Interlaboratory Test Research Articles

Validation of a small-scale method for determination of phosphorus in meat and meat products by molecular absorption spectroscopy

The purpose of this study was to evaluate the applicability of an alternative analytical technique to the reference method for phosphorus detection in meat and meat products established by ISO 2294:1974, revised by ISO 23776:2021. When an analytical method is modified or a new one is developed and implemented, it should be validated before being accepted for routine determinations. Furthermore, it is necessary to demonstrate that the new or alternative method has good performance characteristics in comparison with the reference method. Therefore, a comparison of the performance of the alternative and the reference method should be made. In the present study, a statistical evaluation of the calibration model of the alternative method was made with data from interlaboratory studies made in five consecutive years using fifty analyses of meat and meat products. The statistical parameters evaluated over time for the calibration curve were the y-intercept and slope; correlation and linearity; analytical limits: detection and quantification; working range; and accuracy (precision and trueness). In the interlaboratory tests, the results obtained by the alternative analytical method were compared with those obtained by the reference method, and their performance in these tests was also evaluated. The results obtained by the alternative method indicated better accuracy than the reference method due to lower relative errors, more precision, and a good trueness evaluation through lower absolute values of the z-score. The study demonstrated that the phosphorus alternative method is applicable for the determination of total phosphorus in the matrix of meat and meat products.

Міжлабораторні порівняльні випробування як спосіб оцінки технічної компетентності вимірювальних лабораторій

The article substantiates the necessity of participation of measuring laboratories of coke and coal industry enterprises in interlaboratory comparative tests. It is shown that the decisive factor in the accreditation or certification of testing laboratories is the reliability of the results. Thus, the regulatory documents governing the general requirements for the competence of laboratories specify a number of measures to ensure the quality of the results obtained. Among them, participation in inter-laboratory comparative tests (ILCT) is recognised as the most objective way to verify the reliability of the results obtained in a laboratory. The article defines the ILCT and explains the responsibilities of organisations entitled to conduct them. The data on the experience of the Testing Centre ‘Khartsis’ of SE ‘UKHIN’, approved by the NATIONAL ACCREDITATION AGENCY OF UKRAINE as a provider of verification of the professional level of laboratories in the field of testing lignite, hard coal, anthracite, products of their processing and blast furnace coke, foundry coke, coal coke, coke nuts, coke fines, are presented. In particular, the article analyses the results of four rounds of the Interlaboratory Comparison Programme for the Measurement of Coal and Coke Quality Indicators, implemented by the SE ‘UKHIN’ in 2023, in which measuring laboratories of coke and chemical enterprises, concentrating plants, mines, thermal power plants and other enterprises of various forms of ownership and departmental subordination participated. Using the example of actual results obtained, it is shown that constant participation in the Programme is an effective means of controlling the quality and reliability of the results issued by the laboratory, as it allows timely identification and elimination of the causes of poor quality measurements. Keywords: coal, coke, quality indicators, measuring laboratory, comparative interlaboratory tests, Programme, provider, control sample, round, certification, accreditation. Corresponding author: O.B. Sosnova, e- mail: lenas61.61@gmail.com

Controlling sensory analysis results: tools and importance in assessor selection. Case study: PROVA-ALABE proficiency test

The PROVA-ALABE essay aims to characterize the olfactory, tactile and taste changes underlying the sensory evaluation of wines. It allows assessors to understand the extent to which their perception of a wine is harmonized with that of the other assessors in the trial, contributing to their qualification, as well as the corresponding panel, in detecting and recognizing the most prevalent defects in wines. This work aimed to provide a critical summary of outcomes achieved through interlaboratory tests to identify a primary defect in deliberately contaminated wines. Over three years, interlaboratory tests were performed, corresponding to 60 wines mainly altered with a specific compound. These tests aimed to identify different defects, such as mould, lactic, acescent, reduced, oxidized, vegetable, animal, acidic, bitter, astringency, and others (plastic, sulphur dioxide, bitter almond). However, wine's complexity introduces factors that can affect assessors' perception, with the same defect being perceived differently based on the panel's experience, training, and cultural backgrounds, which can be problematic for an objective analysis. Results of rejection rates and assessor identification percentages suggest that oxidation, mould, and animal defects are more easily recognized. Participation in interlaboratory tests is mandatory for accredited laboratories, serving as an interesting tool for demonstrating results consistency across sensory laboratories. Additionally, such participation can provide valuable information about assessors' performance.

