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USP's validation and verification General Chapters: Current and Proposed Prescription / Non-Prescription Stakeholder Forum Meeting #4 for 2010-2015. The primary objective of the Expert Panel is to develop a consistent approach to validation, verification and related topics, from a compendial perspective.
USP's validation and verification General Chapters: Current and Proposed Prescription / Non-Prescription Stakeholder Forum Meeting #4 for 2010-2015. The primary objective of the Expert Panel is to develop a consistent approach to validation, verification and related topics, from a compendial perspective.
USP's validation and verification General Chapters: Current and Proposed Prescription / Non-Prescription Stakeholder Forum Meeting #4 for 2010-2015. The primary objective of the Expert Panel is to develop a consistent approach to validation, verification and related topics, from a compendial perspective.
USPs Validation and Verification General Chapters: Current and Proposed Prescription/Non-Prescription Stakeholder Forum Meeting #4 for 2010-2015 Thursday, J une 27, 2013 <1225> Validation of Compendial Procedures Developed in late 1980s Define Analytical Performance Characteristics No validation acceptance criteria
<1226> Verification of Compendial Procedures Required at the time of implementation Focus in matrix interference and lab variability Lack of specific directions
<1224> Transfer of Analytical Procedures Applicable were verification is not appropriate High level information Statistical approaches are not fully described (<1010>?)
Validation to Measure Variability Validation & Verification Expert Panel <1200> Requirements for Compendial Validation <XXXX> Statistical Tools for Procedure Validation Elemental impurities / Spectroscopy chapters USP initiatives 3 Validation & Verification Expert Panel 4 The primary objective of the Expert Panel is to develop a consistent approach to validation, verification and related topics, from a compendial perspective, which is requirements driven, supported by appropriate statistical tools and will provide guidance which will add value to industry. Allen Templeton Anne K. McCasland-Keller Christopher Burgess David LeBlond David P. Thomas Elisabeth Kovacs Gregory Martin (Chair) Gyongyi S. Gratzl Membership J ane Weitzel J oachim Ermer J oerge Herrmann J ohn P. Hammond Kimber Barnett Lucinda Buhse (FDA) Paul Curry, J r. Phil Nethercote Rosario LoBrutto Deliverables Lifecycle Management of Analytical Procedures: Development, Performance Qualification, and Performance Verification Scheduled for PF 39(5) 2013 Introduces integrated lifecycle concept, Analytical Target Profile
Revised core USP Chapters <1225> Validation to be updated and expanded <1226>, <1224> may no longer be necessary Informational chapter to provide guidance Establishes the types of data that the USP is expecting to see in order to determine the acceptability of a procedure prior to its inclusion in the USP-NF. Include measurable parameters and clear criteria Acceptability of a procedure is evaluated by means of six standardized studies: PrecisionAccuracy, Specificity, Range, Accuracy, Precision, and Detectability. Eliminates LOQ and Linearity <1200> Requirements for Compendial Validation 7 Precision and Accuracy Study When properly combined Precision and Accuracy yield a probability of passing.
Bias-%CV Tradefoff, 98%-102% limits, True Value = 100, Prob'y Passing 0.95 0 0.2 0.4 0.6 0.8 1 1.2 2.00 1.80 1.60 1.40 1.20 1.00 0.80 0.60 0.40 0.20 0.00 Bias % C V This chapter, intended to be a companion to <1225> Validation of Compendial Procedures, provides appropriate statistical methods and examples to aid method validation. Analytical performance characteristics that are discussed from a statistical perspective in the sections that follow are: Accuracy Precision Detection Limit Quantitation Limit Linearity Range
<XXXX> Statistical Tools for Validation 9 Elemental Impurities / Spectroscopy Chapters 10 Equivalent or Better Concept Option Name Demonstrating Comparison to official procedure Number of characteristics considered 1 Acceptable Procedures Acceptable No Many 2 Performance Equivalence Equivalent or Better Yes
Many
3 Results Equivalence Equivalent Yes
One 4 Decision equivalence Equivalent Yes
One Reproduced from Acceptable, equivalent or better approaches for alternatives to official compendial procedures by W. Hauck et al. PF35(3), 2009 Elemental Impurities / Spectroscopy Chapters 11
Include Validation/Verification acceptance criteria in the chapter <233> Elemental impurities - Procedures <852> Atomic Absorption Spectroscopy <854> Mid-Infrared Spectroscopy <857> Ultraviolet-Visible Spectroscopy <853> Fluorescence Spectroscopy
Summary USP is revisiting validation concepts Introducing concepts of QbD and ATP Including validation acceptance criteria where appropriate