Analytical Method Validationanalytical procedures is equally important to those listed herein, and it may be addressed in subsequent documents. Category II Analytical performance characteristics Category I Quantitative Limit tests Category III Category IV Wide Spectra of Quality Control 8experiments so that, with a minimum number of control analyses, the method and the complete analytical system will provide long-term results to meet the objectives defined in the scope of the method.
Documentation
Validation protocolDepending upon of the culture of the company, a method validation protocol could be simple (listed below) or exhaustive (in addition to the listed items, each parameter to be validated is described in detail): How solutions are going to be made, the experimental design, how the calculations are going to be performed, any software to be utilized (e.g., Excel). If a full-length protocol is required within a particular company, then the writing of this protocol and approval of the protocol would need to be completed prior to the commencement of the validation work. Otherwise, there may be many deviations to the protocol which will be needed to be referenced in the final method validation report. Some companies also have templates for the validation reports, thereby allowing for facile population of the results. Once populated, the file is reviewed to determine if all validation parameters and acceptance criteria were met. If they were not met, a deviation is added and the proper justification must be given. If it is deemed that the justification is not appropriate, then an action plan for the specific figure of merit in question is determined (i.e., repeat analysis, change of the analytical procedure, and revalidation). Also, if the analytical method has not been approved at the time of writing the validation protocol yet, it is recommended to attach a final draft of the method to the protocol. Before starting the experimental work, the protocols must be written by a qualified person and approved by a quality assurance department. Some of the items that are necessary to be specified in the validation protocol are listed below:• The analytical method for a given product or drug substance.• The test to be validated.• The test parameters for each test, including type and number of solutions and number of tests. • The acceptance criteria for each parameter based on an internal standard operational procedure (product or method-specific adaptations may be necessary and are acceptable, if justified). • List of batches of drug substance and/or drug products.• For a drug product the grade/quality of the excipients used in the formulation.• List of reference materials to be used in the validation experiments.• Information of the instruments and apparatus to be used.• Responsibilities [author, chemists, analytical research project leader, quality assurance, and etc.].Wide Spectra of Quality Control 20
ConclusionThis chapter described the fundamentals and figures of merit for method validation in pharmaceutical anal...