Standardization of an antimicrobial resistance surveillance network through data management.

The rapid spread of COVID-19 worldwide within 2 months demonstrated the vulnerability of the world's population to infectious diseases. In 2015, the Global Antimicrobial Resistance and Use Surveillance System (GLASS) was launched to combat antimicrobial resistance (AMR). However, there has been no comprehensive assessment of the decade-long global battle against AMR based on GLASS data. South Korea established Kor-GLASS (Korean-GLASS) to proactively monitor data quality and enable international collaborations. A unique feature of Kor-GLASS is the quality control center (QCC), which uses network hubs and ensures standardized, high-quality data through interlaboratory proficiency testing (IPT) and external quality assessment (EQA). In addition, the QCC multifaceted endeavors for integrated data quality management. Since 2020, high-quality AMR data have indicated fluctuating antibiotic resistance rates in South Korea. This trend does not align with the decrease in antibiotic usage seen in humans but coincides with non-human antibiotic sales, indicating a need for greater monitoring of non-human antibiotic resistance. Comprehensive and robust management taking account of the intricate interplay among humans, animals, and the environment is essential. Kor-GLASS has been expanded into a "One Health" multiagency collaborative initiative. Although a standardized solution is not suitable for all countries, it must align with the local context and international standards. A centralized top-down management structure such as that of the QCC is essential to ensure continuous data quality coordination. Sustained efforts and surveillance systems are crucial for monitoring and managing AMR and safeguarding human health.

Determination of Trace Perchlorate in Soil using Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS)

The international standard (IS) currently used for determining perchlorate in soil is not applicable to trace perchlorate. We developed a quantitative analysis method using liquid chromatography–tandem mass spectrometry (LC-MS/MS) for the trace perchlorate in soil. The perchlorate was extracted from air-dried soil (<150 μm) with distilled water. We proposed the optimum extraction method that included mechanical shaking followed by centrifugation. An internal standard material (Cl18O4-) was added to the extracts and standard solutions at concentration of 5 μg L-1. The samples were analyzed by LC-MS/MS equipped with a reversed phase C18 column packed with core-shell particles containing trimethylsilane functional groups. Samples that may be interfered with organic matter present in the soil should be purified with a C18 cartridge. The method detection limit and limit of quantitation for our method was 1.31 and 4.36 μg/kg, respectively. We verified the proposed method through interlaboratory comparison test; both coefficients of variation for repeatability (CVr) and reproducibility (CVR) were less than 5%. Therefore, we concluded that the proposed method may be used for precise quantitative analysis of trace amounts of perchlorate in soil.

Collaborative cytometric inter-laboratory ring test for probiotics quantification.

Probiotics are live microorganisms that, when administered in adequate amounts, confer a health benefit on the host. From this definition, accurate enumeration of probiotic products is a necessity. Nonetheless, this definition does not specify the methods for assessing such viability. Colony forming units is the de facto gold standard for enumerating viable in probiotic products. The notion of microbial viability has been anchored in the concept of cultivability, which refers to a cell's capacity to replicate and form colonies on agar media. However, there is a growing consensus that the term "viability" should not be exclusively tied to the ability to cultivate cells. For example, bacterial cells can exist in a Viable But Non-Culturable (VBNC) state, characterized by the maintenance of characteristics such as membrane integrity, enzymatic activity, pH gradients, and elevated levels of rRNA, despite losing the ability to form colonies. Herein we present the results of a collaborative inter-laboratory ring test for cytometric bacterial quantification. Specifically, membrane integrity fluorescence flow cytometry (FFC) method and the newer impedance flow cytometry (IFC) method have been used. Both methods interrogate single cells in solution for the presence of intact membranes. FFC exploits fluorochromes that reflect the presence or absence of an intact membrane. IFC probes membrane integrity in a label-free approach by detecting membrane-induced hindrances to the propagation of electricity. A performance ring-test and comparison design on the FFC method showed that the method is robust against the exchange of equipment, procedures, materials, and operators. After initial method optimization with assessments of rehydration medium, wake-up duration, and phase shift gating on the individual strains, the IFC method showed good agreement with the FFC results. Specifically, we tested 6 distinct species of probiotic bacteria (3 Lactobacillus and 3 Bifidobacterium strains) finding good agreement between FFC and IFC results in terms of total and live cells. Together, these results demonstrate that flow cytometry is a reliable, precise, and user-friendly culture-independent method for bacterial enumeration.

