Accreditation and Quality Assurance最新文献

A novel simultaneous estimation and stability-indicating RP-HPLC method was developed and validated for the simultaneous quantification of doxycycline hyclate and aloe-emodin in blend and in novel nanostructured lipid carriers. The mobile phase comprised a phosphate buffer to methanol at ratios of 40:60 (v/v) and 70:30 (v/v), both at pH 8, for the separation of doxycycline hyclate and aloe-emodin, respectively. Detection was performed using a PDA-M20A photodiode array detector at a lambda of 268 nm (doxycycline hyclate) and 250 nm (aloe-emodin). The method was validated according to the instructions of ICH guidelines for precision, accuracy, linearity, specificity, limit of detection, and limit of quantitation. The developed method exhibited linearity in the concentration range of 5–30 µg/mL for both analytes. The limit of detection and limit of quantitation were estimated to be 0.0279 µg/mL and 0.0846 µg/mL for doxycycline hyclate and 0.0262 µg/mL and 0.0795 µg/mL for aloe-emodin, respectively. Accuracy, as estimated by percent recovery, ranged from 180.37% to 216.52% for doxycycline hyclate and from 180.17% to 214.59% for aloe-emodin, depicting high recovery values. Forced degradation studies under five distinct stress conditions depict the competency of the method. The present study explored the simultaneous measurement of aloe-emodin and doxycycline hyclate in the novel nanostructured lipid carriers based gel. The technique demonstrated excellent specificity, accuracy, and sensitivity, with distinct retention times and well-defined peaks for each drug and its degradation products.

Noise in the signal of mass spectrometers is often corrected by an internal standard. This study investigates the effectiveness of internal standard application to environmental samples, namely, inductively coupled plasma-mass spectrometry analysis of particulate matter samples from the UK Heavy Metals Air Quality Monitoring Network at NPL. This Practitioner’s Report describes an investigation that has demonstrated potential drawbacks of internal standardisation using the set-up described, including bias in measured composition, which was found to contribute between 1.3–2.6%. Retrospective estimation of internal analyte content in particulate matter sample was carried out and found to be in good agreement with the literature (Y: 1 pg/m³, Sc: 5 pg/m³, In: 10 pg/m³, Bi: 50 pg/m³). Improvement of the signal to noise ratio is assessed and found to be minimal in the set-up investigated. It is concluded that for this application, introduction of an internal standard for high frequency noise correction gives minimal benefit and can even introduce measurement bias. These findings should be considered the next time the EN 14902 standard is revised.

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.

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.