摘要
目的:探讨方法确认/转移成功的判定标准。方法:结合近年来方法学研究的新进展,特别是统计学在该领域的应用进展,分析目前方法确认/转移法规或文献中的表述不清晰问题,探讨引入统计学中的预测区间、容忍区间和方法能力指数作为确认/转移成功的判定标准。结果:方法确认/转移方案遵循方法验证的操作步骤,实验设计仅需实验者按方法验证要求进行独立重复操作;若该操作过程所获得的报告值在方法验证结果的预测区间内,则可以判定方法确认/转移成功;当该报告值超出方法验证结果的容忍区间,则可判定方法确认/转移不成功;当该报告值在容忍区间和预测区间范围之间时,应关注实验过程并尝试进一步改进方法。此外,也可通过方法能力指数作为判定确认和转移的依据。结论:当使用新的确认/转移实验设计方案时,采用与方法验证结果的预测区间和容忍区间进行比较的方式以及使用方法能力指数进行评估的方式;两者作为判定方法确认和转移是否成功的标准具有明显优势。同时可有效降低方法确认/转移过程所导致的误判风险。
Objective:To explore the criteria for successful method verification and transfer.Methods:Combining with advancements in methodological research in recent years,especially the advancements in the application of statistics in this field,the unclear issues were analyzed in the current guidelines or literature about methods verification/transfer,and the criteria were discussed for successful method verification and transfer by introducing predictive interval,tolerance interval and method capability index.Results:Analysis method verification/transfer protocol followed the protocol of method validation,and the experimental design only required the experimenter to repeat the operation independently according to the requirements of method validation.If the reported value obtained was within the prediction interval of the method validation results,the method verification/transfer could be judged successful.If the report value exceeded the tolerance interval of method validation results,the method verification/transfer could be judged unsuccessful.If the report value was between the tolerance interval and the prediction interval,attention should be paid to the experimental process and further improvement should be attempted.In addition,the method capability index could also be used for determination of verification/transfer.Conclusion:When using the new experiment design mentioned here for method verification/transfer,there are obvious advantages to use the following approaches as criteria to judge whether the method verification/transfer are successful.One is comparing the reported value obtained from method verification/transfer with the prediction interval and tolerance interval from method validation and the other is assessing by calculating the method capability index.At the same time,it can effectively reduce the risk of misjudgment caused by the method verification/transfer process.
作者
李娜
耿颖
谭德讲
杨化新
朱容蝶
马莉
许卉
张庆生
LI Na;GENG Ying;TAN De-jiang;YANG Hua-xin;ZHU Rong-die;MA Li;XU Hui;ZHANG Qing-sheng(NMPA Key Lab for Quality Research and Evaluation of Chemical Drug,National Institutes for Food and Drug Control,Beijing 102629,China;Yantai University,Yantai 264003,China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2021年第4期675-680,共6页
Chinese Journal of Pharmaceutical Analysis
基金
2019年国家药典委员会标准制修订课题(2019Y17)。
关键词
方法转移
方法确认
方法验证
生命周期
等效区间
预测区间
容忍区间
方法能力指数
接收标准
method transfer
method verification
method validation
lifecycle
equivalent interval
prediction interval
tolerance interval
method capability index(MCI)
acceptance criteria
