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Accreditation and Quality Assurance: Journal for Quality, Comparability and Reliability in Chemical Measurement
Journal Prestige (SJR): 0.316

Citation Impact (citeScore): 1
Number of Followers: 27

Hybrid journal (It can contain Open Access articles)
ISSN (Print) 0949-1775 - ISSN (Online) 1432-0517
Published by Springer-Verlag

[2351 journals]

Evaluation of implementation of good quality management practices related
to the support processes in the laboratories of Moroccan faculties of
sciences and techniques
- Authors: Meriem Outaki; Ebrahim Kerak
  Pages: 257 - 267
  Abstract: The evaluation practices in the higher education in Morocco constitute a constitutional and legal requirement and also respond to the requirements of the national and international environment in perpetual evolution. To identify the level of application of good quality management practices related to the scientific research in Morocco, a questionnaire was administered to the research laboratories managers of the faculties of sciences and techniques on a national scale with a percentage of answer of 33 %. This paper concerns the evaluation of the implementation of theses good practices related to the support processes such as the management of material, human and informational resources. The results of this study showed the dissatisfaction of the majority of laboratories managers with regard to their availability. Besides, a minority of the laboratories respect practices related to the control of the function metrology and to the storage and the traceability of reagents. More than two-thirds managers asserted that their research teams are established on the basis of the affinities of the thematic of research of the researchers and are convinced of the homogeneity of the composition of the laboratory teams. This study emphasizes the necessity of increasing investment in the domain of scientific research to improve the availability of the resources. It is also necessary to sensitize the laboratory staff to the importance of the implementation and control of the metrology function to assure reliability of the research results.
  PubDate: 2018-10-01
  DOI: 10.1007/s00769-018-1336-6
  Issue No: Vol. 23, No. 5 (2018)
Correction to: Measurement uncertainty: requirements set in the
accreditation standards
- Authors: Kyriacos C. Tsimillis
  Pages: 253 - 253
  Abstract: Unfortunately, the references 12 and 13 were incorrectly published in the original publication. The correct references are:
  PubDate: 2018-08-01
  DOI: 10.1007/s00769-018-1323-y
  Issue No: Vol. 23, No. 4 (2018)
Cooperation in publicly funded reference material production
- Authors: Håkan Emteborg; Doris Florian; Steven Choquette; Stephen L. R. Ellison; Maria Fernandes-Whaley; Lindsey Mackay; Pearse McCarron; Ulrich Panne; Sylvia G. Sander; Sook-Kyung Kim; Andrea Held; Thomas Linsinger; Stefanie Trapmann
  PubDate: 2018-10-12
  DOI: 10.1007/s00769-018-1349-1
Provision of proficiency testing for histamine mass fraction in canned
tuna to improve the capability of chemical laboratories in the Philippines
- Authors: Benilda S. Ebarvia; Aaron Dacuya; Sharlene R. Cabanilla; Natividad R. Mamplata
  Abstract: In this work, two reference materials (RMs) for mass fraction of histamine in canned tuna were developed to address the need of local testing laboratories for matrix RMs and a PT scheme for histamine. A validated method using HPLC with fluorescence detector (340 nm for excitation and 445 nm for emission) was applied with post-column derivatization for the RM’s homogeneity and stability studies. Acceptable results were obtained after statistical evaluation of homogeneity and stability according to IUPAC Harmonized Protocol and ISO Guide 35, respectively. Two PT exercises for histamine determination based on ISO/IEC 17043 were organized in 2014 and 2015 with the assigned values of 148 and 65 mg/kg, respectively. These reference values were obtained using exact matching liquid chromatography–isotope dilution mass spectrometry (LC–IDMS) with gravimetric sample preparation. The corresponding uncertainty of the reference value was obtained by ISO GUM approach where the characterization of the sample gave the highest contribution (41 %). The satisfactory z-score performance evaluated from the 12 laboratories was 50 % and 58.3 % in the first and second PT round, respectively. Most of the laboratories used AOAC Official Method 977.13 but not all conducted method validation. The 50 % decrease in unsatisfactory results in the second PT round is a significant improvement in the local laboratory performance for histamine analysis. However, the provision of more PT schemes and the increased use of CRMs in the future are still needed by these laboratories for external quality assurance and method validation to enhance the present capability.