European Inter-Laboratory Proficiency Test for Dourine Antibody Detection Using the Complement Fixation Test.

Dourine is a sexually transmitted parasitic disease affecting equids. Its causative agent is referred to as Trypanosoma equiperdum and the prescribed serodiagnosis method is the complement fixation test (CFT). In the context of our European Reference Laboratory mandate for equine diseases (excluding African horse sickness), we organised dourine CFT inter-laboratory proficiency tests (ILPTs) in 2015, 2018 and 2022 to evaluate the performance of the European Union network of National Reference Laboratories (NRLs) for dourine. ILPT panels were composed of horse sera with or without antibodies against Trypanosoma spp. originating from non-infected, immunised or experimentally infected horses. Twenty-two NRLs participated in at least one of the three sessions. In 2015, 2018 and 2022, the percentage of laboratories obtaining 100% of the expected results was 57, 90 and 80, respectively. These dourine CFT ILPTs showed the benefits of standardising the method's detection limit and underlined the constant need to evaluate NRLs to improve the network's performance. These results also argue in favour of the need for a representative bio-bank to improve the representativeness of ILPT samples and to allow the adoption of alternative serological methods for international surveillance of dourine.

The effect of the volume of tests and the number of participants on the assessment of qualification in interlaboratory comparison tests

The results of a comparative analysis of statistical indicators for assessing the proficiency determined during interlaboratory comparison tests (ICT) are presented. The main statistical indicators were selected: the assigned value, standard deviation for assessment the proficiency and standard uncertainty of the assigned value. Statistical indicators were determined in accordance with Algorithm A, GOST R 50779.60. Comparison of the indicators was carried out on the basis of numerical experiment data (random number generation) for the ultimate tensile strength of a D16AT aluminum alloy depending on the number of samples and the number of participants in the ICT qualification program. The calculation and subsequent statistical analysis of the proficiency test scores was based on the values generated by the software. Random number generation is performed for a characteristic that has a normal distribution law with the parameters of the mean equal to 450 MPa and standard deviation equal to 5 MPa. The values of the normal distribution parameters chosen as an example corresponded to the average level of tensile strength values of standard specimens made of D16AT aluminum alloy sheets. The numerical experiment (generation of random values) was carried out for given cases of the number of participants and the number of proficiency testing samples (PTS) independently of each other using separate samples of the appropriate size. A total of 36,000 ultimate tensile strength values were generated for the proficiency testing samples made of D16AT aluminum alloy sheets. As a result of calculations, 48 average values were determined (according to the number of considered implementations of ICT programs, depending on the number of participants and the proficiency testing samples) for each selected statistical indicator of the ICT qualification program. The average value of each statistical indicator was determined on samples with a bulk of 250 to 2000 generated (experimental) values, depending on the number of participants and the number of proficiency testing samples. The analysis thus performed made it possible to evaluate the influence of the volume of tests and the number of participants on the assessment of the proficiency in interlaboratory comparative tests. It is shown that for the selected range of the number of ICT participants (from 5 to 20) and the number of PTS (from 5 to 10), the value of the assigned xpt value does not depend either on the number of tested PTS or the number of ICT participants. The maximum discrepancy between the assigned value and the given level of tensile strength (450 MPa) is 0.13%, which falls within the error (rounding) for this level of values and cannot lead to significant errors in proficiency testing during ICT. The standard deviation for the qualification assessment, regardless of the number of participants, decreases with an increase in the number of proficiency testing samples, but such a decrease is insignificant and does not exceed the standard deviation (SD) value of the ultimate tensile strength (for the selected model for generating experimental values, the SD value is accepted to be 5 MPa). In contrast to the assigned value and the standard deviation for the qualification assessment, it is shown that the standard uncertainty of the assigned value for the ultimate tensile strength of standard samples made of D16AT aluminum alloy sheets depends on the number of participants and the number of proficiency testing samples tested by each participant and decreases with an increase in the number of participants in ICT programs and the number of proficiency testing samples.

