HPLC法测定黄杨宁中环维黄杨星D和有关生物碱检查

HPLC determination of Cyclovirobuxinum D and its related alkaloids in Huangyangning

目的:建立黄杨宁中环维黄杨星 D 含量测定和有关生物碱检查的 HPLC 方法。方法:以氨丙基硅烷键合硅胶为填充剂(Lichrospher-NH_2),乙腈-0.4%的磷酸氢二钾溶液(70:30)为流动相,在柱温、流速和检测波长分别为40℃、1 mL·min^(-1)和210nm 的条件下,对黄杨宁进行直接 HPLC-UV 分析测定。结果:黄杨宁中环维黄杨星 D 与其有关生物碱 HPLC 分离良好,环维黄杨星 D 色谱峰面积与其浓度在0.020～1.00 mg·mL^(-1)范围,具有良好线性响应。结论:建立的氨丙基硅烷键合硅胶柱正相高效液相色谱法能准确、快速地测定黄杨宁中环维黄杨星 D 含量,同时适用于环维黄杨星 D 和黄杨宁制剂中有关生物碱的检查。

Objective： To establish an HPLC method for the determination of Cyclovirobuxinum D and its related alkaloids in Huangyangning. Methods： Cyclovirobuxinum D and its related alkaloids were separated and determined on a Lichrospher- NH2（250 mm ×4. 6mm,5μm） column with a mobile phase of acetonitrile-0. 4% dipotassiurn hydrogen phosphate solution（70： 30） and a flow rate of 1 mL ·min^-1 at 40℃ with the UV detection at 210 nm. Results：Under the established chromatographic conditions, Cyclovirobuxinum D was completely separated with its related alkaloids. The linear calibration curve of the peak area response to concentration was generated from 0. 020 to 1.00 mg·mL^-1 with a correlation coefficient of 0. 9998. Conclusions： The normal phase HPLC method with UV detection is simple and accurate for the assay and related alkaloids test of Cyclovirobuxinum D and its formulations.