通痹止痛合剂工艺优化和质量标准的研究  

Research on Optimization and Quality Standard of Tongbi Zhitong Mixture

作　　者：文建文 孙雪林 徐奎 梁富慧 WEN Jianwen;SUN Xuelin;XU Kui;LIANG Fuhui(The First Affiliated Hospital of Guangxi University of Traditional Chinese Medicine,Nanning 530023,China;Guangxi Traditional Chinese Medicine School,Nanning 530000,China;Traditional Chinese Medicine Hospital of Fang Chenggang,Fang Chenggang 538021,China)

机构地区：[1]广西中医药大学第一附属医院,广西南宁530023 [2]广西中医学校,广西南宁530000 [3]防城港市中医医院,广西防城港538021

出　　处：《中国民族民间医药》2025年第2期65-69,共5页Chinese Journal of Ethnomedicine and Ethnopharmacy

基　　金：广西壮族自治区卫生厅中医药科技专项(编号:GZYZ1213)。

摘　　要：目的:优化通痹止痛工艺,并建立通痹止痛合剂的质量标准。方法:应用正交试验(醇浓度、醇用量、浸泡时间及渗漉速度)优化工艺,采用薄层色谱法(TCL)对独活和当归进行定性研究;采用高效液相色谱法(HPLC)测定通痹止痛合剂中二氢欧山芹醇当归酸酯含量。色谱柱:C_(18)(4.6 mm×250 mm,5μm);流动相:乙腈为A相,0.2%磷酸水为B相,采用梯度洗脱(0~30 min,50%~70%A),检测波长为330 nm,柱温为30℃,流速设定为1.0 mL/min,进样量为10μL。结果:采用60%乙醇,浸渍48 h,渗漉6 mL/min,乙醇用量为12倍为粗粉提取优选工艺;薄层色谱法(TCL)可鉴别出独活和当归对应的特征斑点,且阴性无干扰;采用HPLC法测定二氢欧山芹醇当归酸酯含量,二氢欧山芹醇当归酸酯在0.528~1.408μg范围内,进样量与峰面积之间有良好的线性关系(r=0.9996),平均回收率为98.92%,RSD=1.57%(n=6)。结论:制定的通痹止痛合剂的质量标准操作简单,准确灵敏,专属性强,能评价通痹止痛合剂中二氢欧山芹醇当归酸酯的含量。Objective Optimize the processing of Tongbi Zhitong Mixture and formulate quality standard of Tongbi Zhitong Mixture.Method Orthogonal test was used to optimize the extraction process.Using thin layer chromatography(TCL) detecting Duhuo(angelica pubescens) and Danggui(angelica sinensis);The content of columbianadin was determined by high performance liquid chromatography(HPLC).column:C_(18)(4.6 mm×250 mm,5 μm),mobile phase:acetonitrile as phase A,0.2%phosphate as phase B,gradient elution(0-30 min,50%-70% A),detection wavelength set to at 330 nm,the column temperature was 30 ℃,the flow rate was set at 1.0 mL/min,and the injection volume was 10 μL.Results The optimal process conditions was as follows:60%ethanol,soaking for 48 hours,6mL/min penetrated,and the amount of ethanol is 12 times;The specific spots of angelica pubescensand and angelica sinensis were presented clearly by TLC without interference from the negative control;HPLC was adopted for the content determination of columbianadin in the preparation.A good linear correlation was obtained within the range of 0.528-1.408 μg(r=0.9996) for Columbianadin,The average recovery was 98.92% with RSD of 1.57% for Columbianadin(n=6).Conclusion The established method is simple,accurate,sensitive and specific,The established quality standard can be used to evaluate the content of Columbianadin in Tongbi Zhitong Mixture.

关 键 词：通痹止痛合剂 制备工艺 质量标准 二氢欧山芹醇当归酸酯 薄层色谱法 高效液相色谱法 

分 类 号：R286[医药卫生—中药学]