Doboku Gakkai Ronbunshu

This study aims to present new scientific methods to assess the extent of universities’ commitment to the international standard and to assess the quality level of university units according to the International Quality Management Standard 2015, in addition to applying the current internal audit. These scientific methods included calculating the arithmetic mean and standard deviation and drawing a control panel to determine the extent of commitment to the specification at the beginning and after qualification. Statistical values were calculated, including the arithmetic mean and standard deviation for each paragraph of the international specification after analyzing the questionnaire responses from volunteer students and professors. These forms included two models: the first of which included all paragraphs of the specification and the second was written differently to determine the accuracy and seriousness of the participants in the questionnaire. The standard deviation was 0.0 in most paragraphs of the specification, which means there was no dispersion in the selection of participants, indicating the success of the qualification process and increased awareness and interest in applying the specification among all concerned parties. The degree of importance of these paragraphs reached 5, and this was confirmed by aligning the upper and lower control lines with the average line, which is consistent with the internal audit reports, this proves the accuracy and credibility of this method in the evaluation process.

This study assesses the compliance of a university research laboratory with the ISO/IEC 17025: 2017 standard, focusing on ensuring technical competence and the integrity of analytical results. An analytical approach was employed using a standard checklist to identify gaps and establish a corrective action plan. The evaluation revealed significant deficiencies in the laboratory's structural, resource, and process requirements, resulting in an overall satisfaction rate of only 15%. This percentage reflects the proportion of conformity criteria met by the laboratory in relation to the standard’s requirements. These findings underscore the critical need for improvements in the laboratory’s quality management system to enhance the reliability and credibility of its research outputs. The study also emphasizes the importance of implementing robust quality control measures and continuous staff training to meet international standards, thus positioning the laboratory to achieve full ISO/IEC 17025 compliance in the future.

The risk management approach has become crucial in quality management systems, to the extent that its importance has been reflected in the new version of ISO/IEC 17025:2017. In 2014, the Brazilian Federal Police’s Forensic Genetics Expertise Service (SEPGEF/PF) implemented a quality management system based on NBR ISO/IEC 17025:2005. This article outlines the initial steps taken to embed a risk management culture within the laboratory to align it with the new NBR ISO/IEC 17025:2017 version. The main focus was to analyze SEPGEF’s nonconformity records between august 2014 and april 2024 and, based on this, to develop methods for mapping, assessing and treating the risks associated with these events. Additionally, the main risks that threaten the integrity of DNA samples were discussed. We also presented future prospects for the unit in order to promote more effective management of the risks that affect its objectives.

The goal of the recent study was to establish a simple, precise, reliable, accurate, cost-effective, and stable RP-HPLC method with quality-by-design approach for estimating the amount of articaine in bulk and nanostructured lipid carriers which were developed in house. A fractional factorial design with four factors and eight runs was employed for the initial screening studies. Further optimization of mobile phase ratio and flow rate were conducted using a central composite design. The chromatographic method with reversed-phase chromatographic separation, C-18 column, mobile phase in a mixture of potassium dihydrogen phosphate (KH2PO4) and acetonitrile in an 80:20 (% v/v) with a flow rate of 0.8 mL/min and detection wavelength of 273 nm having retention time of 2.876 was developed. The newly developed method was validated as per the guidelines given by International Council for Harmonisation ICH Q2 (R1) which revealed linearity between 10 to 50 µg/mL with r2 = 0.995. The % RSD for intra-day precision ranged from 0.2089 to 0.5298, while for inter-day precision, it ranged from 0.1973 to 0.3899. The robustness values were less than 2 %. The percent drug recovered for NLCs was 99.12 %. Further, the limits of detection and quantification (LOQ) were determined to be 2.32 µg/mL and 4.12 µg/mL, respectively. The studies showed that the new approach is simple, selective, rapid, and reproducible for the assessment of pure drug and nanostructured lipid carriers-based formulations.

