判断定量类理化分析方法满足预期用途的标准探讨
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摘要
目的:探讨定量检测类理化方法满足其预期用途的判断标准。方法:采用六西格玛(6σ)理论和过程能力指数(CI)工具,衍生出评价方法的方法能力指数(MCI),并对理化方法在质量属性的不同限度标准下的最大变异进行计算。结果和讨论:(1)可以使用CI的理论对MCI进行全面有效的阐述,包括计算所需前提、方法分级依据、MCI与质量标准以及方法误判(不合格)发生概率的关系。(2)给出用于判断方法是否满足预期用途的最大变异值和方法建立初期最小MCI的选择,并阐述选择依据。(3)论述方法总变异不变的情况下,精密度和偏倚的变化关系图,为读者今后在进行定量理化分析类方法的验证时,快速判断所建方法是否满足其预期用途提供理论依据。
Objective:To explore the acceptance criteria for meeting intended uses on evaluating the physicochemical methods for quantitative detection of product components. Methods:Six Sigma(6σ)theory and tool of Process Capability Index(PCI)were used to derive the method capability index(MCI)which was used to calculate the maximum variability of this kind of methods under different acceptance limits of the testing attributes. Results and discussion:(1)The theory about PCI can be used to explain the MCI comprehensively and effectively,including the Prerequisites for calculation,the grading basis of the method,and the relationship among MCI,specification limits and the probability of method misjudgement(out-of-specification,OOS).(2)The method was given to determine the maximum variability of the method to satisfy the intended use(shown in Table 3 in the content)and the minimum MCI selection at the beginning of the establishment,and the basis of choice was elaborated.(3)The relationship between the precision and(relative)bias of the method was diagrammed when the total variation of the method was invariant. The tables,charts and discussions might provide theoretical basis for analysis and convenience for readers to quickly judge whether the proposed method satisfies intended use when confirming quantitative physicochemical analytical method in the future.
Objective:To explore the acceptance criteria for meeting intended uses on evaluating the physicochemical methods for quantitative detection of product components. Methods:Six Sigma(6σ)theory and tool of Process Capability Index(PCI)were used to derive the method capability index(MCI)which was used to calculate the maximum variability of this kind of methods under different acceptance limits of the testing attributes. Results and discussion:(1)The theory about PCI can be used to explain the MCI comprehensively and effectively,including the Prerequisites for calculation,the grading basis of the method,and the relationship among MCI,specification limits and the probability of method misjudgement(out-of-specification,OOS).(2)The method was given to determine the maximum variability of the method to satisfy the intended use(shown in Table 3 in the content)and the minimum MCI selection at the beginning of the establishment,and the basis of choice was elaborated.(3)The relationship between the precision and(relative)bias of the method was diagrammed when the total variation of the method was invariant. The tables,charts and discussions might provide theoretical basis for analysis and convenience for readers to quickly judge whether the proposed method satisfies intended use when confirming quantitative physicochemical analytical method in the future.
引文
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[2]USP 40-NF 35.[S].2015:1780(<1225>Validation of Compendial Procedures)
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[9]JCGM 100:2008 Evalution of Measurement Data—Guide to the Expression of Uncertainty in Measurement(GUM)[S].2008
[10]USP40-NF35[S].2015:935(<1033>BiologicalAssay Validation)
[11]<1210> Statistical Tools for Procedure Validation[[J/OL].2014,40(5)[2017-07-29].http://www.usppf.com/pf/pub/index.html
[12]DESIMONI E,BRUNETTI B.Uncertainty of measurement and conformity assessment:a review[J].Anal Bioanal Chem, 2011,400:1729
[13]OMCL Network of the Council of Europe.PA/PH/OMCL(14)89R.Evaluation and Reporting of Results Annex 2A[EB/OL].(2015)[2018-06-28].https://www.edqm.eu/en/quality-managementguidelines-86.html
[14]USP 41-NF 36[S].2018:7623(<1210> Statistical Tools for Procedure Validation)
[2]USP 40-NF 35.[S].2015:1780(<1225>Validation of Compendial Procedures)
[3]陶靖轩.关于过程能力指数和不合格品率之间的关系研究[J].中国计量学院学报,2012,23(3):315TAO JX.Relationship of process capability index and nonconforming rate[J].J China Jiliang Univ,2012,23(3):315
[4]谭德讲,赵嘉,曹秀堂.过程能力指数及在药品质量控制中的应用探讨[J].中国药事,2014,28(11):1213TAN DJ,ZHAO J,CAO XT.Process capability indexes and their applications in pharmaceutical quality control[J].Chin Pharm Aff,2014,28(11):1213
[5]张根保,刘英.质量管理与可靠性[M].北京:中国科学技术出版社,2001ZHANG GB,LIU Y.Quality Management and Reliability[M].Beijing:China Science and Technology Press,2001
[6]王斌会,胡志萍.过程能力指数与不合格率的关系模型[J].数理统计与管理,2007,26(1):57WANG BH,HU ZP.The relation model between process capability index and nonconforming rate[J].App1 Stat Manage,2007,26(1):57
[7]<1200> Requirements for Compendial Validation[J/OL].USP Pharmacopeial Forum,2015,41(5)[2017-08-07].http://www.usppf.com/pf/pub/index.html
[8]GB/T 28043-2011/ISO 13528:2005利用实验室间比对进行能力验证的统计方法[S].2011GB/T 28043-2011/ISO 13528:2005 Statistical Methods for Proficiency Testing Using Interlaboratory Comparisons[S].2011
[9]JCGM 100:2008 Evalution of Measurement Data—Guide to the Expression of Uncertainty in Measurement(GUM)[S].2008
[10]USP40-NF35[S].2015:935(<1033>BiologicalAssay Validation)
[11]<1210> Statistical Tools for Procedure Validation[[J/OL].2014,40(5)[2017-07-29].http://www.usppf.com/pf/pub/index.html
[12]DESIMONI E,BRUNETTI B.Uncertainty of measurement and conformity assessment:a review[J].Anal Bioanal Chem, 2011,400:1729
[13]OMCL Network of the Council of Europe.PA/PH/OMCL(14)89R.Evaluation and Reporting of Results Annex 2A[EB/OL].(2015)[2018-06-28].https://www.edqm.eu/en/quality-managementguidelines-86.html
[14]USP 41-NF 36[S].2018:7623(<1210> Statistical Tools for Procedure Validation)