HPLC法测定中药常山散中常山乙素、常山甲素的系统适用性研究

Study on system suitability of high performance liquid chromatography for measuring β-dichroine and α-dichroine in Dichroa febrifuga powder

【目的】为制订中药常山散的国家质量标准和指导临床科学用药,进行了高效液相色谱法测定常山乙素、常山甲素含量的系统适用性研究.【方法】选择3种不同类型的液相和色谱柱,包括安捷伦1290型液相色谱仪(配套SB-C_(18)色谱柱)、沃特斯2695型液相色谱仪(配套XTerra@MS C_(18)色谱柱)和岛津SPD-10A型液相色谱仪(配套Amethyst C_(18)-H色谱柱).流动相:乙腈-0.3%冰醋酸(30∶70),三乙胺调pH值至5.2～6.2,流速:1.0mL/min,检测波长:265nm,柱温:25℃,进样量:10μL.【结果】3种类型的高效液相检测结果表明,三批次常山散中常山乙素和常山甲素的含量基本一致,常山乙素和常山甲素峰型较好,与周围杂质分离度较好.【结论】以上色谱条件可用来检测常山散中常山乙素和常山甲素的含量,适用于中药常山散及其相关制剂的质量控制,具有操作简便、稳定性好、精密度高等优点.

【Objective】In order to establish the national quality standard of Dichroa febrifuga powder and guide the clinical medication,the system suitability of high performance liquid chromatography(HPLC)method was studied for the test ofβ-dichroine andα-dichroine in D.febrifuga powder.【Method】Three different types of liquid phase and chromatographic column were chosen,including Agilent 1290 type liquid chromatograph(supporting SB-C 18 chromatographic column),Waters 2695 type liquid chromatograph(supporting XTerra@MS C 18 chromatographic column)and Island ferry SPD-10A type liquid chromatograph(supporting the Amethyst C 18-H chromatographic column).Mobile phase:acetonitrile-0.3%glacial acetic acid(30∶70)and pH value to 5.2~6.2 adjusted with triethylamine,1.0 mL/min of velocity,265 nm of detection wavelength,25℃of column temperature and 10μL of sample volume.【Result】The contents ofβ-dichroine andα-dichroine in 3 batches of D.febrifuga powder from 3 HPLC methods were similar,and better peak type and better separation effect were obtained.【Conclusion】The tested chromatography conditions could be used to detect contents ofβ-dichroine andα-dichroine for the quality control of D.febrifuga powder because of the easy operation,better stability and precision.