四黄栓制备工艺和质量标准研究

Preparation Process and Quality Standard of Sihuang Suppository

目的优选四黄栓的最佳提取工艺和成型工艺,并建立其质量标准。方法考察提取时间、提取次数、加溶剂量3个因素,以出膏率和盐酸小檗碱含量为综合评价指标设计正交试验,优选最佳提取工艺。选择合适的基质,制备四黄栓。采用薄层色谱法对四黄栓中大黄、黄连、黄柏、黄芩进行定性鉴别,采用高效液相色谱法测定栓剂中盐酸小檗碱含量。结果最佳提取条件为加8倍处方药材量溶剂,回流提取3次,每次1 h;出膏率为23.38%,盐酸小檗碱含量为89.49 mg/g。以36型和38型混合脂肪酸甘油酯(1∶1,m/m)为基质,制备四黄栓。薄层色谱中,黄连、黄柏、黄芩和大黄的特征斑点显色清晰,阴性对照无干扰。盐酸小檗碱质量浓度在10.049~100.485μg/mL范围内与峰面积线性关系良好(R2=1.0000,n=6);平均加样回收率为101.72%,RSD为0.98%(n=6);精密度、重复性、稳定性试验的RSD均小于0.50%(n=6)。结论优选出的提取工艺简单合理、稳定可行。所建立的质量标准操作简单、重复性好,可用于四黄栓的质量控制。

Objective To optimize the extraction and molding process of Sihuang Suppository and establish its quality standard.Methods The orthogonal test was designed with the extraction time,extraction times and solvent amount as investigation indexes and the extract yield and berberine hydrochloride content as the comprehensive evaluation indexes to optimize the extraction process.The appropriate matrix was selected to prepare Sihuang Suppository.Rhei Radix et Rhizoma,Coptidis Rhizoma,Phellodendri Chinensis Cortex and Scutellariae Radix in Sihuang Suppository were identified by thin-layer chromatography(TLC)method,and the content of berberine hydrochloride in the Sihuang Suppository was determined by high-performance liquid chromatography(HPLC)method.Results The optimal extraction process was to add 8 times the amount of water,reflux extraction for 3 times and 1 h each time.The extract yield was 23.38%and the content of berberine hydrochloride was 89.49 mg/g.Sihuang Suppository was prepared with type 36 and type 38 mixed fatty acid glycerides(1∶1,m/m)as the matrix.In the TLC chromatograms,the characteristic spots of Coptidis Rhizoma,Phellodendri Chinensis Cortex,Scutellariae Radix and Rhei Radix et Rhizoma were clear,and the negative control had no interference.The mass concentration of berberine hydrochloride had a good linear relationship with peak area in the range of 10.049-100.485μg/mL(R^(2)=1.0000,n=6),the average recovery was 101.72%with an RSD of 0.98%(n=6),the RSDs of precision,repeatability and stability tests were less than 0.50%(n=6).Conclusion The optimized extraction process is simple,reasonable,stable and feasible,and the quality standard established is simple and reproducible,which can be used for the quality control of Sihuang Suppository.