Accreditation and Quality Assurance (v.22, #2)

Current American landscape in laboratory accreditation according to ISO/IEC 17025 by Inês Hexsel Grochau; Carla Schwengber ten Caten; Maria Madalena de Camargo Forte (57-62).
The number of laboratories worldwide seeking accreditation has increased considerably in the last years. These laboratories are from different institutions, some of them higher education institutions (HEIs) and research institutes. The aim of this work is to present the current landscape of accreditation of testing and calibration laboratories, according to ISO/IEC 17025 standard, in the American Continent (North, Central and South America). Data on accredited laboratories were taken from the Web sites of accreditation bodies signatories to the International Laboratory Accreditation Cooperation Mutual Recognition Arrangement. The accredited laboratories were classified by institution type. Countries with a high number of accredited HEI laboratories were identified, as well as a correlation between gross domestic product and total number of accredited laboratories. North American countries have the highest total numbers of accredited laboratories, except for Brazil in South America. This survey highlights strategies and activities adopted in some countries that resulted in high number of accredited HEI laboratories.
Keywords: University testing laboratory; Laboratory accreditation; ISO/IEC 17025; American Continent

Overview of proficiency testing provision in pharmaceutical area in Brazil and an educational scheme for determining mefenamic acid in raw materials by Carlos Eduardo de Oliveira Pereira; Mateus Araújo Castro e Souza; Gerson Antônio Pianetti; Scheilla Vitorino Carvalho de Souza (63-72).
An historical review indicated that the provision of proficiency testing (PT) in the pharmaceutical area in Brazil is critical. Three providers were identified in the period between 2002 and 2015; only one provider was regular, but none was accredited according to the requirements of ISO 17043. A PT was organized without registration fees for educational purposes for the determination of mefenamic acid (2-[(2,3-dimethylphenyl)amino]benzoic acid) in raw materials. Proficiency test items consisted of a mixture of mefenamic acid and polyvinylpyrrolidone in the mass ratio 90:10. This proportion was used to simulate an adulterated raw material. Homogeneity and stability testing was performed and indicated that the materials were suitable for use in the PT scheme. First, 68 pharmaceutical laboratories, of which five were ISO 17025 accredited, were contacted to disseminate information about the specific PT and the benefits of this important quality assurance tool. Then, the proficiency test items were sent to the 13 registered participants, of which two were ISO 17025 accredited. In addition, the participating laboratories were surveyed regarding the technical and management aspects of their quality management system (QMS), such as the status of the accreditation process according to the ISO 17025 requirements, staff training, equipment calibration and participation in other PT schemes. All 11 participants that reported results in the study adopted the United States Pharmacopoeia Official Method. Only one laboratory, representing 9.1 % of the participants, had an unsatisfactory z-score result. Factors such as the reduced number of ISO 17025 accredited laboratories, the low number of participants in the educational PT, the high proportion of laboratories that participated for the first time and the portion of the participants who did not know about PT and its importance were considered as determinants for the restricted availability of the PT supply for medicines, as evidenced in the present study in Brazil. Thus, an urgent need for nationwide actions was identified to promote the critical consciousness of managers regarding QMS in pharmaceutical laboratories, including the importance of participation in PT schemes, as well as the importance of encouraging the providers already structured to broaden their scope in this area.
Keywords: Proficiency testing; Pharmaceutical analysis; Mefenamic acid; ISO 17043

New Japanese certified reference materials for electrolytic conductivity measurements by Toshiaki Asakai; Igor Maksimov; Sachiko Onuma; Toshihiro Suzuki; Tsutomu Miura; Akiharu Hioki (73-81).
The National Metrology Institute of Japan (NMIJ) has established three certified reference materials (CRMs) in electrolytic conductivity with a primary Jones-type cell: aqueous solutions of potassium chloride with different molalities (1 mol kg−1, 0.1 mol kg−1 and 0.01 mol kg−1) all supplied in glass bottles. The uncertainties were estimated from standard uncertainties of measurements (impedance, temperature and integrity of cell geometry), measurement’s repeatability, homogeneity of a batch and the storage stability of solutions. The storage stability of candidate NMIJ CRMs of upper and lower concentrations was examined with a secondary cell.
Keywords: Electrolytic conductivity; Jones-type cell; Potassium chloride; Electrochemical impedance spectroscopy; Certified reference material