The principal objective of this study is to examine the oil and grease (OG) content in surface soil samples using Fourier transform infrared (FT-IR) spectroscopy. The standard solution is a mixture of isooctane and octanoic acid (1:1 by weight) in tetrachloroethylene. The linear working range was established to be between 25 and 350 ppm. The limit of detection (LOD) was determined to be 2.36 ppm, while the limit of quantification (LOQ) was calculated to be 7.87 ppm. The mean recovery value of OG exhibited a range of 82.75% to 93.75% in surface soil samples. To assess the precision and accuracy of the method, standard addition experiments were conducted by spiking the isooctane and octanoic acid mixture, and the resulting spiked samples were analyzed in triplicate. After the completion of the validation studies, the concentrations of OG were determined in surface soil samples collected from regions hypothesized to have varying levels of pollution accumulation. These sampling sites included recreational areas, urban areas, rural areas, locations adjacent to gas stations, and areas near industrial sites. The determined OG concentrations are 15.9 ± 4.57, 6.9 ± 2.02, 2.4 ± 0.93, 14.9 ± 1.71, and 10.1 ± 1.16 µg/g dry weight (dw), respectively. Due to possible barbecue activities and other anthropogenic effects, the highest concentration of oil and grease was observed in the sample of the recreational area. The second highest concentration was found in gas station samples, likely due to heavy traffic and the gas station itself, while the lowest concentration was observed in the rural area, as expected due to the lack of potential pollution sources next to the sampling site. These findings indicate potential environmental risks in areas with high human activity and traffic, highlighting the need for remediation efforts. Also, the method of OG determination using infrared spectroscopy offers a more expedient, cost-effective, and environmentally friendly approach for the analysis of soil samples, particularly due to the minimal use of chemicals. Also, the method of oil and grease determination using infrared spectroscopy offers a more expedient, cost-effective, and environmentally friendly approach for the analysis of soil samples, particularly due to the minimal use of chemicals.

This paper describes the systematic development of green and sustainable HPLC method for quantification of antidiabetic drugs teneligliptin hydrobromide hydrate, metformin hydrochloride and pioglitazone HCl in tablet formulation using Box–Behnken design. Box–Behnken design was used to know the influence of identified critical method parameters, volume of acetonitrile, flow rate and column temperature on the retention time of all three drugs and resolution between two drugs. Statistical analysis by Analysis of variance was computed to understand the potential interactions among critical method parameters. Further mathematical model was validated by using statistical and graphical optimization to define the design space. From the three parameters under investigation the study revealed that the response was more influenced by slight change in volume of acetonitrile, demanding its strict control. A mixture of KH2PO4 phosphate buffer (20 mM): acetonitrile: methanol (40:30:30%v/v) was employed as the mobile phase for chromatographic separation using octadecyl silyl column (250 × 4.6 mm, 5 µm). Detection was performed at 236 nm and 0.86 ml/min was set as the flow rate of mobile phase. The linearity was observed in the range of 12–28 µg/ml for Teneligliptin hydrobromide hydrate, 300–700 µg/ml for Metformin hydrochloride and 9–21 µg/ml for Pioglitazone hydrochloride as shown by r2 ≥ 0.99 for all three drugs. Retention time of Teneligliptin hydrobromide hydrate, Metformin hydrochloride and Pioglitazone hydrochloride was 4.09, 3.01 and 11.44 min, respectively. The % relative standard deviation for accuracy, precision and robustness were all within the specification, less than 2, which indicates that method was validated properly as per guideline. The studies successfully demonstrate the application of Box–Behnken design in the development of accurate and sensitive liquid chromatographic technique with enhanced method performance. Furthermore, greenness of the analytical method was assessed using 12 principles of green analytical chemistry by AGREE, complex GAPI and Analytical eco-scale tool, indicating that the developed method was ecofriendly.

Records of elite athletes’ steroid profiles are maintained by the World Anti-Doping Agency (WADA) to facilitate detection of doping with endogenous steroids. As the steroid measurements comprising these profiles are obtained in a variety of laboratories throughout an athlete’s career. It is critical to ensure their metrological traceability to a fixed reference, which permits meaningful identification of any changes. Certified reference materials (CRMs) are an important tool to ensure the comparability of measurement results. The National Measurement Institute, Australia, has prepared a freeze-dried urine CRM, NMIA MX017, with property values for the mass fractions and mass concentrations of the six steroids specified by WADA as markers for the urinary steroid profile. Its reference values are traceable to the units (kg and m) of the international system of units (SI), and it is now available to be used by WADA-accredited laboratories as a replacement for a previous, exhausted CRM. The certification of NMIA MX017 was performed using a high accuracy reference method developed specifically for this material. A two-dimensional clean-up of the urine matrix by high-performance liquid chromatography provided interference-free quantification of the analytes and their deuterium-labelled analogues by gas chromatography with tandem mass spectrometry. Confirmatory analysis by gas chromatography with high-resolution mass spectrometry was used to verify the absence of bias due to potential influences by matrix coextractives or contaminants. The characterisation of NMIA MX017 and the approach used to obtain a rigorous estimate of the measurement uncertainty of the property values of the CRM are described.

