瑶药祛风活络喷雾剂质量标准及微生物限度检查方法研究

Study on Quality Standard and Microbial Limit Test Method of Yao Medicine’s Qufeng Huoluo Spray

目的:建立瑶药祛风活络喷雾剂的质量标准及微生物限度检查方法。方法:对祛风活络喷雾剂中的四方藤、续断进行薄层色谱的定性鉴别;对指标成分岩白菜素和川续断皂苷Ⅵ进行高效液相色谱法的定量测定,采用Diamonsil C18色谱柱(250 mm×4.6 mm,5μm),以乙腈-0.2%磷酸溶液梯度洗脱;同时按现行药典方法对祛风活络喷雾剂微生物限度检查法进行方法适用性研究。结果:两种药材的TLC鉴别专属性强,阴性对照无干扰;岩白菜素、川续断皂苷Ⅵ的线性范围分别为12.77~127.68μg/mL(r=0.9997)和51.90~518.99μg/mL(r=0.9999),方法学验证均符合规定。三批样品中岩白菜素、川续断皂苷Ⅵ平均含量分别为244.9μg/mL、789.0μg/mL;祛风活络喷雾剂微生物计数应采用薄膜过滤法,控制菌采用常规法。结论:建立的祛风活络喷雾剂质量标准和微生物限度检查方法可用于该制剂的质量控制和评价。

Objective:To establish the quality standard and microbial limit test method of yao medicine’s qufeng huoluo spray.Methods:TLC was used for qualitative identification of dipsaci radix and cissus pteroclada hayata.HPLC was used for the content determination of bergenin and asperosaponinⅥ.Using Diamonsil C18 column(250 mm×4.6 mm,5μm),gradient elution of acetonitrile-0.2%phosphoric acid solution was used.At the same time,according to the current pharmacopoeia method,the method applicability of qufeng huoluo spray microbial limit test method was studied.Results:TLC identification of the two medicinal materials had strong specificity,and the negative control had no interference.The linear range of bergenin and asperosaponinⅥwere 12.77~127.68μg/mL(r=0.9997)and 51.90~518.99μg/mL(r=0.9999).Methodological validation is in compliance with the regulations.In the three batches of samples,the average contents of bergenin and asperosaponinⅥwere 244.9μg/mL and 789.0μg/mL,respectively.Membrane filtration method should be used for microbial count of qufeng huoluo spray,and conventional method should be used for bacterial control.Conclusion:The established quality standard and microbial limit test method can be used for quality control and evaluation of qufeng huoluo spray.