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环糊精修饰的混合胶束电动毛细管色谱法同时分离和测定蛇足石杉及其制剂中的三种石杉碱甲。

Simultaneous separation and determination of three huperzine alkaloids in Huperzia serrata and its preparations by cyclodextrin-modified mixed micellar electrokinetic capillary chromatography.

机构信息

College of Pharmacy, Shanxi Medical University, Taiyuan, PR China.

Translational Medicine Research Center, Shanxi Medical University, Taiyuan, PR China.

出版信息

Anal Biochem. 2021 Jun 15;623:114207. doi: 10.1016/j.ab.2021.114207. Epub 2021 Apr 20.

Abstract

In this study, a simple and sensitive cyclodextrin-modified mixed micellar electrokinetic capillary chromatography (CD-MEKC) method has been developed for the simultaneous separation and determination of Huperzine A (HupA), Huperzine B (HupB) and Huperzine C (HupC) in Huperzia serrata (H. serrata). The optimal conditions (pH 9.3) were composed of 10 mM sodium tetraborate solution, 40 mM sodium dodecyl sulfate (SDS), 50 mM sodium cholate (SC) and 3.0 mM mono-(6-ethylenediamine-6-deoxy)-β-cyclodextrin (ED-β-CD). The separation and determination process were performed on a P/ACE MDQ capillary electrophoresis system, the separation voltage was 15 kV, the temperature was 25 °C and the detection wavelength was 308 nm. Under the optimum conditions, the migration time was less than 9 min. The LOD and LOQ were between 0.38 and 0.80 μg/mL and 1.2-2.3 μg/mL, respectively. The developed method, with excellent precision and accuracy, was applied for the determination of three alkaloids in H. serrata and its formulations.

摘要

在这项研究中,开发了一种简单灵敏的环糊精修饰混合胶束电动毛细管色谱法(CD-MEKC),用于同时分离和测定蛇足石杉中的石杉碱 A(HupA)、石杉碱 B(HupB)和石杉碱 C(HupC)。最佳条件(pH 9.3)由 10 mM 四硼酸钠溶液、40 mM 十二烷基硫酸钠(SDS)、50 mM 胆酸钠(SC)和 3.0 mM 单-(6-乙二胺-6-去氧)-β-环糊精(ED-β-CD)组成。分离和测定过程在 P/ACE MDQ 毛细管电泳系统上进行,分离电压为 15 kV,温度为 25°C,检测波长为 308nm。在最佳条件下,迁移时间小于 9 分钟。LOD 和 LOQ 分别在 0.38 至 0.80μg/mL 和 1.2 至 2.3μg/mL 之间。所开发的方法具有出色的精密度和准确性,用于测定蛇足石杉及其制剂中三种生物碱的含量。

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