Accreditation and Quality Assurance最新文献

A comprehensive study was undertaken to assess residual behaviour and dietary risk associated with a combination product containing trifloxystrobin and propineb in tomato, chilli and apple. Sample analysis was performed using validated QuEChERS method for trifloxystrobin and CGA 321113, while for propineb, method validated by Dubey and Stan (J Food Sci Technol 35:482–485, 1998) was used across all three crops, with residue detection using GC-ECD and UV–Vis spectrophotometer. Trifloxystrobin exhibited half-lives of 2.72–2.77 days in tomatoes, 2.49–2.89 days in chillies and 4.14–4.49 days in apples. Meanwhile, the half-life of propineb in tomatoes, chillies and apples were 1.27–1.51, 1.60–2.27 and 1.73–2.27 days, respectively. Upon comparing estimated daily intake (EDI) in India for both components of combination product with acceptable daily intake (ADI), the cumulative index of risk assessment and hazard index was consistently below 1 in all three crops, indicating no potential risk to consumers.

This review explores sofosbuvir, a nucleoside analog approved for hepatitis C, as a potential inhibitor of SARS-CoV-2 RNA-dependent RNA polymerase (RdRp), compared to remdesivir, which is constrained by hepatic and renal toxicity. RdRp, essential for viral replication, is a key target for COVID-19 therapeutics. Ligand-based virtual screening through the DrugRep virtual screening server, utilizing algorithms like Morgan fingerprint, identified compounds structurally akin to remdesivir. Structure-based molecular docking with CB-Dock2 and AutoDock Vina targeted the RdRp structure (PDB ID: 7BV2), revealing sofosbuvir’s binding affinity of − 7.6 kcal/mol, slightly lower than remdesivir’s − 8.4 kcal/mol, but with strong hydrogen bonds to ARG349 (3.05, 2.99, 2.89 Å) and CYS395 (3.41 Å), alongside Pi-Sigma and Pi-Alkyl interactions with PRO461 and VAL315. Molecular dynamics simulations (30 ns, LAMMPS) suggest sofosbuvir’s stability, with lower RMSD (~ 1.4 Å vs. ~ 1.8 Å for remdesivir) and more persistent hydrogen bonds, supported by its reliable structure and connectivity. Compared to remdesivir, sofosbuvir exhibits fewer unfavorable interactions and a well-established safety profile. Interaction analyses using BIOVIA Discovery Studio and LigPlot + confirmed sofosbuvir’s stability within the RdRp active site, corroborated by in vitro and clinical evidence. These findings highlight the pivotal role of in silico methods in drug repurposing for COVID-19. However, experimental validation is crucial to confirm sofosbuvir’s efficacy, particularly against SARS-CoV-2 variants, and to explore its therapeutic potential for addressing current and future viral threats.

A robust and reproducible LC–MS/MS method was developed and optimized for the simultaneous quantification of artemether (ART) and lumefantrine (LUF) in rat plasma, employing carbamazepine as an internal standard (IS). The mass spectrometer operated in positive ionization mode with electrospray ionization (ESI), yielding product ions at m/z 163.05(ART), m/z 511.95 (LUF), and m/z 194.1 (IS). Chromatographic separation was achieved using a Waters™ X Select C18 column (100 mm × 4.6 mm, 2.5 µm) with a mobile phase of 0.2 % formic acid in water: methanol (10:90) at a flow rate of 0.5 mL/min. Retention times for ART, LUF, and IS were 4.30 min, 1.60 min, and 2.46 min, respectively, within a 6-min runtime. The liquid–liquid extraction (LLE) method utilized ethyl acetate with acidified methanol for optimal analyte recovery, achieving mean recoveries of 92.12 % for ART and 91.07% for LUF. Calibration curves were linear over the range of 5–1000 ng/mL with regression coefficients of ≥ 0.9992. The method demonstrated high precision (%CV: 0.16–1.89) and accuracy (98.24–106.42 %) at the lower limit of quantification (LLOQ: 5 ng/mL). The method exhibited minimal matrix effects, with stability tests confirming analyte integrity under benchtop and freeze–thaw conditions. To the best of our knowledge, this is the first validated LC-MS/MS method developed for the simultaneous quantification of ART and LUF in rat plasma for preclinical pharmacokinetic studies, providing a novel, sensitive, and cost-effective analytical tool for routine high-throughput analysis.

