Review of European Union requirements: quality standards for food analysis laboratories

 The European Union has prescribed strict quality standards for official food laboratories and the methods of analysis to be used in laboratories when carrying out official food control work. These requirements, which are based on accreditation, participation in proficiency testing schemes and using validated methods of analysis, are described in detail. The similar approach being taken within the Codex Alimentarius Commission is also outlined. The procedures prescribed will ensure that official food control laboratories have in place the measures to ensure that consistently reliable data can be produced. Received: 29 November 1995 Accepted: 8 January 1996     

Development, validation and data quality assurance of screening methods: a case study

Despite the growing importance of qualitative screening tests in routine laboratories involved in the EU official control, their validation is not as deeply explained in Commission Decision 2002/657/EC as the validation of quantitative confirmatory methods. At the same time, the issue of quality assurance of screening assays defining internal quality control (IQC) procedures as required by accreditation bodies is undoubtedly less developed in this analytical field. As an example the present study describes the development, the validation and the IQC implemented for a commercial enzyme linked immunosorbent assay (ELISA) able to detect 17-α-19-nortestosterone (α-NT) and 17-β-19-nortestosterone (β-NT) isomers in bullock urine. In order to select a suitable sample treatment, two SPE purification protocols were preliminary compared. The chosen method was therefore fully validated determining the mandatory parameters required by Commission Decision 2002/657/EC: specificity, detection capability and robustness. An in-depth discussion was carried out illustrating the possible validation approaches and their implications especially in the assessment of the key performance characteristic: detection capability. Finally, the control charts implemented for continuous method verification during analyses of real samples were reported.     

Key requirements for introducing quality assurance in measurement laboratories

 The implementation of a quality assurance system is fraught with difficulties. However, these difficulties may be overcome if the laboratory uses suitable means to facilitate the process. It is necessary to mobilise the intelligence and energy of all members of the laboratory. In order to command adherence, the project must be shared, and this necessitates a major effort by all concerned. Communication is a major factor in obtaining the support of all parties. Six important steps must be distinguished: – Defining quality policy – Creating awareness, information, training – Creating a quality structure – Establishing a deadline for obtaining accreditation – Progressive implementation – Experimentation and validation. Even if the task of obtaining and maintaining accreditation remains difficult, it clearly promotes a minimum level of organisation and stepwise progress in quality assurance. The laboratory must keep improving its quality system, using European Standard EN 45001 as an effective management model. Received: 9 April 1997 · Accepted: 11 September 1997     

Quality assurance of qualitative analysis in the framework of the European project ’MEQUALAN’

 The European Commission has supported the G6MA-CT-2000–01012 project on ”Metrology of Qualitative Chemical Analysis” (MEQUALAN), which was developed during 2000–2002. The final result is a document produced by a group of scientists with expertise in different areas of chemical analysis, metrology and quality assurance. One important part of this document deals, therefore, with aspects involved in analytical quality assurance of qualitative analysis. This article shows the main conclusions reported in the document referring to the implementation of quality principles in qualitative analysis: traceability, reliability (uncertainty), validation, and internal/external quality control for qualitative methods. Received: 15 October 2002 Accepted: 20 October 2002 This paper is a summary of the Quality Assurance section included in the final report of the MEQUALAN project. The authors of this paper correspond to the members of the MEQUALAN Consortium. One of them (K.H.) does not fully agree with some parts of the text. Correspondence to A. Ríos     

The American (USA) perspective six years after implementation of CLIA'88 (Federal) regulations

