Validation of analytical methods based on mass spectrometric detection according to the "2002/657/EC" European decision: guideline and application
Validation of analytical methods based on mass spectrometric detection according to the "2002/657/EC" European decision: guideline and application
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DOI：
10.1016/s0003-2670(02)01379-x
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发表时间：
2003-04-25
影响因子：
6.2
通讯作者：
Andre, F
中科院分区：
文献类型：
--
作者：
Antignac, JP;Le Bizec, B;Andre, F
本文件的目的是提出一个新的2002/657/EC欧洲决定中引入的概念的解释，并提出一个实用的指导方针，致力于验证基于质谱的分析方法。考虑到结果的统计学显著性和实际方面，定性方法和定量方法允许达到令人满意的验证的最小试验数量似乎分别为45和55。采用本方案验证的参数包括专属性、灵敏度、线性、决策限（CCalpha）、重复性、检测能力（CCbeta）和回收率。建议根据筛选方法中的最强（或唯一）离子和确证方法中的“临界离子”（根据所需的鉴别点数量，允许明确鉴别分析物的较弱离子）来估计这些参数。本指南的应用，提出和讨论，通过验证的液相色谱-串联质谱（LC-MS/MS）方法，专门用于测定皮质类固醇曲安奈德（三痤疮）在肉类样品。(C)2002 Elsevier Science B. V.保留所有权利。
The purpose of the present paper is to present an interpretation of the concepts introduced in the new 2002/657/EC European decision and to propose a practical guideline dedicated to the validation of analytical methods based on mass spectrometry. Considering both the statistical significance of the results and practical aspects, the minimal number of assays permitting a satisfying validation to be achieved appeared to be 45 for qualitative methods and 55 for quantitative methods. The parameters validated with this protocol are specificity, sensitivity, linearity, decision limit (CCalpha), repeatability, detection capability (CCbeta) and recovery. It is proposed to estimate these parameters on the basis of the most intense (or unique) ion for screening methods and on the basis of the "critical ion" (less intense ion permitting the unambiguous identification of the analyte according to the required number of identification points) for confirmatory methods. An application of this guideline is presented and discussed, through the validation of a liquid chromatography-tandem mass spectrometric (LC-MS/MS) method dedicated to the determination of the corticosteroid triamcinolone acetonide (Tri Acn) in meat samples. (C) 2002 Elsevier Science B.V. All rights reserved.