Abstract Veterinary diagnostic laboratories (VDLs) play a critical role in screening both human and animal samples for SARS-CoV-2. To evaluate the SARS-CoV-2 detection methods used by VDLs, a proficiency test was performed by the US Food and Drug Administration’s Veterinary Laboratory and Investigation and Response Network in collaboration with two other organizations. Thirty-two sets of 12 blind-coded samples were prepared by fortifying Molecular Transport Medium (MTM) or feline feces with SARS-CoV-2 Omicron variant or non-SARS-CoV-2 equine coronavirus RNA at various concentrations and shipped to 32 participants for blinded (unbiased) analysis. Results were analyzed according to the principles of International Organization for Standardization 16140-2:2016 using two approaches such as establishing the rate of detection (ROD) and the success rate by applying the analysis of binary outcome by logit approach. ROD provided the overall assessment of laboratories performance, whereas the novel logit approach provided an insight to more specific analysis based on the complexity of each sample. The ROD was 83% and 98% for MTM samples at 200 and 20000 genome copies per 100 µL, respectively. Fecal samples were classified as challenging exploratory, and results were not included in the assessment of performance but discussion purposes only. Fecal samples exhibited matrix interference impacting the performance. The ROD was 44% and 89% for fecal samples at 2000 and 20000 genome copies per 100 µL, respectively. The non-COVID coronavirus RNA, which was used to address the specificity, did not interfere with methods used. Establishing the success rate by evaluating the qualitative results (detected/not detected) applying a logit approach revealed that, out of thirty-two participants, twenty-eight had satisfactory results, one participant had unsatisfactory results, and three participants had questionable results for MTM samples. For fecal samples, three participants out of thirty-two did not meet the expectations at higher concentrations. Lower concentrations of fecal samples were excluded from this analysis. Again, the fecal samples were considered as challenge samples and the results were provided to assist participants in their continuous efforts to improve their performance and not to evaluate their performance.

During the period 2021–2023, the Italian National Institute of Health (ISS) organised, in collaboration with the Italian Health Ministry, proficiency testing (PTs) for about 22 Italian and other EU laboratories involved in the monitoring programmes for Plant Protection Products (PPPs). The aim of the PTs was to determine the amount of active ingredient in various formulations of PPPs. Overall, the type of formulations to be analysed were soluble concentrate (SL), suspension concentrate (SC), capsule suspension (CS), emulsion water oil (EW), soluble water granule (SG), dustable powder (DP), water dispersible granule (WDG) and emulsion concentrate (EC). In 2021, the ISS organised PTs for the determination of Imazamox, Fenhexamid and Trinexapac-ethyl in three different PPPs as soluble concentrate (SL), suspension concentrate (SC), and capsule suspension (CS), respectively. In 2022, PTs for the determination of Bentazone, Spinosad and Tau-Fluvalinate were organised. For this PTs, commercial PPPs were obtained from the Italian market as SC, emulsion oil water (EW) and soluble water granule (SG). In 2023, the PT was organised to determine the active ingredient Trifloxystrobin, Deltamethrin and Cyprodinil in the commercial product as water dispersible granule (WDG), dustable powder (DP) and emulsion concentrate (EC), respectively. Homogeneity and stability, performed for all PT samples, fulfilled the acceptability criteria. The Jarque–Bera test was used to verify the hypothesis of normality of the data distributions before to calculate the z-score values. Laboratory performances, expressed in terms of z-scores, were satisfactory for almost all participants for all substances.

Valproic acid (VPA) is widely used for the treatment of epilepsy, bipolar disorder and other psychiatric diseases. Because of its narrow therapeutic window, monitoring the concentrations of VPA in patient’s serum is essential. In this paper, an isotope dilution-liquid chromatography-tandem mass spectrometry-(ID-HPLC–MS/MS) based candidate reference measurement procedure (RMP) for the quantification of VPA in human serum was established. After Samples pre-prepared by a simple protein precipitation method, the basic analytical performances of the candidate RMP was validated, including specificity, matrix effect, linearity, limit of quantitation (LOQ) and limit of detection (LOD), intra-and inter-batch precision, recovery rate, carryover, and stability. In order to make the measurement results of VPA traceable, we took all components that affect the accuracy of VPA measurement results into account to evaluate the corresponding uncertainties according to the GUM, including measurement imprecision, the purity of VPA standard, uncertainties caused by weighing during the preparation of calibrators and samples, matrix effect, recovery rate, carryover and sample stability. The candidate RMP separated VPA from potentially interferents in human serum and enabled measurement over a calibrated linear range from 2.60 to 203.57 μg/mL with a good correlation coefficient of 0.9995, and no significant matrix effects were observed. The intra-day and inter-day coefficients of variation (CV%) were 0.30–1.64% and 0.67–1.39%, respectively. The average recovery rates were between 94.55% and 96.93%. The LOD and LOQ were 0.23 μg/mL and 2.10 μg/mL, respectively. The expanded measurement uncertainties were 3.19% (k = 2) at 9.45 μg/mL, 3.14% (k = 2) at 48.86 μg/mL, and 2.95% (k = 2) at 97.23 μg/mL (k = 2), respectively.

