Laboratory quality validated testing procedures

Validation Validation was defined in Section 3. It is the process of evaluating a method, an instrument or other piece of equipment, a standard material, etc. to determine whether it is appropriate for the work at hand and whether it will meet all expectations and needs for a given analysis. For example, an analyst may propose that a new gas chromatograph, one that has a new design of electron capture detector, be used for a certain pesticide analysis performed in the laboratory. A validation process would involve testing the new instrument (alongside the unit currently used in the procedure) with standards and samples used in the analysis to validate whether the new unit will perform up to the standards that have been set for the work. If it can be documented that the quality of the overall analysis by the new instrument meets expectations, then it can be brought "online."... 

Nowadays it is generally accepted that laboratory proficiency testing schemes are an important quality assurance tool in environmental monitoring programmes. Apart from using validated analytical methods and internal laboratory quality control procedures, the regular participation of laboratories in interlaboratory comparisons is required to ensure the accuracy and comparability of data. 

Quality measurements have several elements. Quality assurance plans and quality control procedures are an essential beginning. In addition, it is necessary to have qualified scientists whose training needs to be documented and updated on a continuous basis. Quality measurements also require proper use of reference materials where available, and laboratories must repeatedly test their ability to perform through taking part in proficiency testing schemes. The provision of another essential element in quality measurements, namely validated methods, is the primary contribution from the work of AOAC. 

Every manufacturer should have access to a control laboratory. The laboratory should be staffed and fully equipped for performing all quality control tests required. The tests should be performed in accordance with written and validated procedures, instruments should be calibrated at suitable intervals and reagents should be of appropriate quality. 

Analytical validation seeks to demonstrate that the analytical methods yield results which permit an objective evaluation of the quality of the pharmaceutical product as specified. The person responsible for the quality control laboratory should ensure that test methods are validated. The analytical devices used for these tests should be qualified and the measuring instruments used for the qualifcation should be calibrated. Each new test procedure should be validated. 

Nevertheless, it is important to point out that the laboratories where the different validation methods are carried out should be certified in the execution of the good laboratory practice (GLP). These principles of GLP are a group of rules, procedures and estabUshed practices and are developed by the OECD (Organisation for Economic Cooperation and Development). This normative has been assumed by the EU in the directives 87/18/CEE and 99/11/CE ""The purpose of these principles of good laboratory practice (GLP) is to promote the development of quality test data. Comparable quality of test data forms the basis for the mutual acceptance of data among countries. If individual countries can confidently rely on test data developed in other countries, duplicative testing can be avoided, thereby saving time and resources. The application of these principles should help to avoid the creation of technical barriers to trade, and further improve the protection of human health and the environment . 

The software life cycle activities extend until retirement of the software. However, in a manner of speaking, life cycle activities extend even beyond retirement since the data must be able to be reconstructed at any time during the life of the product, i.e., the archived record must always be accessible and readable even if the software is no longer commercially available or typically employed in the laboratory. Additional software validation includes implementation of the code and integration and performance testing. There also must be system security, change control procedures, audit trails, calibration, preventative maintenance, and quality assurance. 

By using the combination of specific method accreditation and generic accreditation it will be possible for laboratories to be accredited for all the analyses of which they are capable and competent to undertake. Method performance validation data demonstrating that the method was fit-for-purpose shall be demonstrated before the test result is released and method performance shall be monitored by on-going quality-control techniques where applicable. It will be necessary for laboratories to be able to demonstrate quality-control procedures to ensure compliance with the EN 45001 Standard,3 an example of which would be compliance with the ISO/AOAC/IUPAC Guidelines on Internal Quality Control in Analytical Chemistry Laboratories.12... 

The laboratory shall have quality control procedures for monitoring the validity of tests and calibrations undertaken. 

Traditionally, the education that chemists and chemistry laboratory technicians receive in colleges and universities does not prepare them adequately for some important aspects of the real world of work in their chosen field. Today s industrial laboratory analyst is deeply involved with such job issues as quality control, quality assurance, ISO 9000, standard operating procedures, calibration, standard reference materials, statistical control, control charts, proficiency testing, validation, system suitability, chain of custody, good laboratory practices, protocol, and audits. Yet, most of these terms are foreign to the college graduate and the new employee. 

Analytical method validation forms the first level of QA in the laboratory. Analytical quality assurance (AQA) is the complete set of measures a laboratory must undertake to ensure that it is able to achieve high-quality data continuously. Besides the use of validation and/or standardized methods, these measures are effective IQC procedures (use of reference materials, control charts, etc.), with participation in proficiency testing schemes and accreditation to an international standard, normally ISO/IEC 17025 [4]. Method validation and the different aspects of QA form the subject of Section 8.2.3. 

Accreditation is the procedure by which the competence of a laboratory to perform a specified range of tests or measurements is assessed against a national or international standard. The accreditation covers the kinds of materials tested or measured, the procedures or methods used, the equipment and personnel used in those procedures, and all relevant systems that the laboratory has in place. Once accredited, the laboratory is entitled to endorse test results with their accreditation status which, if it has any validity, is an imprimatur of some degree of quality and gives the client added confidence in the results. Accreditation therefore benefits the laboratory, by allowing the laboratory to demonstrate competence in particular tests, and the client, by providing a choice of accredited laboratories that are deemed competent. 

Laboratory equipment and procedures must be qualified and validated. Every NDA/ANDA inspection will include both an evaluation of laboratory controls and procedures and an audit of some of the raw data used to generate results. These data may be located in research and development test logs. The authenticity and accuracy of data used in the development of a test method should be established. (See the Guide to Inspection of Pharmaceutical Quality Control Laboratories, July 1993.)... 

Validation of testing methods always involves a balance between costs, risks and the technical capabilities of a given laboratory (NBN-EN-ISO-CEI 17025, 1999). Laboratory administrators must establish minimum quality requirements before starting the process of validation and implementation, or before starting the whole development process. Procedures of validation for a small laboratory could not be the same as for commercial validation of a new method, whether or not new kits from a manufacturer are used. There are many cases in which the range and uncertainty of the test result values can only be given in a simplified way due to lack of information. 

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