麝香拔湿膏质量标准研究

Quality Standard of Shexiang Bashi Ointment

目的建立麝香拔湿膏的质量标准。方法采用TLC法鉴别颠茄流浸膏中的硫酸天仙子胺;采用HPLC法测定盐酸苯海拉明的含量;色谱柱为Shiseido C18柱(4.6 mm×250 mm,5μm),以甲醇-1%硫酸铵溶液(41∶59)为流动相,检测波长为210 nm,流速为1.0 mL·min^-1,进样体积为10μL,柱温30℃。结果薄层色谱鉴别斑点清晰,阴性无干扰;盐酸苯海拉明在0.408~12.240μg呈现良好的线性关系(r=1.000),平均回收率为98.8%,RSD为1.5%(n=6)。结论该方法具可行性,方法准确可靠,操作简单,重复性好,可用于成品的质量控制。

OBJECTIVE To establish the quality standard of Shexiang Bashi ointment.METHODS Hyoscyamine sulfate in Atropa belladonna liquid extract were identified by TLC qualitatively.The content of diphenhydramine hydrochloride was determined by HPLC.The chromatographic separation was performed on a Shiseido C18 column(250 mm×4.6 mm,5μm).The mobile phase consisted of methanol-1%ammonium sulfate solution(41∶59)with gradient elution at a flow rate of 1.0 mL·min^-1,and the injection volume was 10μL.The detection wavelength was 210 nm.The Column temperature was at 30℃.RESULTS The spots in TLC were clear without any interferences.The linear range of diphenhydramine hydrochloride was 0.408 to 12.240μg with a good correlation(r=1.00).The average recovery was 98.8%and the RSD was 1.5%(n=6).CONCLUSION The method is reliable and easy to operate,which can be used for the quality control of the products.