  PubDate: 2018-10-09
  DOI: 10.1007/s00769-018-1347-3
Innovative reference material for improving the quality control in the
sucroenergetic sector
- Authors: Maria I. V. Martínez; Rolf Zeisler; Elisabete A. De Nadai Fernandes; Márcio A. Bacchi
  Abstract: Analytical techniques in the sucroenergetic sector can now for the first time be supported by an innovative matrix-matching reference material produced from sugarcane leaves. This will further enhance the validity of the measurement results and contribute significantly to the quality assurance of plant nutrition analysis. The candidate reference material obtained had a low residual moisture and appropriate particle size. Neutron activation analysis was used to determine the mass fraction of Al, Br, Ca, Cl, Ce, Co, Cs, Cu, Fe, Hf, K, La, Mg, Mn, Mo, Na, P, Rb, Sb, Sc, Sm, Sr, Th, V and Zn, and the Kjeldahl method for N. Statistical techniques were applied to evaluate minimum sample mass and within-bottle homogeneity (ANOVA, Tukey test and PCA) and between-bottles homogeneity (ANOVA). It is demonstrated in this paper that the material is homogeneous using 50 mg mass sample for most chemical elements. However, sample masses of 200 mg or greater are required for Co, Na, Sb and V.
  PubDate: 2018-10-03
  DOI: 10.1007/s00769-018-1348-2
Toward the determination of estrogenic compounds in the framework of EU
watch list: validation and implementation of a two-step solid phase
extraction–liquid phase chromatography coupled to tandem mass
spectrometry method
- Authors: Sophie Lardy-Fontan; Véronique Le Diouron; Carine Fallot; Sophie Vaslin-Reimann; Béatrice Lalere
  Abstract: In this paper, development and optimization of a new method for determination of the three hormones (estrone, 17-β-estradiol and 17-α-ethinylestradiol) of the Watch list were described. The validated method relies on isotope dilution—two-step solid phase extraction–liquid phase chromatography mass spectrometry method. The measurement procedure validation has been performed in real matrices, including matrix with high suspended particulate matter and high organic carbon contents, to demonstrate its fitness for purpose. Method performances were in agreement with the requirements of the decision 2015/495/EU (maximal acceptable method detection limit and whole-water analysis). Limits of quantification of the method were of 0.4 ng L−1 for estrone and 17-β-estradiol and 0.1 ng L−1 for 17-α-ethinylestradiol. Expanded uncertainties (k = 2) at limit of quantification were equal to 35 % for estrone and 17-β-estradiol and 50 % for 17-α-ethinylestradiol. The method was successfully implemented to monitor French inland surface waters contamination. The survey reveals a chronic state of contamination by estrone (96 % quantification rate) and significant one by 17-β-estradiol and 17-α-ethinylestradiol (15 % quantification rate). Maximum measured concentrations are above predicted no-effect concentrations, indicating potential risk toward the environment.
  PubDate: 2018-09-26
  DOI: 10.1007/s00769-018-1346-4
Congresses, conferences, workshops and courses
- PubDate: 2018-09-17
  DOI: 10.1007/s00769-018-1345-5
Results of an unannounced proficiency test for the quantification of
hepatitis C virus (HCV) RNA in Shanghai, China
- Authors: Xueliang Wang; Fen Liu; Lingli Jiang; Yun Bao; Yixiao Yang; Yanqun Xiao; Hualiang Wang
  Abstract: Sensitive and accurate hepatitis C virus (HCV) RNA quantification is essential for the management of chronic hepatitis C therapy. Currently, in Shanghai, China, many laboratories offer to quantify the HCV RNA level using various reverse transcription-polymerase chain reaction (rRT-PCR) assays, but the degree of proficiency may vary between them. The objective of this study was to realistically evaluate the performance of clinical laboratories for HCV RNA quantification by a new way of proficiency test program (unannounced inspection). Inactivated chimeric influenza viral particles (CIVP) encapsulating specific RNA sequences of HCV were prepared as positive samples. The sample panel, which consisted of two negative and eight positive samples with different concentrations of CIVP (25 IU/ml to 2.5×106 IU/ml), was distributed to 40 clinical laboratories for HCV RNA quantification. The results reported by the participating laboratories were compared and scored. It was found that 75 % (30/40) of the laboratories obtained an acceptable or better performance score, while the other 10 laboratories had room for improvement. Reported results for individual samples ranged from 125 IU/ml (minimum) to 6.0×104 IU/ml (maximum). The greatest variation was observed for samples with a relatively low concentration. Interlaboratory variability among replicate samples was significantly greater than intralaboratory variability (p < 0.05). Our results demonstrate that there is room for some laboratories to improve their performance in the quantification of HCV RNA in Shanghai. Additionally, this study underlines the importance of unannounced inspection for realistically monitoring the quality of diagnostic laboratories.
