[关键词]
[摘要]
建立了芦丁的毛细管电泳电化学发光(CE-ECL)快速分离检测方法。将芦丁与五种仲胺进行衍生反应得到叔胺类化合物,先进行紫外扫描筛选,再将进行CE-ECL检测。银杏叶样品采用70%乙醇水溶液超声波辅助提取。考察检测电位、检测池缓冲液和运行缓冲液的浓度和pH值、进样电压、分离电压和时间等因素对芦丁分离检测的影响。在最佳实验条件下,芦丁在5 min内实现分离。该方法的线性范围为0.002~2 μg/mL,回归方程为y=1958.4x+7600.4,相关系数为0.994,检出限为0.0004 μg/mL。对0.2 μg/mL芦丁标准溶液衍生物进行7次检测,其迁移时间、峰高和峰面积的RSD分别为1.1%、1.2%和2.0%。此方法应用于银杏叶中芦丁的检测,加标回收率在92%~103%之间。
[Key word]
[Abstract]
A rapid and efficient separation method was established for the determination of rutin by capillary electrophoresis- electrochemiluminescence (CE-ECL). Tertiary amine compounds, obtained by derivatization reaction of rutin and five secondary amines, were screened by UV, and then detected by CE-ECL. Ginkgo leaf samples were extracted with 70% ethanol aqueous solution by ultrasonic-assisted extraction. The influences of detection potential, concentration and pH of separation buffer and running buffer, separation voltage, injection voltage and injection time on the separation and detection of rutin were investigated. Under the optimal conditions, rutin was separated in 5 minutes, and the linear concentration range for rutin was 0.002~2 μg/mL. Besides, the regression equation was y=1958.4x+7600.4, with a correlation coefficient of 0. 994 and a detection limit of 0.0004 μg/mL (S/N=3). The relative standard deviations (RSD) of migration time, peak height and peak area for seven continuous injections of 0.2 μg/mL rutin were 1.1%, 1.2% and 2.0%, respectively. The proposed method was applied to the determination of the rutin in Ginkgo leaf with the recoveries of 92% -103%.
[中图分类号]
[基金项目]
陕西省科技厅农业科技创新与攻关项目(2015NY130);陕西理工大学研究生创新基金项目(SLGYCX1623);陕西理工大学博士后专项项目(SLGBH16-01)