The Cardbox/Cardview Database for residues in live animals and their products

The growing interest of the public opinion in environmental problems has resulted in the establishment of national and international norms and regulations. Among others, the protection of human health requires the constant monitoring of several groups of potentially toxic substances as well as of their residues in live animals and their products. For this reason in recent years the European Commission decided to establish four Community Reference Laboratories (CRLs) for the analysis of residues in products of animal origin. The current mandate and operative conditions of the CRLs are described in the Council Directive 96/23/EC of 29 April 1996, which has the goal of promoting and supporting the harmonization of approaches among National Reference Laboratories (NRLs). In this context the CRL at the Istituto Superiore di Sanità of Rome is responsible for chemical elements, organochlorine compounds (including PCBs), carbamates, pyrethroids and organophosphorus compounds. The supply of updated information on the literature of relevance to the tasks of the NRLs is one of the duties of the Rome CRL. To this end, the so-called Cardbox Database has been set up, which for the time being is fully operative for chemical elements and organochlorine compounds.     

A CRL–IRMM joint proficiency test for trace elements in fish tissue

The Community Reference Laboratory (CRL) for residues and contaminants in food of animal origin at the Istituto Superiore di Sanità (ISS) plans and undertakes on a regular basis Proficiency Tests Schemes (PTSs) focused on the residues under its responsibility, as prescribed by the Council Directive 96/23/EC of April 29, 1996. In consideration of the benefits ensuing from a constant monitoring of the daily activities of the National Reference Laboratories (NRLs) for residues in the Member States, the ISS–CRL frequently prepares test materials to promote comparability of data and support harmonisation of routine analytical procedures. When target values for the analytes are set, the PTSs also provide objective assessment and improvement of the analytical trueness in the daily work.In this context, an interlaboratory comparison for trace elements in tuna fish matrix was organised in cooperation with the Institute for Reference Materials and Measurements (IRMM), Joint Research Centre, European Commission. Freeze-dried tuna fish samples were sent out to the NRLs for chemical elements in the Member States. Participants were requested to carry out at least three independent measurements of the elements As, Cd, Cr, Cu, Fe, Hg, Pb and Zn. The assessment of the proficiency was based on the z-score approach and a relative bias better than or equal to 10% of the target value was deemed to be an acceptable performance for this kind of measurements. On this basis, more than 50% of the laboratories returned accurate results for As, Cu, Fe, Hg and Zn, whereas the analysis of Cd, Cr and Pb appeared to be more problematic.     

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     

Trace elements in bovine muscle: an ongoing project for a new certified reference material

In the framework of the activities of the Community Reference Laboratory (CRL) for residues at the Istituto Superiore di Sanità (ISS) of Rome, a number of proficiency tests were performed in order to assess and improve, wherever necessary, the quality of regulatory residue analysis within the EU. In this context, a pilot study was undertaken with the purpose of ascertaining the feasibility of a project for the certification of a new reference material for trace elements in bovine muscle. On behalf of the ISS, approximately 70 kg of bovine muscle, collected at a slaughterhouse in Geel (Belgium), were freeze-dried, homogenized, stabilized and bottled under argon atmosphere by the Institute for Reference Materials and Measurements, Joint Research Centre, European Commission (IRMM-JRC-EC). Preliminary analyses were carried out with Quadrupole (Q) and High Resolution (HR) Inductively Coupled Plasma Mass Spectrometry (ICP-MS) to evaluate the content of As, Cd, Cu and Pb, whereas the Flow Injection Mercury System (FIMS) was used to quantify Hg. Digestion of the matrix was achieved by acid-assisted microwave irradiation. The mean values of experimentally obtained data were the following (in nanograms per gram): As, 24.2±1.2; Cd, 5.48±0.29; Cu, 4765±95; Hg, 3.37±0.73; and Pb, 184±7. Subsequently, 16 National Reference Laboratories (NRLs) for residues in the Member States plus the Norwegian one and eight Italian public laboratories were accepted to participate in the project and received one bottle of the freeze-dried bovine muscle. The laboratories were requested to perform three different analytical runs (in three different days), each consisting of three individual measurements. Preliminary results showed good agreement and fair evidence for homogeneity of the entire mass, thus setting the stage for the future certification of this candidate CRM.     