  PubDate: 2018-08-28
  DOI: 10.1007/s00769-018-1341-9
Preparation and characterization of in-house reference material for four
organochlorine pesticides in tea matrix
- Authors: Jie Feng; Jingguang Fan; Yansong Zhang; Haipeng Ma
  Abstract: Production and evaluation of in-house reference material for incurred residues of four organochlorine pesticides, named hexachlorobenzene, dicofol, pp′-DDE, and op′-DDT, in tea sample has been performed. Raw materials (tea samples) were confirmed to contain certain levels of incurred organochlorine pesticide residues by a validated gas chromatography–mass spectrometry method. After the materials had been milled and thoroughly mixed, 400 bottles each having 20 g sample were prepared and their homogeneity (within-bottle and bottle-to-bottle variation) was found to be sufficient. The materials demonstrated satisfying stability of four organochlorine pesticides in both short-term (30 days) and long-term (12 months) stability studies. The reference values were characterized using an accurate isotope dilution gas chromatography–mass spectrometry method. The mass fraction (± expanded uncertainty) of hexachlorobenzene, dicofol, pp′-DDE, and op′-DDT in the reference material was (2.1 ± 0.2) mg kg−1, (513.3 ± 31.3) mg kg−1, (8.3 ± 0.6) mg kg−1, and (14.9 ± 1.0) mg kg−1, respectively. The reference materials have been distributed for use in laboratory quality assurance.
  PubDate: 2018-08-25
  DOI: 10.1007/s00769-018-1328-6
Microbiology proficiency testing schemes in wine
- Authors: Caterina Mazzoni; Abdelkader Boubetra; Sandrine Nguyen; Anne Tirard
  Abstract: The number of laboratories performing microbiological analyses of wines has gradually increased in recent years over the world. However, the lack of regular proficiency testing schemes (PTS) in this field is an obstacle for the monitoring of the laboratory performance. The complexity of wine matrix in terms of bacterial ecology and biochemical aspects is a factor to be taken into account in developing a PTS, especially during the preparation of stable and homogeneous samples. Since February 2016, BIPEA set up tests on Brettanomyces analyses in wine, gathering more than 20 laboratories around the world. For each test, the statistical treatment of the data is performed according to ISO 13528. The assigned and tolerance values are calculated from the participants’ data, and the performances of the laboratories are evaluated individually and collectively according to ISO/IEC 17043 and ISO/DIS 22117. The results obtained in these first tests are satisfactory with a progressive improvement of the dispersion of participants’ results over the series. These data confirm that participating in a PTS is particularly important for the laboratories in order to assess and improve analytical performances and to obtain recognition of their analytical procedures by the accreditation bodies according to ISO/IEC 17025.
  PubDate: 2018-08-25
  DOI: 10.1007/s00769-018-1342-8
Proficiency testing in analytical chemistry, microbiology and laboratory
medicine: discussions on current practice and future directions
- Authors: Brian Brookman; Owen Butler; Laura Ciaralli; Monika Horsky; Caroline Laurent; Tracey Noblett; Ulf Örnemark; Marina Patriarca; Lorens P. Sibbesen; Ulla Tiikkainen; Kees van Putten; Piotr Robouch
  Abstract: A summary of the working group discussions on proficiency testing (PT) and external quality assessment (EQA) held at the Eurachem Workshop, Portorož, Slovenia, 9–12 October 2017, is provided. The working groups covered a range of issues concerned with current practice and future directions; the importance of interpretative PT/EQA schemes; changes to PT/EQA schemes in developing countries over the last 10 years; implementing ISO/IEC 17043 for sampling PT/EQA schemes; traditional versus virtual PT/EQA items; experience of the implementation of EA-4/18; and use and treatment of measurement uncertainty in PT/EQA schemes. Delegates from fifty-two countries attended the workshop, and this diversity of different backgrounds was represented on each of the working groups to capture a range of views and experience from a number of different measurement sectors. Working group representatives included PT/EQA providers, participants in PT/EQA schemes, end users of PT/EQA results such as accreditation bodies and regulatory authorities, national measurement institutes, laboratory associations, suppliers, universities and independent consultants from countries around the world.
