参威骨痹颗粒的提取工艺研究

Study on the extraction technology of Shenweigubi Granules

目的研究及优化参威骨痹颗粒的提取工艺。方法挥发油提取选择共水蒸馏法,以挥发油得率为指标,进行单因素实验,对浸泡时间、加水量和提取时间分别进行考察;以芍药苷转移率和干膏得率的综合评分为指标,采用正交实验考察了加水倍量、提取时间和提取次数3个因素对水提工艺的影响。结果最佳工艺为浸泡2h,加10倍量水,提取6h,挥发油提取率为0.258%;最佳水提条件为:煎煮2次,每次加8倍量水,煎煮2h;芍药苷含量测定色谱条件:色谱柱:十八烷基硅烷键合硅胶作为填充剂(250mm×4.6mm,5μm);以乙腈-1mL·L^(-1)磷酸溶液(14∶86)为流动相;检测波长为230nm。理论板数按照芍药苷峰计算不低于2 000;流速:1mL·min^(-1);进样量:10μL,柱温:25℃;芍药苷在0.262~6.550μg范围内,进样量与峰面积呈良好线性关系,线性方程为y=10.666x+0.381 5(r=0.999 9),平均加样回收率为100.14%,RSD值为1.1%。结论确定的提取工艺路线合理可行,优选得到的提取工艺条件稳定,具有重复性和可操作性,可作为参威骨痹颗粒制备的提取工艺。

Objective To study and optimize the extraction conditions of Shenweigubi Granules.Methods Common water distillation method was used to extract volatile oil,and using the yield of volatile oil as evaluation index.The soaking time,water volume and extraction time were studied by single factor respectively.By taking the comprehensive transfer rate of paeoniflorin and dry cream yield as the index,the effects of water consumption,extraction time and extraction times on the water extraction process were investigated by orthogonal test.Results The optimal extraction conditions were as follows：soaking for 2 h,adding 10 folds of water,extraction for 6 h,the extraction rate of volatile oil was 0.258%;the optimal water extraction process was obtained as follows：adding 8 folds of water,decocting for 2 times,each time for 2 h.The chromatographic conditions of the determination of paeoniflorin were as follows：the octadecyl silane bonded silica chromatographic column（250 mm×4.6 mm,5μm）was used with acetonitrile-1 mL·L^-1phosphoric acid solution（14∶86）as the mobile phase.The detection wavelength was 230 nm,and the number of theoretical plates should not be less than 2 000.The flow rate was 1 mL·min^-1,the injection volume was 10μL,and the column temperature was 25 ℃.Paeoniflorin showed a good linear relationship between 0.262 and 6.550μg with regression equation y=10.666 x＋0.381 5（r=0.999 9）.The average recoveries of paeoniflorin were 100.14% and the RSD was 1.1%.Conclusion The extraction route is reasonable and feasible.The extraction process is stable,reproducible and operable.Therefore,these traits can be used as extracting process of Shenweigubi Granules in preparation.