山香圆有效成分的制备及HPLC测定质量标准建立

Preparation of active ingredients in Shanxiangyuan and establishment of quality standards for HPLC determination

制备山香圆中有效成分女贞苷,并通过高效液相色谱(HPLC)建立了质量标准。以70%乙醇为溶剂加压提取山香圆中有效成分女贞苷,并以女贞苷得率为指标优化提取条件。结果显示,山香圆中有效成分女贞苷的较佳提取工艺:料液比为1∶30(g∶mL),提取温度为90℃,萃取时间为2.0 h;较佳纯化工艺:提取溶剂流速为1.0 mL/min,洗脱溶剂流速为2.0 BV/h,洗脱溶剂体积为2.0 BV/h。采用HPLC,C18色谱柱(250 mm×4.6 mm,5μm),流动相A相为甲醇,B相为0.5%磷酸,流速为1.0 mL/min,检测波长为360 nm,柱温为室温;结果表明,女贞苷均在0.309~39.126μg/mL范围内线性关系良好(r2=0.9999),重复性RSD<4.0%(n=6),稳定性(24 h内)RSD<2.0%(n=6),平均加样回收率为95%~105%。山香圆有效成分制备工艺简单,HPLC测定质量标准方法简便、准确,重复性好,可为将来山香圆有效成分含量质量控制提供实验依据。

The active ingredient Ligustrum lucidum in Shanxiangyuan was prepared and the quality standard was established based on high performance liquid chromatography(HPLC).The extraction conditions were optimized according to the yield of Ligustrum lucidum as the index,in which 70%ethanol was used as the solvent under pressure.The results showed that,the optimized extraction process was as follows:The solid-liquid ratio was 1∶30(g∶mL);the extraction temperature was 90℃;the extraction time was 2.0 h.The optimized purification process was as follows:The flow rate of extraction solvent was 1.0 mL/min;the flow rate of elution solvent was 2.0 BV/h;the elution solvent volume was 2.0 BV/h.In HPLC determination,C18 column(250 mm×4.6 mm,5μm)was used,mobile phase A was methanol,phase B was 0.5%phosphoric acid,the flow rate was 1.0 mL/min,the detection wavelength was 360 nm,and the column temperature was room temperature.The results showed that,the linearity was good in the range of 0.309-39.126μg/mL(r2=0.9999),the repeatability was RSD<4.0%(n=6),the stability(within 24 h)was RSD<2.0%(n=6),and the average spiked recoveries were 95%-105%.The preparation process of the active ingredients of Shan Xiang Yuan was simple,and the quality standard based on determination by HPLC method was simple,accurate and reproducible,which could provide an experimental basis for the quality control of the content of active ingredients in Shanxiangyuan in future.