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     

Quality assurance in research laboratories

During the last decade, it has become increasingly important that researchers demonstrate that research is conducted to the highest standards. The implementation of quality assurance for research laboratories will enable all fields of research and development to be judged impartially. There are no specific standards for research laboratories but where possible, existing standards can be adapted. This review is structured around two approaches. The first considers research to be a logical extension of testing, and it is assumed that testing standards can be applied methodically to each step in a research project. The second advocates a flexible approach, with research-specific criteria for assessing quality. The important papers published on this topic have been reviewed. The conclusions are that the general quality management approach, encompassed by the ISO 9000 series of standards with the emphasis on customer satisfaction and ‘fitness for purpose’, is suitable for implementing quality assurance in research laboratories.     

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     

Quality assurance in the microbiology laboratory

 The pertinent issues necessary for the establishment of quality assurance in the microbiology laboratory are discussed. Quality assurance is a planned system of control measures that enables management to ensure that the analytical data produced in the laboratory are valid. To introduce quality assurance, all activities in the laboratory that affect the production of analytical data must be documented and controlled. These include sampling, method selection, laboratory environment, equipment, reagents and media, staff, reference materials and internal and external quality control. Laboratory accrediation in accordance with EN45001 and ISO Guide 25 enables laboratories demonstrate to an external agency their ability to perform analytical work and produce valid analytical data. This gives creditability to the laboratory and allows management to have confidence in the data produced. Received: 6 June 1995 Accepted: 3 July 1995     

Are there two decks on the analytical chemistry boat?

 This paper examines some problems of implementation of quality assurance (QA) principles in chemical measurement in the university academic environment. Being developed and introduced in practice by industrial and independent commercial laboratories, the 'quality lifestyle' has been largely ignored by the academic analytical community. The academic community is now faced with the fact that teaching, education and training of analytical QA and analytical quality management are no longer a matter of choice.     

Alternative methods for internal quality control in research laboratories for environmental analysis: a programme for the performance evaluation of equipment, methods and staff

In analytical research laboratories, the problem of quality assurance is more difficult to solve than in laboratories devoted exclusively to routine analysis: the former usually have to deal with a much greater variety of samples and may have to develop entirely new methods of analysis. For research laboratories we have developed several alternative methods of quality assurance. These methods can be used to distinguish between different analytical methods, between different types of equipment, between different levels of skill among laboratory technicians, or even between the performance of technicians of the same level of skill.     

The current state of analytical control in Lithuania

In Lithuania research and development in chemical analysis are concentrated in scientific institutes and universities. The main fields of interest focus on biosensors, electrochemical sensors, sampling techniques and methods, study of atomization processes in spectrochemical analysis and noise evaluation in analytical measurements. Some laboratories also take part in international environmental monitoring programmes. There are about 50 researchers at the Ph.D. level engaged in analytical chemistry and several hundred technicians specialized in the field of analytical control. About one hundred chemical laboratories are active in scientific institutes, universities and factories. Specialized laboratories of chemical analysis are at the disposal of Environmental Control and Health Protection Departments and forensic investigation organizations. So far no laboratories are accredited according to the ISO 9000 norms. Special courses on analytical chemistry are offered at a few schools of higher education in the country. Only at the Department of Analytical Chemistry of the University of Vilnius specialized programmes are available to postgraduate students working towards a Ph.D. to improve their skills in current techniques of analytical chemistry. Recently the Technical Committee TC-16 for Chemical Analysis was formed within the standardization system of Lithuania. Its main activities are centered on issues such as national terminology, certified reference materials (CRMs), analytical methods and analytical quality assurance. There are numerous problems related to national terminology, the preparation of special documents in the field of analytical control and the production of regional environmental CRMs. Problems, also arise in obtaining and using CRMs for analytical instrument calibration and validation.     