Intra- and interlaboratory reproducibility of the RIATOL qPCR HPV genotyping assay.

The implementation of cervical screening based on human papillomavirus (HPV) continues to progress rapidly across countries. Evidence has shown that assays detecting high-risk human papillomavirus (hrHPV) deoxyribonucleic acid (DNA) are more effective than cytology-based screening. Validation of new hrHPV DNA assays requires both noninferior clinical accuracy compared to a standard comparator for cervical precancer and good reproducibility. This study builds upon previous diagnostic accuracy assessments of the RIATOL HPV genotyping qPCR assay and aims to evaluate the international validation criteria for reproducibility. The intra- and interreproducibility of the RIATOL-qPCR assay were assessed using 550 remnant cervical cell material from the cytology archive of the National Reference Center for HPV in Belgium. Specimens were collected in the context of cervical cancer screening and tested in two different laboratories. The international reproducibility criteria include the lower bound of 95% confidence interval of the intra- and interlaboratory agreement regarding the detection of hrHPV DNA exceeding 87% with kappa ≥0.50. The RIATOL-qPCR assay demonstrated excellent intralaboratory reproducibility, achieving an overall agreement of 98.2 (95% CI 96.6-99.1%) and a kappa of 0.96. Interlaboratory testing showed an overall agreement of 98.5 (95% CI 97.1-99.4%) with a kappa of 0.97. The RIATOL-qPCR assay fulfills the third criterion for HPV test reproducibility requirement for use in cervical cancer screening.

Interlaboratory comparison using inactivated SARS-CoV-2 variants as a feasible tool for quality control in COVID-19 wastewater monitoring

Wastewater-based SARS-CoV-2 epidemiology (WBE) has proven as an excellent tool to monitor pandemic dynamics supporting individual testing strategies. WBE can also be used as an early warning system for monitoring the emergence of novel pathogens or viral variants. However, for a timely transmission of results, sophisticated sample logistics and analytics performed in decentralized laboratories close to the sampling sites are required. Since multiple decentralized laboratories commonly use custom in-house workflows for sample purification and PCR-analysis, comparative quality control of the analytical procedures is essential to report reliable and comparable results.In this study, we performed an interlaboratory comparison at laboratories specialized for PCR and high-throughput-sequencing (HTS)-based WBE analysis. Frozen reserve samples from low COVID-19 incidence periods were spiked with different inactivated authentic SARS-CoV-2 variants in graduated concentrations and ratios. Samples were sent to the participating laboratories for analysis using laboratory specific methods and the reported viral genome copy numbers and the detection of viral variants were compared with the expected values.All PCR-laboratories reported SARS-CoV-2 genome copy equivalents (GCE) for all spiked samples with a mean intra- and inter-laboratory variability of 19 % and 104 %, respectively, largely reproducing the spike-in scheme. PCR-based genotyping was, in dependence of the underlying PCR-assay performance, able to predict the relative amount of variant specific substitutions even in samples with low spike-in amount. The identification of variants by HTS, however, required >100 copies/ml wastewater and had limited predictive value when analyzing at a genome coverage below 60 %.This interlaboratory test demonstrates that despite highly heterogeneous isolation and analysis procedures, overall SARS-CoV-2 GCE and mutations were determined accurately. Hence, decentralized SARS-CoV-2 wastewater monitoring is feasible to generate comparable analysis results. However, since not all assays detected the correct variant, prior evaluation of PCR and sequencing workflows as well as sustained quality control such as interlaboratory comparisons are mandatory for correct variant detection.

Results of the 2020 Genomic Proficiency Test for the network of European Union Reference Laboratory for Antimicrobial Resistance assessing whole-genome-sequencing capacities.