Criteria for using proficiency test results for estimation of measurement uncertainty: feed analysis example by Waldemar Korol; Jolanta Rubaj; Grażyna Bielecka; Sławomir Walczyński; Joanna Reszko-Zygmunt; Ryszard Dobrowolski (83-89).
On the basis of long-standing proficiency testings (PTs) for the small number of PT participants p (7 ≤ p ≤ 30), laboratory bias and uncertainty were calculated by applying inter-laboratory experimental approaches. Uncertainty was estimated in two ways, according to Eurolab TR No 1/2007 and Nordtest TR 537 (2012). In the case of 24 tested feed components (basic nutrients, macro- and microelements, undesirable elements and some feed additives including vitamins A and E, lysine, threonine, methionine and urea) in the large variety of feed samples, differences between the expanded uncertainties calculated according to Eurolab TR No 1/2007 and Nordtest TR 537 did not exceed 1.4 % for all tested feed and analytes in wide concentration ranges. In order to get a reliable evaluation of bias and uncertainty, minimum of 6 PT rounds and a sufficient number of laboratories participating (p ≥ 10) are recommended. When the above parameters are applied and the standard deviation of the bias s bias ≤ 5 %, the expression s bias 2 /n can be omitted while calculating bias. Generally, both approaches fit the purpose of feed evaluation and the calculated uncertainties can be used for compliance assessment.
Keywords: Feed proficiency testing; Bias; Uncertainty; Practical approach; Within-laboratory reproducibility

LC–MS/MS quantification of ractopamine in bovine and swine muscle: stability of matrix-matched calibration solutions by Leila Rodrigues Caldeira; Josefa Abucáter Lima; Flávio Alves Santos; Mary Ane Gonçalves Lana; Ana Cláudia dos Santos Rossi Ribeiro; Elcio Cruz de Oliveira (91-96).
Ractopamine is used as an animal feed additive, but its adverse effects led to the necessity of the current monitoring programs of ractopamine residues in food products, so its reliable quantification is indispensable. This work aims to demonstrate the stability of solutions of ractopamine used for calibration of a liquid chromatography–tandem mass spectrometry method. Naturally contaminated samples with ractopamine were quantified using solutions prepared on different days. The stability study was based on an empirical model that considered a straight line (slope = 1) to describe the degradation mechanism. No significant change in the slope was detected. It could be concluded that solutions underpinning calibration curves at two different working intervals were stable for at least 11 months and 5 months, respectively.
Keywords: Stability study; Ractopamine; Calibration solutions; Bovine and swine muscle; Liquid chromatography–tandem mass spectrometry (LC–MS/MS)

More and more testing procedures with different principles are being developed covering both quantitative and qualitative analyses. To ensure the reliability of them and relevant testing results, performance evaluation and method validation are necessary. Following the investigation into a variety of testing procedures, this paper is intended to discuss the rational classification of them according to the nature and purpose of testing. Five kinds of testing procedures are summarized according to different combination of input and output properties of the testing model, which are properties on nominal, ordinal, interval and ratio scales. On this basis, the method validation and performance evaluation parameters, statistical approaches and tools available for each group of testing procedures are discussed. The classification of testing procedures seems helpful for inter-comparison of testing procedures with different purposes and application fields, and the development of some general rules for the performance evaluation and validation of them.
Keywords: Testing procedure; Method performance; Method classification; Validation

Risk-based thinking for chemical testing by Siu-kay Wong (103-108).
As a result of the changes to the ISO 9001 in 2015, integration of risk-based thinking into the quality management system is going to be a new requirement in ISO/IEC 17025. Though the concept of risk should not be new to the testing laboratories as it has been implicit in the previous editions of ISO 9001 and ISO/IEC 17025 as well, there might be concern on how risk-based thinking could be introduced to their daily operations in a practical and effective way. As a means to address the concern, this paper recommends an initial process review followed by an ongoing risk management process. Besides, a number of potential risks were identified and ways to avoid them were also discussed. Furthermore, there were discussions on the implementation of the risk management process and how could the management make use of the outcome of regular assessments to explore opportunities for increasing the effectiveness of the management system, achieving improved results and preventing negative effects.
Keywords: ISO/IEC 17025; Risk-based thinking; Quality management system