敦煌安寐丸质量标准研究

Quality standard of Dunhuang Anmei Wan(敦煌安寐丸)

目的建立敦煌安寐丸的质量标准。方法参照《中华人民共和国药典(四部)》2020年版通则大蜜丸质量要求,采用薄层色谱(TLC)法对敦煌安寐丸中丹参、首乌藤、远志、黄芩、黄连、枳壳等6味中药进行定性鉴别;采用高效液相色谱(HPLC)法对敦煌安寐丸中的指标性成分斯皮诺素、柚皮苷、黄芩苷及丹参酮ⅡA进行含量测定;建立HPLC指纹图谱并进行相似度分析。结果TLC法能够有效鉴别6味中药,薄层斑点清晰且阴性对照无干扰。斯皮诺素、柚皮苷、黄芩苷及丹参酮ⅡA的回归方程分别为Y=1.6895×10^(7)X-5.5407×10^(4)(r=0.9999),Y=9.2072×10^(7)X-2.0461×10^(4)(r=0.9999),Y=1.2132×10^(8)X-1.7738×10^(5)(r=0.9999),Y=1.2987×10^(7)X-9.7682×10^(4)(r=0.9999);线性范围分别为0.006~0.120,0.060~1.200,0.070~1.400,0.002~0.040 mg;平均加样回收率分别为100.29%,101.42%,99.79%,101.59%;RSD分别为1.69%,1.60%,1.53%,1.89%;15批样品中斯皮诺素、柚皮苷、黄芩苷及丹参酮ⅡA含量范围分别为0.1087~0.2981,0.0485~0.1258,0.1925~0.5699,0.1214~0.2998 mg/g。建立了15批敦煌安寐丸的HPLC指纹图谱,相似度均大于0.9,共确定了21个共有峰,并指认其中4个共有峰。结论所建立的质量控制方法专属性强、简便、快捷,可用于该制剂的质量控制。

Objective To establish quality standard of Dunhuang Anmei Wan(敦煌安丸).Methods In accordance with the quality requirements of Pharmacopoeia of the People's Republic of China(Part IV),2020 edition,the six traditional Chinese medicines,including salvia miltiorrhiza,Polygonummultiflorum,Radix Polygalae,Radix Scutellariae,Rhizomacoptidis and Fructus Auranti in Dunhuang Anmei Wan were qualitatively identified by TLC;The content of the index components in Dunhuang Anmei Wan,such as spinocin,naringin,baicalin and tanshinone I A,was determined by HPLC;HPLC fingerprint was established and similarity analysis was performed.Results TLC method can effectively identify the above mentioned 6 traditional Chinese medicines,and the thin layer spots are clear and the negative control has no interference.The regression equations of spinocin,naringin,baicalin and tanshinone II A are Y=1.6895×10^(7)X-5.5407×10^(4)(r=0.9999),Y=9.2072×10^(7)X-2.0461×10^(4)(r=0.9999),Y=1.2132×10^(8)X-1.7738×10^(5)(r=0.9999),Y=1.2987×10^(7)X-9.7682×10^(4)(r=0.9999);The linear range is 0.006~0.120,0.060~1.200,0.070~1.400,0.002~0.040 mg;The average recoveries of sample addition were 100.29%,101.42%,99.79%and 101.59%respectively;RSD is 1.69%,1.60%,1.53%and 1.89%respectively;The content range of spinocin,naringin,baicalin and tanshinone II A in 15 batches of samples is 0.1087~0.2981,0.0485~0.1258,0.1925~0.5699,0.1214~0.2998 mg/g.HPLC fingerprints of 15 batches of Dunhuang Anmei Wan were established,and the similarity was greater than 0.9.A total of 21 common peaks were identified,and 4 common peaks were identified.Conclusion This Simple,feasible,reproducible and specific method can be used for the quality control of Dunhuang Anmei Wan.