The global surveillance and outbreak investigation of antimicrobial resistance (AMR) is amidst a paradigm shift from traditional biology to bioinformatics. This is due to developments in whole-genome-sequencing (WGS) technologies, bioinformatics tools, and reduced costs. The increased use of WGS is accompanied by challenges such as standardization, quality control (QC), and data sharing. Thus, there is global need for inter-laboratory WGS proficiency test (PT) schemes to evaluate laboratories' capacity to produce reliable genomic data. Here, we present the results of the first iteration of the Genomic PT (GPT) organized by the Global Capacity Building Group at the Technical University of Denmark in 2020. Participating laboratories sequenced two isolates and corresponding DNA of Salmonella enterica, Escherichia coli and Campylobacter coli, using WGS methodologies routinely employed at their laboratories. The participants' ability to obtain consistently good-quality WGS data was assessed based on several QC WGS metrics. A total of 21 laboratories from 21 European countries submitted WGS and meta-data. Most delivered high-quality sequence data with only two laboratories identified as overall underperforming. The QC metrics, N50 and number of contigs, were identified as good indicators for high-sequencing quality. We propose QC thresholds for N50 greater than 20 000 and 25 000 for Campylobacter coli and Escherichia coli, respectively, and number of contigs >200 bp greater than 225, 265 and 100 for Salmonella enterica, Escherichia coli and Campylobacter coli, respectively. The GPT2020 results confirm the importance of systematic QC procedures, ensuring the submission of reliable WGS data for surveillance and outbreak investigation to meet the requirements of the paradigm shift in methodology.

Rheological Behaviors of Waste Polyethylene Modified Asphalt Binder: Statistical Analysis of Interlaboratory Testing Results

Abstract This article investigated the effect of waste polyethylene (PE) on the modified asphalt binders’ rheological behavior from a statistical point of view. The interlaboratory testing results from the RILEM Technical Committee 279 Valorization of Waste and Secondary Materials for Roads Task Group 1 were used for this purpose. First, an unaged 70/100 penetration graded neat binder was selected as the reference material. Next, a single 5 % content of waste PE additives (PE-pellets and PE-shreds) was mixed with a 95 % neat binder to prepare two PE modified binders. Then, dynamic shear rheometer–based temperature-frequency sweep tests were performed over a wide range of temperatures and frequencies to evaluate the rheological properties of these three binders. Different rheological behaviors were observed in the isochronal plots at high temperatures. Based on a reproducibility precision requirement proposed for phase angle, 28°C was set as the transition temperature across the rheological behaviors. Next, according to the three rheological behaviors defined in a previous study by the authors, statistical analysis was introduced to identify sensitive rheological parameters and determine the thresholds. Results indicate that the phase angle measured above 28°C and 1.59 Hz can be used as a sensitive parameter to discriminate the three rheological behaviors of PE modified binders. The thresholds among different behaviors were also calculated as an example for phase angle measured at the highest common testing temperature of 70°C. Additional experimental evaluations on more types of PE modified binders, especially at intermediate and high temperatures, are recommended to better understand their influence on the rheological behavior of PE modified binders.

Sample preparation techniques on dynamic shear rheometer testing: round robin tests on bitumen

Three interlaboratory tests conducted by European laboratories were studied, in which 37 laboratories participated in 2018, rising to 46 in 2019 and 2020. A RTFO-aged neat bitumen 20/30 and PMB 45/80-55 in RTFO-aged and unaged conditions were tested using a DSR at frequency of 1.59 Hz with PP08 and PP25 geometries at temperatures ranging from 10°C to 65°C. To assess variation in numerous areas of test method EN14770:2012 practices and the underlying impact on test outcomes, a statistical analysis on G* and δ is reported. The finding emphasises the need of using a detailed written sample preparation protocol to limit operators’ latitude while conducting tests. The statistical investigation suggests that the sample mounting onto rheometer stage and the sample manufacturing oven setup process require more attention. Furthermore, δ precision outperforms the EN14770:2012 criteria; nevertheless, |G*| precision does not match EN14770:2012 for all the testing combinations.