 On September 1, 1992 all testing sites in the United States were required to comply with the Clinical Laboratory Improvement Amendments of 1988 (CLIA'88). These regulations, based on both total quality management (TQM) and continuous quality improvement (CQI) principles, reshaped the environment for more than 90% of laboratories. CLIA'88 represented a revolutionary change by imposing universal, uniform regulations based on test complexity for all sites examining materials derived from the human body for the purpose of providing information for the diagnosis, prevention, or treatment of disease. CLIA'88 specifies minimum requirements for personnel, quality control, and proficiency testing (PT). In addition, laboratories are required to follow manufacturers' directions and comply with other specified good laboratory practices. PT is mandated for most of the frequently run analyses and quality assurance requirements integrate the principles of CQI as well as TQM into the regulatory process. Biannual inspection is integral to CLIA'88, however, laboratories can choose other federally approved ("deemed") professional organizations, such as the Commission on Office Laboratory Accreditation, the College of American Pathologists, or the Joint Commission on Accreditation of Healthcare Organization, having standards that meet or exceed those of CLIA'88. CLIA'88 has still not been finalized. This article discusses the impact and changes since CLIA's implementation in 1992. Received: 5 October 1998 · Accepted: 20 October 1998     

Quality assurance in the view of a commercial analytical laboratory

 The necessity for analytical quality assurance is primarily a feature of the analytical process itself. With the full establishment of the EU domestic market, it is also becoming a legal necessity for an increasing number of analytical laboratories. The requirements which laboratories will need to fulfil are stipulated in DIN EN 45 001. Accredited testing laboratories must in fact provide evidence that they work solely in accordance with this standard. National and EU commissions, which are legislative authorities, tend therefore to specify analytical methods, e.g. in the form of regulations or appendices thereto, intended to ensure that results from different laboratories will be comparable and hence will stand up in a court of law. The analytical quality assurance system (AQS), introduced by the Baden-Württemberg Ministry for the Environment in 1984, obliges laboratories to regularly participate in collaborative studies and thereby demonstrate their ability to provide suitably accurate analyses. This alone, however, does not sufficiently demonstrate the competence of a laboratory. Only personal appraisal of the laboratory by an auditor, together with the successful analysis of a sample provided by the same and performed under his observation, can provide proof of the competence of the laboratory. From an analytical point of view, the competence of a laboratory must be regarded as the decisive factor. Competence can only be attained through analytical quality assurance, which thus must be demanded of all laboratories. Received: 4 October 1996 Accepted: 15 January 1997     

Reliability of food measurements – a South African perspective

 High quality analysis of food involves a comprehensive process, which includes proper sampling, validated methodology, experienced technical staff and the use of standard reference materials. Today there is more international emphasis not only on generating food composition data but also on data quality and the main issue is that South African data should be internationally recognized as acceptable and representative. Quality is multi-dimensional and should at least include aspects of accuracy, precision and representativeness. A major step forward is that laboratories can apply for accreditation, which involves, inter alia, documented, validated methodology, regular interlaboratory studies, the use of certified reference materials and the existence of a sound quality system. The South African National Accreditation System (SANAS) is a regulatory body in South Africa, which is internationally recognized. Assessment of laboratories against specific standards is performed regularly and laboratories have to comply with certain managerial and technical requirements. Once a laboratory is accredited, ongoing validation and verification of results as well as regular assessment ensure reliability of results and overall competency of the laboratory. With a quality assurance programme in place, the reliability of results of the Irene laboratory is beyond doubt and nutrient data could be included in food composition tables. Received: 31 January 2002 Accepted: 4 February 2002 Correspondence to Louwrens Erasmus Smit     

Reliability of measurement results in food microbiology: the contribution of reference laboratories in the European Union and of international/European standardization

The contribution of reference laboratories in the European Union and of European/international standardization to the reliability of food microbiology measurement results is discussed. A set of European Union reference laboratories has been established. Each of them coordinates a network of national reference laboratories which, in turn, coordinate networks of laboratories in charge of official testing and sometimes own checks in each European Union country. Their contribution to the reliability of food microbiology measurement results is illustrated by three food safety cases: Listeria monocytogenes, coagulase positive staphylococci and milk/milk products. The contribution of European/international standardization focuses on two topics: method validation and measurement uncertainty. The standards covering these topics—EN ISO 16140 and ISO/TS 19036—are briefly discussed, and an update given on their ongoing revision.     

