克敏芪丹鼻喷剂中5种指标成分的含量测定及制剂喷雾特性考察

Content determination of five index components in Keminqidan nasal spray and investigation of spray characteristics of the preparation

为建立高效液相色谱(HPLC)法同时测定克敏芪丹鼻喷剂中升麻素苷、毛蕊异黄酮葡萄糖苷、阿魏酸、山梨酸钾、5-O-甲基维斯阿米醇苷的含量;并采用激光粒度测定仪考察制剂的粒径分布、喷雾模式和喷雾形态。采用Boston-C18柱(250 mm×4.6 mm,5μm)色谱柱;0.05%磷酸水溶液-乙腈的流动相,梯度洗脱;流量为1.0 mL/min;柱温为25℃;进样量为10μL,检测波长为300 nm。采用Spraytecness喷雾粒度测定仪、牛津激光测定仪考察制剂的喷雾特性。结果表明:5种成分在相应浓度范围内线性关系良好;精密度、稳定性、重复性良好,RSD<1.36%;平均加样回收率在100.68%~105.34%,RSD<1.13%;喷雾形态角度在39°左右;喷雾模式椭圆率在1.16%~1.27%;雾滴粒径主要集中在13~85μm范围内,V%<10μm的雾滴小于5%。该HPLC方法操作简便,专属性强,准确灵敏,重复性好;克敏芪丹鼻喷剂喷雾特性良好。该方法可为克敏芪丹鼻喷剂及其类方制剂的新药开发提供参考。

To develop an HPLC method for the simultaneous determination of cimicifugin,calycosin-7-O-β-Dglucoside,ferulic acid,potassium sorbate and 4'-O-β-D-glucosyl-5-O-methyl-visamminol in Keminqidan nasal spray.The droplet size distribution,spray pattern and plume geometry of the preparation were investigated by laser particle size analyzer.A Boston-C18 column(250 mm×4.6 mm,5μm)was used,and gradient elution was performed with mobile phases composed of 0.05%phosphoric acid aqueous solution-acetonitrile,with the flow rate at 1.0 mL/min,column temperature at 25℃,and injection volume of 10μL.The detection wavelength was set at 300 nm.The Spraytec laser particle size analyzer and Oxford laser particle size analyzer were used to investigate the spray characteristics of the preparation.Good linear relationships were obtained for each compound within their analytical concentration ranges.The RSDs of precision,stability and repeatability tests were less than 1.36%,and the average recoveries of accuracy were 100.68%-105.34%with RSDs<1.13%.The angle of plume geometry is about 39°;the ovality of spray pattern is in the range of 1.16%-1.27%;the droplet size is mainly concentrated in the range of 13-85μm,the droplets with V%<10μm are less than 5%.The HPLC method were developed and fully validated with accepted specificity,accuracy,sensitivity and precision.It indicated that Keminqidan nasal spray had good spray characteristics.The methods can provide reference for the new drug development of Keminqidan nasal spray and its similar formulations.