  PubDate: 2018-08-25
  DOI: 10.1007/s00769-018-1343-7
Ruggedness testing of an analytical method for pesticide residues in
potato
- Authors: Britt Maestroni; Alan R. Vazquez; Valeria Avossa; Peter Goos; Veronica Cesio; Horacio Heinzen; Joerg Riener; Andrew Cannavan
  Abstract: The best demonstration of the ruggedness of a method is monitoring its performance on an ongoing basis as part of the analytical quality control applied in the laboratory. However, an initial demonstration of the ruggedness is often performed as one aspect of the method validation, to give confidence that the method should perform well under normal variations in conditions in routine application. This initial ruggedness testing is typically performed using either multiple replicate analyses or application of design of experiments (DoEs) which minimizes the number of analyses, time and effort required to detect influences on the measurement results. Two DoEs were applied for ruggedness testing for a modified QuEChERS multiresidue method for the detection of pesticide residues in potato by GC–MS/MS. Seven experimental factors were studied using an eight-run Plackett–Burman design replicated three times and an augmented definitive screening design with 34 runs. The relative effectiveness of the two approaches is discussed, in terms of their statistical significance, their cost-effectiveness and the richness of information they provide on the effects of the parameters investigated and the actual robustness of the method being tested.
  PubDate: 2018-08-24
  DOI: 10.1007/s00769-018-1335-7
Acquisition of stability data for pesticides in water sample through
proficiency tests
- Authors: Eric Ziegler; Anne Tirard; Abdelkader Boubetra; Marie de Bort
  Abstract: In the framework of a proficiency test for multiresidue determination, three water samples, coming from the same batch, were sent to each of the 25 participants. They were asked to analyze the first one 2 days after the production (D + 2), the second one at D + 4 and the last one at D + 9. D + 2 was selected as the first date of analysis in order to allow all the participants to receive their samples. Prior to the analysis, the samples were stored at 4 °C. The samples were distributed in 1-l bottle from a batch spiked with more than 100 pesticides. The spiking concentrations ranged from 120 ng/l to 227 ng/l. Apart from the usual proficiency evaluation with assigned values and z-scores, comparisons between the results at the different dates of analysis were made. Most of the substances were found to be stable during the considered period in the conditions of the test, but some profiles of evolution were highlighted for some others.
  PubDate: 2018-08-16
  DOI: 10.1007/s00769-018-1339-3
Application of post-column reaction GC for accurate and direct
determination of musty odor substances in standard solution
- Authors: Yuko Kitamaki; Naoki Saito; Masahiko Numata; Toshihide Ihara
  Abstract: By using post-column reaction GC, a method for accurate and direct characterization of musty odor substances (2-methylisoborneol and geosmin) in a candidate standard solution has been developed. Because the GC system gives a response depending on the number of carbon atoms constituting the organic compound by combustion and conversion to methane, naphthalene and diethyl phthalate, purity of which had been accurately assessed, were used as reference materials for calibration. To verify the method, concentrations of 2-methylisoborneol and geosmin in the sample determined by the method were compared with the concentrations calculated based on gravimetric mixing that is one of the general methods for the characterization of the organic standard solutions. The analytical results of each analyte obtained by the two methods agreed within a deviation of about 0.5 % or less.
  PubDate: 2018-08-06
  DOI: 10.1007/s00769-018-1338-4
Congresses, conferences, workshops and courses
- PubDate: 2018-07-24
  DOI: 10.1007/s00769-018-1340-x
Validation of an in-house measurement procedure for determination of
selected priority hazardous substances in water and estimation of
measurement uncertainty
- Authors: Marijana Kragulj Isakovski; Jelena Molnar Jazić; Snežana Maletić; Aleksandra Tubić; Jasmina Agbaba; Jelena Tričković; Božo Dalmacija
  Abstract: This study investigates measurement procedure validation for the determination of hexachlorobenzene, pentachlorobenzene and trifluralin as priority hazardous pesticides in water with suspended solids < 12 mg/L by liquid–liquid extraction with hexane and gas chromatography with electron capture detector analysis. Two water matrices were used: synthetic matrix and a natural matrix—Danube surface water. Limit of detection was in the range 2.2 ng/L–3.9 ng/L. Trueness expressed as recovery was determined at pesticide concentrations of 20 ng/L and 50 ng/L in both water matrices. The intermediate precision was determined as relative standard deviations (RSD) and represents an agreement between replicates. Trueness was 72 %–121 % with RSD < 20 %. Expanded uncertainty of measurement was similar for all compounds (33.3 %–37.5 %) with a 95 % confidence level, for coverage factor k = 2. The validity of the measurement procedure was confirmed by participation in a PT Scheme with satisfactory z -score smaller than 2. Based on these results, it can be concluded that this low-cost measurement procedure is fit for the intended use measurements.