Analysis of Clinical Laboratory Detecting Challenging Variants from Exome Sequencing Using Simulated Patient–Parent Trio Sample: Pilot Study for Neurodevelopmental Disorder de Novo Variants

To date, there has been no systematic analysis for the clinical laboratory in detecting technically challenging variants using the trio-based exome sequencing (ES) approach. Here, we present an interlaboratory pilot proficiency testing study that used synthetic patient-parent specimens to assess the detection of challenging variants with de novo dominant inheritance modes for neurodevelopmental disorders using various trio-based ES. In total, 27 clinical laboratories that performed diagnostic exome analyses participated in the survey. One of the 26 challenging variants was identified by all laboratories, whereas all 26 variants were identified by only nine laboratories. The lack of identification of mosaic variants was often due to the bioinformatics analysis that excluded the variant. For missing intended heterozygous variants, probable root causes were related to the technical bioinformatics pipeline and variant interpretation and reporting. For each missing variant, there may be more than one probable reason from the different laboratories. There was considerable variation in interlaboratory performance for detecting challenging variants using trio-based ES. This finding may have important implications for the design and validation of tests for different variant types in clinical laboratories, especially for technically challenging variants, and necessary workflow modification can potentially improve trio-based ES performance.

THE STUDY OF METROLOGICAL CHARACTERISTICS OF THE OBTAINED SUBSTANCES OF FAT-SOLUBLE VITAMINS BY INTERLABORATORY COMPARISON TESTS

Relevance. This article discusses the possibility of using substances isolated from natural raw materials of fat-soluble vitamins retinol-palmitate (vitamin A), cholecalciferol (vitamin D3), tocopherol-acetet (vitamin E) in order to create domestic standard samples of approved type (SSS). The use of SSS in analytical practice, as well as in scientific research, makes it possible to ensure the accuracy and reliability of experimental results, to ensure the traceability of the result when performing analyses within the framework of repeatability and reproducibility (precision). The paper addresses issues related to the production and standardization of domestic pharmaceutical substances, as well as issues of standardization and conformity assessment of finished products of the pharmaceutical industry and other sectors of the national economy (food industry, agriculture, perfumery and cosmetics, the industry of production of goods for children's practice, etc.). The purpose of the work. To establish the quantitative content of fat-soluble vitamins A, D3, E, in the obtained substances claiming the status of SS with the approved type, as well as to determine their stability and uniformity by means of interlaboratory comparison tests (hereinafter referred to as ICT). Material and methods. The quantitative content of fat-soluble vitamins in the obtained substances was assessed by HPLC in 6 accredited analytical laboratories. The results were processed by evaluating the data provided for the presence of outliers and quasi-outliers using the Kohren, Grubbs and Mandel method. Results. The conducted studies under the comparison program showed that the results of the quantitative determination of the obtained vitamins are within the norms of the certified characteristic "Mass fraction of vitamin, %" in relation to the content of the determined characteristic in reference substances of imported production. Conclusions. As a result of the statistical data obtained, we have proved that the substances obtained from fat-soluble vitamins A, E, D3 comply with regulatory requirements based on the results of interlaboratory comparisons and can be recommended for the manufacture of domestic SS with the approval of their type, and it can also be assumed that the manufacturing processes of domestic and imported SS are harmonized. The quality of domestic SS is at an identical level with respect to foreign SS, but each is produced exclusively in the legal field of the manufacturer's state and is legitimate in its territory of application, which once again confirms the high need to create a domestic reference pharmaceutical base.

Busulfan Interlaboratory Proficiency Testing Program Revealed Worldwide Errors in Drug Quantitation and Dose Recommendations.