An overview of reference materials prepared for standardization of DNA typing procedures

Although DNA typing is an accurate, precise, and robust procedure, quality assurance is enhanced by availability of a suitable reference material. The National Institute of Standards and Technology (NIST) recently released a Standard Reference Material (SRM) that meets the calibration and quality assurance needs of laboratories that perform DNA typing. Each step of the analytical process of DNA typing may be verified by one or more of twenty different components of the SRM. As newer, more sensitive methods for DNA typing have been introduced into the human identification laboratory repertoire, new SRMs will be required for quality assurance. A second SRM for PCR-based tests is under development and soon to be available, is also described.     

From misconception to a must: The measured merits of total quality management and accreditation in INAA

Increasingly govemmental bodies and industry require that supporting analytical laboratories have their quality assurance program implemented in a quality system by international standards such as derived from the ISO-25 guide. Neutron activation analysis (NAA) laboratories may have to deal with this trend too. In universities and research laboratories the need for it, and the implications of total quality management system are sometimes misconceived by unfamiliarity with the issue. The laboratory for INAA in Delft has been accredited for its quality system since 1993. Some of the tangible improvements since the introduction of quality management are presented. Four strategical considerations are given to consider the introduction of quality management at NAA laboratories, viz. with respect to the role of NAA for the validation of other methods, the role of NAA in the certification of reference materials, the preservation of knowledge and the acceptance of NAA as a respectable method.     

Different approaches to legal requirements on validation of test methods for official control of foodstuffs and of veterinary drug residues and element contaminants in the EC

 In order to ensure food consumer protection as well as to avoid barriers to trade and unnecessary duplications of laboratory tests and to gain mutual recognition of results of analyses, the quality of laboratories and test results has to be guaranteed. For this purpose, the EC Council and the Commission have introducedprovisions – on measures for quality assurance for official laboratories concerning the analyses of foodstuffs on the one hand and animals and fresh meat on the other, – on the validation of test methods to obtain results of sufficient accuracy. 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 requirements have to be revised and further additions have to be made.     

A harmonized European framework for method validation to support research on emerging pollutants

Any investigation of environmental processes related to chemical substances or their effects depends on reliable, comparable analytical data. This also holds true for the impact of climate change on occurrence, distribution and effects of emerging pollutants, with respect to which there is particular concern regarding the reliability of analytical data, due to lack of harmonization in method validation and requirements for quality assurance and quality control (QA/QC).We present a recent European approach to developing a harmonized framework for method validation, QA/QC and provision of environmental data on emerging pollutants. The validation approach has been tested and improved by three case studies. We outline the main concept of the validation approach as well as the results of the case studies. This European validation framework turned out to be a feasible tool to check the fitness for purpose of analytical methods and to improve the reliability of environmental analytical data, particularly for emerging pollutants.     

Reference materials for large-scale metal deposition surveys

 In order to ensure quality assurance in large-scale environmental contamination studies involving many different analytical laboratories, the use of calibrated reference materials is essential. Prior to a survey of atmospheric metal deposition in 1995 comprising 20 countries and covering large parts of Europe, the lack of suitable reference materials of moss and organic-rich soil was apparent. In order to improve the quality of analytical data to be produced in this international survey, candidate analytical laboratories were invited to participate in an intercomparison exercise. Three moss and three soil humus reference samples specifically prepared for this purpose were distributed anonymously among the laboratories, which were asked to report data for ten priority elements (V, Cr, Fe, Ni, Cu, Zn, As, Cd, Hg, Pb) and as many additional elements as they determined normally. In this paper the analytical data from the intercomparison are evaluated, and recommended values for the ten priority elements and 17 additional elements (B, Na, Mg, Al, S, K, Ca, Mn, Co, Se, Rb, Sr, Sb, Cs, Ba, La, Th) in each of the six reference samples are established. These samples should be useful for similar future studies including areas where the contamination levels are very low. Received: 17 October 1996 Accepted: 2 January 1997     

