景参丸中红景天苷和丹酚酸B含量测定方法的建立及干燥工艺考察

Content determination of salidroside and salvianolic acid B in Jingshen Pills and investigation of drying process

目的:建立高效液相色谱(HPLC)法同时测定景参丸中红景天苷和丹酚酸B的含量,并优化景参丸的干燥工艺。方法:(1)采用Agilent ZORBAX Eclipse Plus C;色谱柱(250 mm×4.6 mm,5μm),以甲醇-0.1%磷酸水溶液为流动相进行梯度洗脱,流速1 ml/min,检测波长278 nm,柱温35℃,进样体积10μl。并进行方法学考察。(2)以丸剂外观、水分、溶散时限以及红景天苷和丹酚酸B的含量为评价指标,考察室温(25℃)除湿干燥、60℃热风干燥、70℃热风干燥、80℃热风干燥、90℃热风干燥及100℃热风干燥对景参丸质量的影响,采用综合评分法优选最佳干燥工艺。结果:(1)所建立的含量测定方法,线性关系、精密度、重复性、稳定性、加样回收率等均符合要求。(2)优选的景参丸最佳干燥工艺为70℃热风烘干干燥,铺层厚度1.5 cm,干燥时间2 h。结论:所建立的含量测定方法简便,重复性和稳定性好,精密度高,可为景参丸的质量控制提供参考。优选出的景参丸干燥工艺稳定、可行,可最大限度保留有效成分,且干燥效率高。

Objective:To establish a high performance liquid chromatography(HPLC)method for simultaneous determination of salidroside and salvianolic acid B in Jingshen Pills,and optimize the drying process of Jingshen Pills.Methods:(1)The determination was performed on an Agilent ZORBAX Eclipse Plus C;column(250 mm×4.6 mm,5 μm)at flow rate of 1 ml/min with methanol-0.1%phosphoric acid containing water(gradient elution). The determination wave length was 278 nm,the column temperature was 35 ℃,and the injection volume was 10 μl. The methodology was investigated.(2)Taking the appearance,water content,time-limit of dissolution and contents of salidroside and salvianolic acid B in Jingshen Pills as evaluation indexes,the effects of different drying processes on the quality of Jingshen Pills were investigated,including dehumidification drying at room temperature(25 ℃),hot air drying at 60 ℃,hot air drying at 70 ℃,hot air drying at 80 ℃,hot air drying at 90 ℃ and hot air drying at 100 ℃. The best drying process was optimized by comprehensive scoring method.Results:(1)For the established HPLC method,the linear relationship,precision,repeatability,stability and recovery all met the requirements.(2)The optimum drying process of Jingshen Pills was hot air drying at 70 ℃,the layer thickness was 1.5 cm and the drying time was 2 hours.Conclusion:The established content determination method is simple and convenient,with good repeatability and stability and high precision,which can provide reference for the quality control of Jingshen Pills. The optimized drying process of Jingshen Pills is stable and feasible,which can retain the effective components to the greatest extent and show high drying efficiency.