The clinical outcomes of busulfan-based conditioning regimens for hematopoietic cell transplantation (HCT) have been improved by personalizing the doses to target narrow busulfan plasma exposure. An interlaboratory proficiency test program for the quantitation, pharmacokinetic modeling, and busulfan dosing in plasma was developed. Previous proficiency rounds (ie, the first 2) found that 67%-85% and 71%-88% of the dose recommendations were inaccurate, respectively. A proficiency test scheme was developed by the Dutch Foundation for Quality Assessment in Medical Laboratories (SKML) and consisted of 2 rounds per year, with each round containing 2 busulfan samples. In this study, 5 subsequent proficiency tests were evaluated. In each round, the participating laboratories reported their results for 2 proficiency samples (ie, low and high busulfan concentrations) and a theoretical case assessing their pharmacokinetic modeling and dose recommendations. Descriptive statistics were performed, with ±15% for busulfan concentrations and ±10% for busulfan plasma exposure. The dose recommendations were deemed accurate. Since January 2020, 41 laboratories have participated in at least 1 round of this proficiency test. Over the 5 rounds, an average of 78% of the busulfan concentrations were accurate. Area under the concentration-time curve calculations were accurate in 75%-80% of the cases, whereas only 60%-69% of the dose recommendations were accurate. Compared with the first 2 proficiency test rounds (PMID 33675302, October, 2021), the busulfan quantitation results were similar, but the dose recommendations worsened. Some laboratories repeatedly submit results that deviated by more than 15% from the reference values. The proficiency test showed persistent inaccuracies in busulfan quantitation, pharmacokinetic modeling, and dose recommendations. Additional educational efforts have yet to be implemented; regulatory efforts seem to be needed. The use of specialized busulfan pharmacokinetic laboratories or a sufficient performance in busulfan proficiency tests should be required for HCT centers that prescribe busulfan.

Interlaboratory test results comparisons for active and reactive energy meter

The article is dedicated to the organization and performance of bilateral interlaboratory comparisons of test results for active and reactive energy meter. Interlaboratory comparisons of test results are presented. Evaluation of the laboratory test results bias is provided by means of functioning statistics En criterion. Analysis and conclusions concerning laboratory competence are obtained.

Preventing Mislabeling: A Comparative Chromatographic Analysis for Classifying Medical and Industrial Cannabis.

Gas chromatography (GC) techniques for analyzing and determining the cannabinoid profile in cannabis (Cannabis sativa L.) are widely used in standard laboratories; however, these methods may mislabel the profile when used under rapid conditions. Our study aimed to highlight this problem and optimize GC column conditions and mass spectrometry (MS) parameters to accurately identify cannabinoids in both standards and forensic samples. The method was validated for linearity, selectivity, and precision. It was observed that when tetrahydrocannabinol (Δ9-THC) and cannabidiolic acid (CBD-A) were examined using rapid GC conditions, the resulting derivatives generated identical retention times. Wider chromatographic conditions were applied. The linear range for each compound ranged from 0.02 μg/mL to 37.50 μg/mL. The R2 values ranged from 0.996 to 0.999. The LOQ values ranged from 0.33 μg/mL to 5.83 μg/mL, and the LOD values ranged from 0.11 μg/mL to 1.92 μg/mL. The precision values ranged from 0.20% to 8.10% RSD. In addition, forensic samples were analyzed using liquid chromatography (HPLC-DAD) in an interlaboratory comparison test, with higher CBD and THC content than GC-MS determination (p < 0.05) in samples. Overall, this study highlights the importance of optimizing GC techniques to avoid mislabeling cannabinoids in cannabis samples.

Applications of functional materials-based solid phase microextraction technique in forensic science

