OOS-附件2A.doc
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1、201410 PA/PH/OMCL (14) 89 结果的评估和报告-附录2A 定量检测项目的复验程序举例OMCL Network of the Council of EuropeQUALITY ASSURANCE DOCUMENTPA/PH/OMCL (14) 89Evaluation and Reporting of Results结果的评估和报告Annex 2AFull document title and referenceEvaluation and reporting of Results-Annex 2A Examples of Re-test Programmes for Qu
2、antitative Tests PA/PH/OMCL (14) 89全名和索引结果的评估和报告-附录2A定量检测项目的复验程序举例PA/PH/OMCL(14)89Document typeGuideline文件类型指南Legislative basis/法规依据无Date of first adoptAugust 2014首次采纳日期2014年8月Date of original entry into forceOctober 2014首次实施日期2014年10月Date of entry into force of revised document/修订版生效日期无Previous tit
3、les/other references/last valid version/之前题目/其它索引号/上一有效版本无Custodian OrganisationThe present document was elaborated by the OMCL Network/EDQM of the Council of Europe责任机构现行文件由欧盟委员会EDQM/OMCL网络编制Concerned NetworkGEON相关网络GEONANNEX II AOF THE OMCL NETWORK GUIDELINE“EVALUATION AND REPORTING OF RESULTS”EXA
4、MPLES OF RE-TEST PROGRAMMES FOR QUANTITATIVE TESTSTABLE OF CONTENTINTRODUCTION概述Approach 1: Active pharmaceutical ingredient, 2 initial determinations方法1:原料药,2次初始检测Approach 2: Active pharmaceutical ingredient, 3 initial determinations方法2:原料药,3次原始检测Approach 3: Impurity tests (e.g. Related substances
5、by HPLC)方法3:杂质检测(例如HPLC检测有关物质)Approach 4: Finished products方法4:制剂检测Approach 5: Products with insufficient validation data方法5:验证数据不充分的产品Approach 6: Re-test programme based on statistical assay layouts (Ph. Eur. 5.3)方法6:根据统计学含量布局制订的复验计划(欧洲药典5.3)Approach 7: Re-test programme based on known intermediate
6、 precision方法7:根据已知中间精密度的复验程序Approach 8: Approach for cases of unexplained lack of repeatability方法8:缺乏重复性又不能解释情况下所用的方法INTRODUCTION概述This document is an Annex to the core document “Evaluation and reporting of results”,PA/PH/OMCL (13) 113(in its current version), and it should be used in combination wi
7、th it when planning, performing and documenting the evaluation process and reporting of results of quantitative tests with the expected Gaussian distribution.本文件是“结果的评估与报告”核心文件PA/PH/OMCL (13) 113(现行版本)的附录。在计划、实施和记录符合正态分布的定量测试结果的评估过程和报告结果时要与核心文件一起使用。The core document contains the Introduction, Scope
8、and General requirements for the evaluation of results (in routine cases or otherwise) and the reporting of results.核心文件包括结果评估(在常规情形还是其它情形)和报告的概述、范围和通用要求。The proposed approaches are only relevant if the decision is based on observed repeatability1. In all cases, the laboratory should make a decision
9、 based on documented and sound scientific judgement. This Annex should not be taken as a list of compulsory requirements. It is left to the professional judgement and background experience of each OMCL to decide on the most relevant procedures to be undertaken in order to give evidence that the eval
10、uation and reporting of results is well managed. Although two or three initial determinations are described in most examples of this Annex, each OMCL is responsible for deciding what is the minimum number of replicates that should be taken into account for a certain test.如果基于观察到的重复性来做出决定,则提议的方式仅是相关而
11、已。在所有情形下,化验室应根据书面的科学合理判断来做出决定。本附录不应作为是强制要求的清单,每个OMCL应该根据专业判断和背景知识来决定采用最相关的程序,以提供证据证明对结果的评估和报告有良好的管理。虽然在本附录的大多数例子中描述了2次或3次初始检测,但每个OMCL应决定在某个具体的测试中需考虑的平行检测的最少次数。This Annex presents several examples of the evaluation of results for quantitative testing of medicinal products, which could be set up in co
