相色谱法，测定人血浆中三种乌头生物碱及其代谢物。血浆样品通过基质固相分散直接纯化，所得洗脱液经涡旋辅助分散液液微萃取浓缩并进一步澄清。详细研究了影响萃取效率的一些重要参数，如分散吸附剂的类型和用量、洗脱溶剂的类型和体积、萃取溶剂的类型和体积、盐浓度以及样品溶液的pH值。在最佳条件下，该方法具有良好的重复性和重现性，日内和日间相对标准偏差分别低于5.44%和5.75%。乌头生物碱的回收率在73.81%至101.82%之间，检测限在1.6 - 2.1 ng/mL范围内。该方法具有良好的适用性、灵敏度、简单性和可行性，适用于测定人血浆样品中痕量乌头生物碱。