EC initiatives for quality assurance training in analytical chemistry

Quality in the analytical laboratory is essential nowadays, must prove to meet the needs of customers, attract their confidence (and that of others who make use of the results), and represent value for money. There are innumerable areas where the results of chemical analysis are important (e.g., in the determination of the quality of manufactured products, in support of health and safety, in establishing environmental legislation, and in forensic science). However, although the concept of quality control and quality assurance is well understood by modern laboratories (whether commercial or with national responsibilities) –which are often accredited in various analytical sectors – there is an enormous gap in the transfer of knowledge to smaller laboratories. Training actions are therefore urgently needed, especially for analysts working in routine laboratories. This article describes two initiatives carried out under the umbrella of the EC Standards, Measurements and Testing Programme.     

Interlaboratory study to improve the quality of trace element determinations in rainwater

This is the first publication which describes the development of a reference material (RM) for the determination of 11 trace elements (Cu, Pb, Mn, Ni, Zn, Fe, Cd, Co, V, As and Al) in rainwater at microgram per liter concentrations. An interlaboratory comparison study for the determination of trace elements in rainwater was carried out for material performance studies to establish analyte concentrations with a stated uncertainty. Fifteen reputed laboratories from Asia, Europe and North America participated in the study. These laboratories used their regular in-house methods to analyze the rainwater samples. The aim of this study is to establish concentration levels of trace elements in rainwater based on interlaboratory study results. Details of the production, homogeneity and stability of the reference sample are given in this article. The organization of the study and the quality assurance measures undertaken at the organizer's laboratory are described. The analytical results obtained from individual laboratories and the analytical methods used for the determination of trace elements in rainwater are discussed. Based on the results obtained from the intercomparison study, certified values as well as informative values are assigned to the 11 trace elements in rainwater.     

Determination of essential and potentially toxic trace elements in honey by inductively coupled plasma-based techniques

The mandate assigned by the European Union to the Community Reference Laboratory for residues at the Istituto Superiore di Sanità covers, among other things, the assessment of trace elements in living animals as well as their products. To better protect the health of the consumer, this task aims in particular at harmonizing the procedures in use at the National Reference Laboratories (NRLs) for residues of the Member States for such determinations as well as at developing new approaches wherever the need arises. In this context an investigation was undertaken to appraise the average levels of a number of key elements in several types of honey with special regard to the influence of the various processing steps. Instrumental methods of election for the analysis of this matrix turned out to be inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS) depending on the actual concentrations of the elements of interest. Dissolution of the samples for suitable presentation to the analytical systems could be easily achieved by gentle heating at ca. 50 degrees C, sonication and addition of high-purity water. The ranges ascertained are as follows (in ng g(-1)): As, <0.50-0.70; Cd, <0.50-0.74; Cr, 1.03-3.93; Cu, 144-216; Fe, 191-651; Mn, 223-580; Ni, 17-49; Pb, 3.20-186; Pt, <0.50; Sn, <4-27; V, 1.22-1.94; and Zn, 565-1144. As a rule, concentrations of elements in honey from different beehives were similar. A few exceptions were noted for As, Cu, Fe, Ni and Zn. On the other hand, although data obtained with different analytical approaches for the same types of honey and beehive were generally in good agreement, yet some inconsistencies occurred, as in the case of Cu in freshly collected, extracted and ripened honey, Ni in extracted honey and Fe in ripened honey. These could not be traced back to specific procedural facts; rather, they should be ascribed to the inherent heterogeneity of the raw material. The experience gained with this exploratory study will be exploited to set up wider surveys and to plan the preparation of a new certified reference material in a matrix of honey to the benefit of NRLs for residues.     

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.