12、mbination with the general requirements given in the core document. The examples are not intended to be all-inclusive, and other valid approaches may be adopted for evaluation of the acceptability of test results.本附录给出了几个药品定量检测中结果评估的例子,它们可以与核心文件中的通用要求结合来看。这些例子无意列举出所有可能,在检测结果的可接受度评估中也可以采用其它有效方法。This
13、document is based on publications inPharmeuropaVol. 9, No. 1, 148-156 (1997) andPharmeuropaVol. 11, No. 4, 571-577 (1999). The proposals for approach 1, 2 and 4 were tested against datasets obtained from proficiency tests and have been shown to be satisfactory for making a decision.本文件是依据欧洲药典在线卷9第1篇
14、页148-156(1997)和欧洲药典在线卷11第4篇页571-577(1999)而制订的。方法1、2和4所用的方案经过了专业测试所获得的数据系列的测试,显示很令人满意,可以用以做出决策。The following table gives an overview about the described possible approaches and the situations where they may be applied, see below:下表给出了所述可能方法的概览,以及这些方法可能适用的情形。Approach方法Title标题Situation情形1Active pharmac
15、eutical ingredient, 2 initial determinationsThis approach is applicable for APIs only原料药,2次初始检测本方法仅适用于原料药2Active pharmaceutical ingredient, 3 initial determinationsThis approach is applicable for APIs only原料药,3次初始检测本方法仅适用于原料药3Impurity tests (e.g.: Related substances by HPLC)This approach is intended
16、 for trace level tests and may be used for quantitative impurity tests, where an analytical/instrumental response is obtained (peak area, for example)杂质检测(例如,HPLC检测有关物质)本方法用于痕量检测,可以用于利用分析方法/仪器响应(例如峰面积)来进行定量杂质检测的情况4Finished productsThis approach is intended for finished products with fully validated
17、methods regarding repeatability and intermediate precision described in the MA file. It is not intended for analyte concentrations at trace level.制剂本方法适用于经过完整验证的制剂检测方法,且方法的重复性和中间精密度在MA文件中有载。不适用于痕量水平的分析物浓度检测。5Products with insufficient validation dataThis approach is to be regarded as a tool to estab
18、lish an acceptance criterion for precision of the replicates of a certain test, when the laboratory has no other mean to evaluate the dispersion of the results, as the available validation data are scarce or there are no validation data at all. It is not intended for analyte concentrations at trace
19、level.验证数据不充分的产品本方法是作为一种工具,当化验室没有其它方法来评估结果的分散度,且已有验证数据很少,或完全没有验证数据时,用来建立一个方法重复检测时的精密度的可接受标准。6Retest programme based on statistical assay layouts (Ph. Eur. 5.3)Results from bioassays in statistical layout according to Ph. Eur. 5.3. For combination of assays it is desirable that the individual results
20、 are obtained in identical or similar assay layouts.基于统计学含量布局的复验计划(欧洲药典5.3)根据药典5.3统计学生效含量所得的结果。对于含量结果的合并,最好单个结果具有相同或类似的含量布局7Retest programme based on known intermediate precisionThis approach is intended for assays with well-known in-house intermediate precision, e.g. in OCABR routine analysis根据已知中间
21、精密度的复验计划本方法适用于已知内部中间精密度的含量,例如,在OCABR常规分析中8Approach for cases of unexplained lack of repeatabilityFor products where sample recovery problems are encountered or there is no plausible reason for lack of precision缺乏重复性且不能解释的情形所用方法用于样品有回收问题的药品,或缺乏精密度没有貌似有理的原因Approach 1: Active pharmaceutical ingredient,
22、 2 initial determinations方法1:原料药,2次初始检测Perform two determinations. If theRSD22is smaller than theRSDmaxpermitted for two determinations (seeTable 1), and the mean falls within the content limits, the sample passes. If either of these two conditions is not met, one further determination is performed.
23、 If theRSD3 of the three values meets the criterion and the mean of the three results falls within the content limits, the sample passes. This can be repeated up to a maximum of six determinations. The sample can only be rejected if the mean is outside the content limits and the criterion for the RS
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