  PubDate: 2018-07-07
  DOI: 10.1007/s00769-018-1334-8
A fitness for purpose approach to validation and verification of
analytical measurements
- Authors: M. Alvarez-Prieto; J. Jiménez-Chacón
  Abstract: Validation (and in some extension verification) are concepts often applied to analytical procedures (or methods). The new edition of ISO/IEC 17025 clearly distinguishes between them. However, the established practice in analytical chemistry is not in harmony with the definitions given in the International Vocabulary of Metrology. It is stressed that both concepts should be applied to the analytical process (i.e., the measurement) instead of to the written analytical procedure (or method). Formal new definitions of basic and complementary metrological characteristics are given in order to properly understand the concepts of metrological requirements (MRs), verification and validation, and how they should be applied in practice. Also, validation is conceptually linked to the intended use of results, that is, to make the correct decision with a given high probability. To understand the rationale behind these concepts, a logical flow diagram is discussed. The way to compare basic metrological characteristics and the previously obtained ones for verification, as well as how to compare them with MRs for validation is discussed. Conversion of product characteristics into MRs plays an important role in this latter case. Some general guidelines on extension (and depth) of verification and validation are offered. Some of the discussed ideas could be applied in other branches of metrology.
  PubDate: 2018-07-03
  DOI: 10.1007/s00769-018-1331-y
Influence of probability distribution in measurement uncertainty of
plane-strain fracture toughness test
- Authors: Daniel Antonio Kapper Fabricio; Carla Schwengber ten Caten; Lisiane Trevisan; Afonso Reguly
  Abstract: The evaluation of measurement uncertainty by testing laboratories has a direct impact on the interpretation of the results. In several cases, it is recommended to determine the measurement uncertainty by the Monte Carlo method (MCM), which considers the propagation of distributions rather than the propagation of uncertainty. Measurement uncertainty of plane-strain fracture toughness KIC test was evaluated through the MCM and an examination of the influence of the probability distribution on the uncertainty values was performed through analysis of variance (ANOVA). In addition, results were compared to those obtained by the Guide to the Expression of Uncertainty in Measurement (GUM). Results demonstrate the importance of using the Monte Carlo method for the evaluation of measurement uncertainty and confirm that the probability distribution of input data has a significant influence on the expanded uncertainty values obtained for the plane-strain fracture toughness test.
  PubDate: 2018-07-02
  DOI: 10.1007/s00769-018-1326-8
Characterisation of folic acid by mass balance versus quantitative NMR
- Authors: Andrea Lodi; Cees-Jan Nap; Silvia Metzger-Maurer; Christelle Schwartzenberger
  Abstract: Two approaches were used to determine the mass fraction of a sample of folic acid, one indirect (mass balance) where the components other than folic acid were measured, and one direct, using quantitative nuclear magnetic resonance (qNMR). The procedures used for the mass balance were essentially those described in the European Pharmacopoeia monograph for folic acid. qNMR is a technique for quantifying the main component within an organic compound (Quantitative NMR (qNMR)—BIPM in https://www.bipm.org/en/bipm/chemistry/organic-analysis/qnmr/, Santosh and Raja in Trends Anal Chem 35:5–26, 2012), whereas mass balance quantifies its minor components. The results obtained with the two approaches are independent. In this study, their joint application generated information that was used in a more than complementary fashion. The mass balance characterisation, in particular the results obtained by liquid chromatography with ultraviolet detection (LC–UV), allowed to improve the accuracy of the qNMR result by subtracting the interfering contribution of a related structure impurity. On the other hand, qNMR enabled concluding that the non-uniform response of UV detection at a single wavelength was not critically biasing the LC–UV results. In the end, the mass fractions obtained by mass balance and qNMR were not that different. It is concluded that mass balance and qNMR may be not only complementary but also synergistic. It was also observed that access to monographs of the European Pharmacopoeia, when available, gives skilled analysts an important tool for improved substance characterisation.
  PubDate: 2018-06-28
  DOI: 10.1007/s00769-018-1327-7
Correction to: Motivations, benefits and challenges on ISO/IEC 17025
accreditation of higher education institution laboratories
- Authors: Inês Hexsel Grochau; Carla Schwengber ten Caten; Maria Madalena de Camargo Forte
  Abstract: Unfortunately, figure 3 was incorrectly published in the original publication and the correct version is updated here.
  PubDate: 2018-06-18
  DOI: 10.1007/s00769-018-1333-9