Practical uses of proficiency testing as valuable tools for validation and performance assessment in environmental analysis

Besides their role as an external quality control tool, PT results or samples could be used as an alternative to fulfil some of the quality assurance requirements such as analytical precision, uncertainty assessment, and internal quality control. This additional use of proficiency testing could help laboratories to reduce the financial impact of their quality assurance process. The purpose of this paper is to highlight some practical uses of PT results or samples in the environmental analytical field, which have been implemented at ISSeP (Institut Scientifique de Service Public), either for method validation or for internal quality control.Presented at the Eurachem PT Workshop September 2005, Portorož, Slovenia     

External quality assurance programmes in medical laboratories

 Medical laboratories have a long tradition of external quality assessment. Starting from pure quality control of laboratory performances, most schemes have evolved to a powerful tool for improving quality of clinical outcome of results. External quality assurance in medical laboratories not only includes laboratory performance evaluation, but also evaluation of method performance, post-marked vigilance, training and help. In the future, the quality of programmes must further be improved by accreditation of schemes and by using electronic data interchange. Received: 9 December 2000 Accepted: 14 December 2000     

Quality assurance in analytical laboratories engaged in research and development activities

 Research and development activities are carried out by various types of laboratories that are not the typical testing and calibration laboratories for which the ISO/IEC 17025 is the quality assurance implementation reference. In this paper, such laboratories engaged in R&D activities are classified and different approaches they can adopt with a view to implementing a quality system that are suited to their characteristics and the type of work they conduct are proposed. These approaches take account of existing standards for the certification/accreditation of laboratories and of guides on quality assurance for non-routine analytical laboratories. Received: 11 July 2002 Accepted: 29 November 2002 Presented at Analytica Conference, 23–26 April 2002, Munich, Germany Correspondence to M. Valcárcel     

QASKI – the quality assurance system of the National Institute of Chemistry

 The quality assurance system (QASKI) developed and implemented in the National Institute of Chemistry is presented. It tries to eliminate the incompatibilies between the present methods of quality assurance used in research and development institutes such as good laboratory practice and accreditation. Since 1991, QASKI has been used for internal accreditation of laboratories located in the institute, regardless of the fact that some of them deal with routine analyses and others with research and development. Every laboratory that wishes to ensure the credibility of its research or routine work enters QASKI and at the same time chooses an external method of approval. All interested laboratories, study directors, principal investigators, internal auditing staff, heads of documentation, quality assurance unit staff, the Director of the institute and the Quality Management Board participate in the internal system.     

The College of American Pathologists laboratory accreditation program

The College of American Pathologists (CAP) operates voluntary programs in proficiency testing (PT) and quality monitors, which are briefly described. Additionally, a peer-based laboratory accreditation program covers over 6,100 clinical laboratories. Participation requires successful PT and on-site inspections using a series of 18 checklists structured along traditional subdisciplines of laboratory medicine and anatomic pathology. The laboratory general checklist contains over 250 questions covering broad issues affecting all disciplines. Among these are three items within the computer services section that specifically probe the laboratory’s use of autoverification. Data autoverification is defined as the process by which the computer performs the initial verification of test results; any data that fall outside of set parameters should be reviewed by the human operator. Central to these questions is the role of the laboratory director in approving the rules and validation. CAP does not define the specific technical details, recognizing the uniqueness of each laboratory setting and the patients it serves. Received: 8 August 2002 Accepted: 10 August 2002 Presented at the European Conference on Quality in the Spotlight in Medical Laboratories, 7–9 October 2001, Antwerp, Belgium Correspondence to A. Rabinovitch     

IMEP-12: trace elements in water; objective evaluation of the performance of the laboratories when measuring quality parameters prescribed in the European Directive 98/83/EC

