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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0.002~2μg/mL,回归方程为y=1958.4x+7600.4,相关系数为0.994,检出限为0.0004μg/mL。对0.2μg/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。
The rapid determination of rutin by capillary electrophoresis electrochemiluminescence (CE-ECL) was established. Rutin and five kinds of secondary amine were derivatized to obtain tertiary amines. UV scanning screening and CE-ECL detection were carried out. Ginkgo biloba samples using 70% aqueous ethanol ultrasound-assisted extraction. The effects of test potential, concentration and pH of test buffer and running buffer, injection voltage, separation voltage and time on the detection of rutin were investigated. Under the optimal experimental conditions, rutin was separated within 5 min. The linear range of the method was 0.002 ~ 2μg / mL, the regression equation was y = 1958.4x + 7600.4, the correlation coefficient was 0.994, the detection limit was 0.0004μg / mL. The RSDs of 0.2μg / mL rutin standard solution were detected seven times, and the RSDs of migration time, peak height and peak area were 1.1%, 1.2% and 2.0% respectively. This method was applied to the detection of rutin in Ginkgo biloba L. The recoveries were in the range of 92% -103%.