Qualification method

Method qualification is based on ICH method validation guidelines. Method type (purity or identity) will dictate the level of qualification testing necessary. Several strategies for method qualification and validation exist and are based on needs, resources available, and the project timeframe. One approach is to perform minimal development and qualification, which may be necessary for projects with shorter timelines, but it may place more burden and risk on future validation activities for robustness testing, and can result in failure. As discussed in Chapter 4, an alternate approach would invest more time and resources into method development, followed by extensive qualification and robusmess testing to determine if further development is... 

TABLE I Interpretation of ICH Guidelines for Method Qualification/Validation... 

As an identity (ID) test, per ICH guidelines, only selectivity is required in method qualification and validation. Repeatability and intermediate precision are often included to ensure reliability of p7 determinations. Additionally, method robustness should be tested to assure that the assay performance is suitable for QC environment. Quantitative parameters such as LOD/LOQ are not required for an ID assay. If a cIEF method is used for purity determination, then all the purity parameters shown in Section 4 should be qualified. The following sections illustrate an example of method development and qualification procedures for cIEF. 

References of Relevant Information List the internal and external instrument validation guidance documents, compendial reference methods, qualification testing, and related SOPs for validation. 

Rationale for the IND specifications (drug substance and drug product) Specifications (test, limits, and methods) for drug substance and drug product(s), including placebo (release and retest/stability, if different) Methods qualification/validation for methods included in IND specifications... 

METHOD DEVELOPMENT AND METHOD QUALIFICATION FOR EXPLORATORY APPLICATIONS... 

The method detection limit or limit of detection (LOD) and method qualification limit or limit of quantification (LOQ) for the matrix/analytes combination and the extraction/analysis procedure is computed as ... 

Methods qualification/validation for methods included in IND specifications Stability data... 

NDT has a very important formal status. Requirements for performanee of NDT, acceptance criteria and requirements for personnel qualification are implemented in codes and standards. The NDT procedure is part of the contract. During the many years that NDT methods have been used in industry a well-established situation has evolved, enabling the use of NDT for the evaluation of welds against Good Workmanship Criteria on a routine basis, thus maintaining workmanship standards and minimising the risks of component failure. 

It seems almost perfect. Established methods, established acceptance criteria, established procedures and personnel qualification schemes. Almost perfect. Because the reason of this presentation is, to show that things could be improved. 

In compliance with the requirements stated in the System of accreditation to the practical experience and qualification the technical manager in NDT must have at least level 2 on each of NDT methods used in the laboratory seeking accreditation, where not more than 3 NDT methods are in practice, and level 3 on the basic method used in the laboratory where there are more than 3 methods. Moreover all specialists must be certified in relevant NDT method and industrial sector. 

This approach enables also to substantiate acceptance criteria for detection and qualification limits in impurity control method validation. 

If a standard form was used in the qualification phase, a system should exist to rank the respondents that are being considered. Such a system can be as simple as the reviewers making a written recommendation summarizing the strong points of their selections. Some companies have developed forms that allow the final scores to be quantified. Appendix C, Sample Toller Assessment—Qjiantitative Format contains such an example. With either method, the client should consider having two or more reviewers discuss the candidates and agree on the recommended finalists. 

If the critical impurities are known, then only a selected list of elements need to be examined, with some improvement in the cost effectiveness of the analysis. However, the list of elements to be included in the qualification analysis is often historical and related to the limitations of the analytical methods previously used for qualification rather than for technological reasons related to the end use of the metal. As a result, problems in application can arise for no obvious reason. The time and cost of extending the impurity list for GDMS analysis to include essentially all elements is minimal, considering the additional information gained. 

Using fire models, locations of equipment, heat transfer calculations, and environmental qualifications of the equipment, it is possible to estimate the time to failure. Fragility cuives that relate fire durations and equipment damage while considering the probability of fire suppre.ssion are produced to relate to the overall PSA. These fragility curves and their use is simitar the methods ised for seismic analysis. 

Method of seismic and qualification and results for typical electrical abinets and switchgear. 

Materials selection for low-temperature service is a ecialized area. In general, it is necessary to select materials and fabrication methods which will provide adequate toughness at all operating conditions. It is frequently necessary to specify Charpy V-notch (or other appropriate) qualification tests to demonstrate adequate toughness of carbon and low-alloy steels at minimum operating temperatures. 

In 1965, Van der Grinten4 introduced the interesting concept of measureable-ness a as qualification of an analytical method in relation to the process to be regulated, with its specific fluctuation velocity. In this connection he also defined... 

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