The International Measurement Evaluation Programme (IMEP) is an interlaboratory comparison scheme, founded, owned and co-ordinated by the Institute for Reference Materials and Measurements (IRMM) since 1988. IMEP-12, for the fourth time in the series, focused on trace elements in water and it was designed specifically to support European Commission directive 98/83/EC. Reference values for the concentration of ten elements were established with expanded uncertainties according to GUM. In total, 348 laboratories from 46 countries in five continents participated in the comparison and the degree of equivalence between the results of the laboratories and the reference values is presented graphically. Samples from the same batch were distributed to ten laboratories from European Countries, which represented their country in the framework of the EUROMET project 528. Participation in this comparison was offered to the European Co-operation for Accreditation (EA) for participation of accredited laboratories from all over Europe in the framework of the collaboration between IRMM and EA and to laboratories from the EU new member states and acceding countries in the frame of IRMM’s ‘Metrology in Chemistry support program for EU new member states and acceding countries.’     

Interlaboratory comparisons – demonstrating degree of equivalence

 The role of matrix reference materials in the process of demonstrating the degree of equivalence of measurement results obtained from intercomparisons is outlined, reviewing exemplary selected experience gained at BAM regarding the determination of organic contaminants in environmental matrices. The specific characteristics of reference materials employed in the process of demonstrating equivalence between laboratories in the course of proficiency testing as well as the development, comparison and validation of methods are elaborated. The demand is for series of appropriately characterised samples which are fit for the purpose and it is seen from representative examples that the utilisation of such tailor-made RM designed to tackle the specific need of an analytical problem dominates over certified matrix reference materials in this context. Concluding, the role of certified matrix reference materials in quality assurance is briefly looked at both from the user’s and providers’ points of view. Received: 9 September 2002 Accepted: 16 December 2002 Presented at CERMM-3, Central European Reference Materials and Measurements Conference: The function of reference materials in the measurement process, May 30–June 1, 2002, Rogaška Slatina, Slovenia Correspondence to R. Becker     

IMEP in support of the comparability of measurement results across the Romanian chemical metrology infrastructure

On the basis of quantitative chemical measurements many important decisions are made in support of legislation or in industrial processes or social aspects. For this reason it is important to improve the quality of chemical measurement results and thus make them comparable and acceptable everywhere. The measurement quality is important to enable an equivalent implementation of the European Union regulations and directives across an enlarged EU. In this context, the European Commission–Joint Research Centre–Institute for Reference Materials and Measurement (EC-JRC-IRMM) set up a programme to improve the scientific basis for metrology in chemistry (MiC) in EU candidate countries in the framework of EU enlargement. Several activities were initiated, such as training, fellowships, sponsoring of seminars, conferences and participation in interlaboratory comparisons. To disseminate measurement traceability, IRMM provides through its International Measurement Evaluation Programme (IMEP) an interlaboratory tool to enable the benchmarking of laboratory performance. IMEP emphasizes the metrological aspects of measurement results, such as traceability and measurement uncertainty. In this way it has become a publicly available European tool for MiC. The Romanian Bureau of Legal Metrology – National Institute of Metrology (BRML-INM) actively supports the participation of Romanian authorized and field laboratories in IMEP interlaboratory comparisons. This paper describes the interest of Romanian laboratories participating in this programme, the analytical and metrological problems that became relevant during these exercises and some actions for improvement. The results from Romanian laboratories participating in IMEP-12 (water), IMEP-16 (wine), IMEP-17 (human serum) and IMEP-20 (tuna fish) are presented. To conclude, the educational and training activities at national level organized jointly by the Romanian National Institute of Metrology (INM) and IRMM are also mentioned.     

