麝香壮骨膏中盐酸麻黄碱和盐酸伪麻黄碱的含量测定及质量评价

Content determination of ephedrine hydrochloride and pseudoephedrine hydrochloride in Shexiang zhuanggu plaster and its quality evaluation

目的建立麝香壮骨膏中盐酸麻黄碱和盐酸伪麻黄碱的含量测定方法,并对41家企业生产的222批次麝香壮骨膏的质量进行评价。方法采用高效液相色谱(HPLC)法进行测定:使用Shimadzu Shim-pack GIS-C18色谱柱进行分离,以乙腈-0.1%磷酸溶液(3∶97,V/V)为流动相,流速为0.9 mL/min,柱温为30℃,检测波长为210 nm,进样量为10μL。以222批次样品的含量数据为指标,采用Hiplot生物医学数据可视化和分析平台绘制聚类热图。结果方法学考察结果均符合2020年版《中国药典》(四部)通则要求。41家企业生产的222批次样品中盐酸麻黄碱和盐酸伪麻黄碱的总含量在0.646~6.325μg/cm^(2)之间。聚类热图分析结果显示,41家企业生产的样品可被聚为3类。不同企业生产的样品中成分含量差异较大,且部分企业生产的不同批次样品也存在含量差异较大的现象。若拟定本品限度为每1 cm2含盐酸麻黄碱和盐酸伪麻黄碱的总量不得低于1.00μg,则222批次样品中有23批次不合格。结论本研究所建麝香壮骨膏中盐酸麻黄碱、盐酸伪麻黄碱含量测定的方法准确、精密,可用于其质量控制。部分企业应优化生产工艺,加强质量控制。

OBJECTIVE To establish the method for the content determination of ephedrine hydrochloride and pseudoephedrine hydrochloride in Shexiang zhuanggu plaster,and to evaluate the quality of 222 batches of Shexiang zhuanggu plaster from 41 manufacturers.METHODS HPLC method was established.The determination was performed on Shimadzu Shim-pack GIS-C18 column with mobile phase consisted of acetonitrile-0.1%phosphoric acid(3∶97,V/V)at the flow rate of 0.9 mL/min.The column temperature was set at 30℃,the detection wavelength was 210 nm,the sample size was 10μL.Taking the content data of 222 batches of samples as index,the cluster heatmap was drawn by Hiplot biomedical data visualization and analysis platform.RESULTS The results of the methodological investigation were in line with the requirements of the general principles stated in 2020 edition of Chinese Pharmacopoeia(partⅣ).The total contents of ephedrine hydrochloride and pseudoephedrine hydrochloride in 222 batches of samples from 41 manufacturers were 0.646-6.325μg/cm^(2).Results of cluster heatmap analysis showed that these samples of 41 manufacturers could be divided into 3 categories.The contents of components in samples from different manufacturers varied greatly,and the contents of components in different batches of samples from the same manufacturers also varied greatly.If the proposed limit of this product was that the total amount of ephedrine hydrochloride and pseudoephedrine hydrochloride per 1 cm2 would not be less than 1.00μg,23 of the 222 batches of samples were unqualified.CONCLUSIONS The established method for the content determination of ephedrine hydrochloride and pseudoephedrine hydrochloride in Shexiang zhuanggu plaster is accurate and precise,and can be used for the quality control.Some manufacturers should pay attention to optimizing production process and strengthening quality control.