Sample extraction is a crucial step in forensic analysis, especially when dealing with trace and ultra-trace levels of target analytes present in various complex matrices (e. g., soil, biological samples, and fire debris). Conventional sample preparation techniques include Soxhlet extraction and liquid-liquid extraction. However, these techniques are tedious, time-consuming, labor-intensive and require large amounts of solvents, which poses a threat to the environment and health of researchers. Moreover, sample loss and secondary pollution can easily occur during the preparation procedure. Conversely, the solid phase microextraction (SPME) technique either requires a small amount of solvent or no solvent at all. Its small and portable size, simple and fast operation, easy-to-realize automation, and other characteristics thus make it a widely used sample pretreatment technique. More attention was given to the preparation of SPME coatings by using various functional materials, as commercialized SPME devices used in early studies were expensive, fragile, and lacked selectivity. Examples of those functional materials include metal-organic frameworks, covalent organic frameworks, carbon-based materials, molecularly imprinted polymers, ionic liquids, and conducting polymers, all widely used in environmental monitoring, food analysis, and drug detection. However, these SPME coating materials have relatively few applications in forensics. Given the high potential of SPME technology for the in situ and efficient extraction of samples from crime scenes, this study briefly introduces functional coating materials and summarizes the applications of SPME coating materials for the analysis of explosives, ignitable liquids, illicit drugs, poisons, paints, and human odors. Compared to commercial coatings, functional material-based SPME coatings exhibit higher selectivity, sensitivity, and stability. These advantages are mainly achieved through the following approaches: First, the selectivity can be improved by increasing the π-π, hydrogen bonds, and hydrophilic/hydrophobic interactions between the materials and analytes. Second, the sensitivity can be improved by using porous materials or by increasing their porosity. Third, thermal, chemical, and mechanical stability can be improved by using robust materials or fixing the chemical bonding between the coating and substrate. In addition, composite materials with multiple advantages are gradually replacing the single materials. In terms of the substrate, the silica support was gradually replaced by the metal support. This study also outlines the existing shortcomings in forensic science analysis of functional material-based SPME techniques. First, the application of functional material-based SPME techniques in forensic science remains limited. On one hand, the analytes are narrow in scope. As far as explosive analysis is concerned, functional material-based SPME coatings are mainly applied to nitrobenzene explosives, while other categories, such as nitroamine and peroxides, are rarely or never involved. Research and development of coatings is insufficient and the application of COFs in forensic science has not yet been reported. Second, functional material-based SPME coatings have not been commercialized as they don't yet have inter-laboratory validation tests or established official standard analytical methods. Therefore, some suggestions are proposed for the future development of forensic science analyses of functional material-based SPME coatings. First, research and development of functional material-based SPME coatings, especially fiber coatings with broad-spectrum applicability and high sensitivity, or outstanding selectivity for some compounds, is still an important direction for SPME future research. Second, a theoretical calculation of the binding energy between the analyte and coating was introduced to guide the design of functional coatings and improve the screening efficiency of new coatings. Third, we expand its application in forensic science by expanding the number of analytes. Fourth, we focused on the promotion of functional material-based SPME coatings in conventional laboratories and established performance evaluation protocols for the commercialization of functional material-based SPME coatings. This study is expected to serve as a reference for peers engaged in related research.

IMPLEMENTATION OF THE SYSTEM OF HONEY SAFETY CONTROL ON THE EXAMPLE OF ANALYZING OF RESIDUES OF TETRACYCLINE GROUP ANTIBIOTICS

The National Reference Laboratory of Drug Residues Control has implemented a system of "classical" honey safety control based on the parameters of antimicrobial drug residues: samples testing by the screening enzyme-linked immunosorbent assay (ELISA) method and, in the case of positive or possibly positive samples occurring, – retesting by confirmatory UPLC-MS/MS multi-method developed in the laboratory. The article presents the results of ELISA screening method validation for the determination of residual amounts of tetracycline group antibiotics (tetracycline, oxytetracycline, chlortetracycline, doxycycline) in honey samples using Tetracyclin® RIDASCREEN test kits by R-Biopharm (Germany) and Oxytetracycline ELISA by EuroProxima (the Netherlands) and its verification by means of the confirmatory method.&#x0D; In accordance with the Commission Implementing Regulation (EU) 2021/808, the validation of test kits proposed by the manufacturers was carried out taking into account the minimum required limit of detection. The fitness-for-purpose of the methods was confirmed based on the establishment of main validation parameters for screening methods (technical threshold and cut-off factor) using control (blank) and fortified honey samples with standard solutions of tetracycline at the level of ½ of the minimum required limit of detection, according to the "added-received" criterion. The proposed methods are the simple in carrying out, time- and cost-effective, which are their main advantages.&#x0D; The reliability of the results obtained by the proposed methods was verified using the developed confirmatory UPLC-MS/MS multi-method. The results of comparative studies of control (blank) honey samples and fortified with a standard solution of tetracycline antibiotics at the level of 2.5 and 5.0 μg/kg, as well as the results of the interlaboratory testing with the accredited laboratory (Germany) are presented.