Quality management, certification and accreditation in medical laboratories – the view of ECLM

 Increasing demands from health care planners and industrialists conducting clinical trials, as well as general competition, are forcing medical laboratories to seek third-party recognition of their quality management systems. There is a tendency to move from certification of a laboratory director, via certification of the laboratory quality system (ISO 9000 family), to accreditation needing proof of professional and technical competence in laboratory tasks. The requirements of accreditation are presented in several national schemes and in the European Standards series (EN 45 000) and the International Organization for Standardization's guide, ISO/IEC 25, to be amalgamated soon. The latter system provides transnational recognition through participation of the accrediting bodies in the European co-operation for Accreditation. Necessary supplementary guidelines exist for chemical laboratories (Eurachem) and medical laboratories CEAC/ECLM). Traceability and reliability of results are obtained by utilizing a global reference examination system and by participating in transdisciplinary work. The costs of achieving accreditation are considerable and mainly involve the production of quality handbooks and written work procedures by personnel. The rewards are an open system, smoother work, emphasis on prevention of mistakes, and satisfied stakeholders. Received: 5 October 1998 · Accepted: 20 October 1998     

Development and in-house validation of an LC-MS/MS method for the determination of stilbenes and resorcylic acid lactones in bovine urine

Stilbenes and zeranol are nonsteroidal estrogenic growth promoters which are banned in the European Union (EU) for use in food-producing animals by Council Directive 96/22/EC. A liquid chromatography–tandem mass spectrometry (LC-MS/MS) method was developed for the screening and confirmation of stilbenes (diethylstilbestrol, dienestrol, hexestrol) and resorcylic acid lactones (zeranol and its metabolites taleranol and zearalanone as well as the mycotoxins α-zearalenol, β-zearalenol and zearalenone) in bovine urine. The method permits the confirmation and quantification of stilbenes and resorcylic acid lactones at levels below 1 μg L⁻¹ and 1.5 μg L⁻¹, respectively. The validation was carried out according to Commission Decision 2002/657/EC, Chap. 3.1.3 “alternative validation” by a matrix-comprehensive in-house validation concept. Decision limit CCα, detection capability CCβ, recovery, repeatabiliy, within-laboratory reproducibility and the uncertainty of measurement were calculated. Furthermore, a factorial effect analysis was carried out to identify factors that have a significant influence on the method. Factors considered to be relevant for the method in routine analysis (e.g. operator, matrix condition, storage duration of the extracts before measurement, different cartridge lots, hydrolysis conditions) were systematically varied on two levels. The factorial analysis showed that different cartridge lots, storage durations and matrix conditions can exert a relevant influence on the method.     

Accreditation of small laboratories

 This paper presents the result of an investigation concerning which areas of EN 45001 are considered as especially problematic by small laboratories (<10 employees). The investigation was performed by distributing questionnaires to European laboratories. To be able to differentiate between areas considered as problematic only by small laboratories and areas considered as problematic by laboratories in general, some questionnaires sent in by larger (>10 employees) laboratories were used. The determination of measurement uncertainties within reasonable efforts and the requirements to take part in round robin and proficiency testing were considered problematic by laboratories of all sizes. Training is an area where small laboratories have specific problems and so are the requirements for the identification of all equipment. Other problematic areas for small laboratories are areas were there are needs for personnel, e.g. appointing supervising personnel and expenditure for internal audits. The last area to be considered as problematic is matters concerning documentation. Finally some advice concerning assessment of small laboratories is given. Received: 25 February 2000 / Accepted: 20 April 2000     

Quality assurance in analytical measurement

 The peculiarities of analytical measurement require to check characteristics of the error (its components) of the obtained analysis results to assure the quality of the measurements. This article deals with the various quality assurance procedures and algorithms which are used to check the quality indices, i.e. the accuracy, reproducibility, certainty and repeatability of analytical measurements: These procedures include: laboratory rapid control; Intra-laboratory statistical control (statistical selection control by alternative attribute, statistical selection control by quantity method of periodic check of the analysis procedure for conformity to the specified requirements) and external control (inter-laboratory control checks, inter-laboratory comparison tests, and intra-laboratory control algorithms carried out by the appropriate supervisory body.) in the separately taken laboratory. The respective algorithms, control plans and control requirements, specified according to the different control aims and assurance tasks, enable the quality and certianty of analytical information obtained in laboratories in Russia to be assured. Received: 9 November 1998 / Accepted: 24 November 1998