AbstractThe procedures used to assign values to certified reference gas mixtures and to evaluate their associated uncertainties, which are described in ISO 6143, and that were variously improved by Guenther and Possolo (Anal Bioanal Chem 399:489–500, 2011. 10.1007/s00216-010-4379-z), are further enhanced by the following developments: (i) evaluating and propagating uncertainty contributions derived from comparisons with historical reference gas mixtures of similar nominal composition; (ii) recognizing and quantifying mutual inconsistency (dark uncertainty) between primary standard gas mixtures used for calibration; (iii) employing Bayesian procedures for calibration, value assignment, and uncertainty evaluations; and (iv) employing state-of-the-art methods of meta-analysis to combine cylinder-specific measurement results. These developments are illustrated in examples of certification of two gas mixture Standard Reference Materials developed by the National Institute of Standards and Technology (NIST, USA). These examples serve only to demonstrate the methods described in this contribution and do not replace any official measurement results delivered in the certificates of any reference materials developed by NIST.

The present paper outlines a joint proficiency testing (PT) programme established between the Asia–Pacific Metrology Programme (APMP) and the Asia Pacific Accreditation Cooperation (APAC). This programme aims to assess the analytical performance and enhance measurement proficiencies in laboratories across various economies, with a focus on the quantification of benzoic acid in fish sauce. This PT programme was organised by the Government Laboratory, the designated institute of metrology in chemistry for Hong Kong, China (GLHK). A comprehensive invitation extended to both APMP and non-APAC members resulted in the participation of 41 laboratories from 19 different economies. The metrological reference value for benzoic acid, provided by GLHK, was determined utilizing isotope-dilution mass spectroscopy (IDMS) with traceability to the International System of Units (SI). This SI-traceable reference value enhances the quality of participants’ measurements and promotes the awareness of traceability among the participants, enabling a more accurate evaluation of their results. Concurrently, this approach facilitates the building of measurement capabilities among participants, fostering more robust connections between metrology institutes and testing laboratories. The programme also revealed a notable deficiency in the understanding of statistical concepts among some participants, including the coverage factor, degrees of freedom, standard uncertainty, and expanded uncertainty. Proper interpretation of zeta-scores or En scores based on measurement uncertainties, when analysed alongside z-scores, proves to be indispensable for an accurate assessment of the participants’ measurement competencies and their ability to evaluate measurement uncertainty. The assessment of participants’ performances, taking into account measurement uncertainties, serves as a benchmark for participants to gauge the validity of their measurement uncertainty evaluations.

Sometimes, analytical laboratories receive requests with a small number of determinations and/or samples or outside the typical scope of analytical services. As a result, they may not have historical data on the performance of the required analytical procedures and/or appropriate reference materials. Under these conditions, it is difficult or uneconomical to use traditional quality control charts. This is the so-called start-up problem of these charts. Quesenberry’s Q charts are appropriate in these situations because they do not require a prior training phase. In the first part of this series of publications, the fundamentals and the algebraic expressions of the Q charts were presented for the individual measurements for the mean (four cases) and for the variance (two cases). This experimental study was carried out with data from quality control of mass fractions of Co in a serpentinite CRM and SiO2 in a laterite CRM, by ICP-OES. The performance of Q charts is discussed in two situations: when the analytical process showed a clear systematic error from the beginning and when small shifts in mean and variance occurred simultaneously. In the first situation, performances of Q charts for the mean depended on the case: two of them were very sensitive even in the short run and the other two were insensitive and useless. In the second situation, the Q charts showed delayed alarms, but with a comparable behavior to the chart for individual measurements and the moving range of two. EWMA charts associated to Q charts were an excellent complement.