European standard method validation

The method was applied for determination of the quality of the detection media on test pieces following the type testing of the European standard [4] in order to check the validity of the method. The other application was the determination of the visibility in dependance of the variations of the inspection parameters (application of the detection medium, magnetization, inclination, viewing conditions) in a range which may appear in the practical inspections. The results leads to conclusions on the visibility level which is a measure of the probability of recognition for the indication that means of the reliability of the method. 

The integration of analytical methods in European standards requires their acceptance by several national experts within special working groups and in a final weighted vote of National Standards Bodies. Therefore, there needs to be very high confidence in the performance of methods. Consequently, methods should be tested in inter-laboratory method validation studies, with the exception of those multiresidue methods which are widely used throughout Europe. In the case of CEN methods there is no doubt about residue definition but detailed requirements about the number of matrices and concentration levels in validation experiments do not exist. Eor this reason it may be that CEN methods are validated for important crops only. 

Multi-residue Method S19 of the DFG Manual,including Cieanup Procedure Xll-6 (gel-chromatographic cleanup), has been used successfully in many laboratories because of its broad applicability for the gas-chromatographic determination of pesticide residues in foodstuffs. DFG method S19 is also included in the respective European Standards. Subsequently, a modification of the extraction and partition step has been implemented. The modified method requires less experimental effort and eliminates the use of dichloromethane, which is an undesirable solvent for toxicological and ecological reasons. As the results from validation studies demonstrate,... 

Significant progress has been made in the field of analytical detection of irradiated food to improve consumers confidence and to assist international trade of irradiated food [135,136]. Due to national and international programs and activities of the European Committee for Standardization (CEN), five validated and standardized detection methods are now available. The CEN is also considering the adoption of further five detection methods three will be screening methods (positive results from a screening method must be confirmed using a standardized method) [136]. 

Generally, the analysis of environmental pollutants is considered as a necessary expense that is performed solely if stated by law. With less expensive screening methods and automated modern equipment to analyze suspect samples, the cost of analysis will become much lower. Hence, the attitude towards QA would most probably be more positive and the analytical work much more reliable for the customers. This also strengthens the international competitiveness of European producers. The credibility of the entire monitoring chain (screening methods, reference and standardized methods, as well as CRMs for the quality control of these methods) lies in the adequacy and integration of all three levels of the system. The adequate development and validation of methods is a prerequisite for a harmonized measurement system [80]. 

Its implementation is easy in small countries due to centralization of management and ease of surveillance of this new form of accreditation by a national accreditation body. Due to the long-standing establishment of validation of food microbiological methods in some countries, the beginning of validation of water microbiological methods, and establishment of European standards for the validation of food microbiological test methods (Microval project), the flexible-scope type of accreditation must be adapted to certain national requirements, but could prove less complex than the standard requirements. 

This article deals with legal requirements in the European Union on basic principles of laboratory quality assurance for official notification to the EC Commission and on method validation concerning official laboratories. Widespread discussions and activities on measurement uncertainty are in progress, and the European validation standards for official purposes may serve as a basis for world-wide efforts on quality harmonization of analytical results. Although much time has already been spent, definitions and require-... 

Analytical methods and specifications must be established and validated so as to define and control the quality and purity of the raw materials, intermediates and the finished product. For many standard chemical raw materials, the development of specifications will not be necessary as they are already published in US and European pharmacopoeia (for example, standards for water, organic solvents and various excipients). The ultimate objective of these activities is to be able to manufacture the drugs required for clinical trials in accordance with good manufacturing practice (GMP). 

Thus, as for the European Union, the requirements are based on accreditation, proficiency testing, the use of validated methods of analysis and, in addition, the formal requirement to use internal quality control procedures which comply with the Harmonised Guidelines. Although the EU and Codex Alimentarius Commission refer to different sets of accreditation standards, the ISO/IEC Guide 25 1990 and EN 45000 series of standards are similar in intent. It is only through these measures that international trade will be facilitated and the requirements to allow mutual recognition to be fulfilled will be achieved. 

The European Commission has mandated the European Committee for Standardization to establish a validated method of analysis for the determination of OMLs and SMLs. If a product complies with the compositional requirements of the directives, i.e., it is produced from authorized monomers and additives, then it may be tested for any desired application. If it meets the migration requirements, it is acceptable for use in cases covered by that test method. Typical food simulants used in the tests are hot water, acetic acid, ethyl alcohol and olive oil. The choice of an appropriate simulant depends on the type of food expected to come into contact with the packaging. 

Following the success of these collaborative trials, standard methodologies for the application of the EPR method for the identification of irradiated meat bones, fish bones and some fruits have been prepared and are about to be submitted to the European Committee of Normalization. At the time when these trials were carried out there was not sufficient information available to permit inclusion of Crustacea among the products being examined and thus validation of the method for the identification of these irradiated foods has to be undertaken. 

It is interesting that regulations such as these are not effective in isolation. For example ER 3 of the CPD, requiring that chemical emissions from products used indoors must not adversely impact the indoor environment, became European law in 1989. However, it has not yet been effectively implemented. This is partly because there has not, hitherto, been a validated and broadly applicable (horizontal) standard test method available to carry out emissions measurement in compliance with the regulation. 

Continuing with the above example of ER3 of the European Construction Products Directive horizontal emissions test methods (i.e., applicable to multiple product types) have been developed by CEN and ISO for compliance with the CPD and are now available as parts 6, 9,10 and 11 of EN/ISO standard 16000 (see Table 6.1). Furthermore, a program of work led by CEN TC351 has now been instigated under European Council Mandate M/366 to amalgamate and validate these standards. Once this work is completed (estimated 2010) it is understood that chemical emissions testing will become a mandatory part of CE marking for construction products. 

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