摘要
目的:建立麝香关节止痛膏中盐酸苯海拉明的含量测定方法,并对3家企业生产的87批次麝香关节止痛膏的质量进行评价。方法:采用高效液相色谱(HPLC)法进行测定:使用Hypersil-Gold C_(18)(250 mm×4.6 mm, 5μm)色谱柱进行分离,以流动相为甲醇-1%硫酸铵(47∶53,V/V);流速;1.0 mL·min^(-1);柱温为35℃;检测波长为210 nm。以87批次样品的含量数据为指标,绘制直方图、箱式图和三维散点图,进行质量评价。结果:方法学考察结果均符合《中国药典》2020年版(四部)通则要求。盐酸苯海拉明进样量的线性范围为0.200 4~5.010μg(r=1.000 0);平均回收率为94%, RSD=1.9%。3家企业生产的87批次样品中盐酸苯海拉明的含量在1.22~8.74 mg·100 cm^(-2)。结论:本研究所建麝香关节止痛膏中盐酸苯海拉明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参数,加强质量控制。
Objective:To establish the method for the determination of diphenhydramine hydrochloride in Shexiang guanjie zhitong plaster,and to evaluate the quality of 87 batches of Shexiang guanjie zhitong plaster produced by 3 manufactures.Methods:HPLC method was established.The determination was performed on Hypersil Gold C_(18)(250 mm×4.6 mm,5μm)column with the mobile phase consisted of methanol-1%ammonium sulfate(47∶53,V/V)at the flow rate of 1.0 mL·min^(-1).The column temperature was set at 35℃,the detection wavelength was 210 nm.With the content data of 87 batches of samples as the index,histogram,box chart and three-dimensionalscatterplot are drawn,and adopt those to evaluate the quality.Results:The results of methodological investigation were in line with the requirements of the general principles stated in 2020 edition of Chinese Pharmacopoeia(partⅣ).The linear range of diphenhydramine hydrochloride injection volume is 0.2004-5.010μg(r=1.0000),the average recovery was 94%,RSD=1.9%.Thecontent of diphenhydramine hydrochloride in 87 batches of samples from 3 manufacturers were 1.22-8.74 mg·100 cm^(-2).Conclusion:The established method for the determination of diphenhydramine hydrochloride in Shexiang guanjie zhitong plaster is accurate and precise,and can be used for its quality control.Some manufacturers should pay attention to optimizing production process parameters and strengthen quality control.
作者
朱殿龙
季雪
胡景莲
ZHU Dian-long;JI Xue;HU Jing-lian(Dalian Inspection and Certification Technology Service Center,Liaoning Dalian 116021,China)
出处
《中国药物评价》
2023年第2期137-141,共5页
Chinese Journal of Drug Evaluation
基金
2022年国家药品评价性抽检中央补助地方经费项目(No.11)。
关键词
麝香关节止痛膏
盐酸苯海拉明
含量测定
质量评价
Shexiang guanjie zhitong plaster Diphenhydramine hydrochloride
Content determination
Quality evaluation
