硝苯地平控释片中释放度测定的不确定度评定  

Determination of uncertainty in release of nifedipine in controlled-release tablets

作　　者：郝海光 许朗晴 刘晶 王威 HAO Hai-guang;XU Lang-qing;LIU Jing;WANG Wei(Beijing Institute for Drug Control,NMPA,Key Laboratory for Research and Evaluation of Generic Drugs,Beijing Key Laboratory of Analysis and Evaluation on Chinese Medicine,Beijing 102206)

机构地区：[1]北京市药品检验研究院<北京市疫苗检验中心>,国家药品监督管理局仿制药研究与评价重点实验室,中药成分分析与生物评价北京市重点实验室,北京102206

出　　处：《中南药学》2025年第1期234-239,共6页Central South Pharmacy

摘　　要：目的评价高效液相色谱法测定硝苯地平控释片中硝苯地平释放度的不确定度。方法采用2020年版《中国药典》中释放度项下规定的方法进行试验,并依据《测量不确定度评定与表示》JJF 1059.1—2012中的相关规定,建立数学模型,对硝苯地平测定过程中不确定度的来源进行分析,计算合成不确定度和扩展不确定度。结果试验中测得硝苯地平4、8、12、16、24 h取样点平均释放度的合成不确定度分别为0.04294、0.04641、0.05310、0.06112、0.06845,扩展不确定度分别为(11.5±0.98)%、(38.7±3.60)%、(66.6±7.08)%、(83.9±10.26)%、(96.9±13.26)%(k=2,置信区间为95%)。结论硝苯地平控释片中硝苯地平释放度的不确定度贡献:4 h取样点主要来源于供试品测量重复性;8、12、16、24 h取样点主要来源于供试品溶液配制,本试验量化了分析方法的不确定度,可为控释片释放度的检查提供更加科学的依据。Objective To determine the uncertainty of the release of nifedipine in nifedipine controlledrelease tablets by HPLC.Methods The test was conducted with the methods specified in the release section in the 2020 Edition of Chinese Pharmacopoeia.According to relevant provisions in JJF 1059.1—2012 of Evaluation and Expression of Measurement Uncertainty,a mathematical model was established to analyze the source of uncertainty in the determination of nifedipine.The synthetic uncertainty and the extended uncertainty were calculated.Results The synthetic uncertainties of nifedipine release at 4,8,12,16 and 24 h were 0.04294,0.04641,0.05310,0.06112,and 0.06845,respectively.The extended uncertainties were(11.5±0.98)%,(38.7±3.60)%,(66.6±7.08)%,(83.9±10.26)%,and(96.9±13.26)%(k=2,confidence interval was 95%).Conclusion The uncertainty of nifedipine release in nifedipine controlled-release tablets:4 h sampling point mainly come from the measurement repeatability of test subjects;while the sampling points at 8,12,16 and 24 h are mainly derived from the preparation of the test product solution.This experiment quantifies the uncertainty of the analysis method,and provides a scientific basis for the inspection of controlled-release tablets.

关 键 词：硝苯地平控释片 不确定度 释放度 高效液相色谱 

分 类 号：R969.1[医药卫生—药理学] R94[医药卫生—药学]