Simultaneous high-performance thin-layer chromatography (HPTLC) method was developed and validated for the quantification of rivaroxaban and its aminomethyl process impurity/metabolite. Using a toluene–methanol–triethylamine (6:3.5:0.5%v/v/v) mobile phase, the method achieved optimized Rf values of 0.75 for rivaroxaban and 0.38 for the impurity. The method exhibited a linear response for both analytes in the range of 800–1300 ng/band, with correlation coefficients of 0.998 and 0.997, respectively. Sensitivity assessments revealed detection limits of 0.0086 ng/band for rivaroxaban and 0.0165 ng/band for the impurity, with quantification limits of 0.026 ng/band and 0.050 ng/band, respectively. Robustness and precision tests confirmed the method’s reliability, with %RSD values below 2.0 for all parameters. This validated HPTLC method offers an efficient solution for simultaneous determination of rivaroxaban and aminomethyl impurity/metabolite of rivaroxaban in pharmaceutical formulations. This simple HPTLC method provides a comprehensive approach for impurity profiling and quality control in pharmaceutical formulations. Its high sensitivity, reproducibility, and robustness make it a valuable tool in ensuring drug safety and compliance with regulatory standards.

Accurate serological testing relies on robust quality control (QC) procedures and the identification of factors influencing assay reliability. This retrospective study evaluated the impact of ambient laboratory conditions and reagent lot variability on the performance of the Euroimmun Anti-Measles Virus NP IgM ELISA, using data from 215 valid assay runs conducted between January 2023 and December 2024. QC metrics—Positive Control, Negative Control (NC), and Internal Quality Control (IQC) ratios—were analyzed across nine reagent kit lots. The IQC material, prepared and validated by the national serology reference laboratory, was used consistently to monitor longitudinal performance. Ambient temperature (20.0–25.0 °C) and humidity (21–84%) showed no significant linear correlation with QC ratios (p > 0.05). However, statistically significant variation in QC values was observed across reagent lots, especially for NC and IQC. NC failures (~ 7.7%) were dispersed and not linked to environmental extremes, suggesting possible procedural variation. In select instances, the IQC flagged deviations not captured by kit-supplied controls, underscoring its added value. These findings highlight reagent lot variability as the primary contributor to QC variation and reinforce the need for lot-specific validation, consistent monitoring, and integration of independent IQC materials as part of a robust quality assurance framework in accredited serological laboratories.

In this work, a simple, specific, accurate, and precise Reverse-Phase High-Performance Liquid Chromatography (RP-HPLC) method for estimating lidocaine hydrochloride and diltiazem hydrochloride in bulk and pharmaceutical dosage forms is developed and validated. The method uses an isocratic RP-HPLC approach for the separation and quantification of these compounds. Chromatographic analysis was performed on a Waters HPLC system that was fitted with a Thermo Scientific C₁₈ ODS column (250 mm × 4.6 mm, 5 μm). The mobile phase was supplied at a flow rate of 1.0 mL/min and consisted of methanol, acetonitrile, and buffer (orthophosphoric acid) in a 70:20:10 ratio. At 233 nm, a sharp, symmetrical peak with retention periods of 2.5 and 4.4 min was obtained through detection. Many parameters, such as linearity, accuracy, precision, specificity, and robustness, were evaluated for the method's validation. The method showed linearity throughout a concentration range of 20–100 µg/mL with correlation coefficients (r²) of 0.999 and 0.998, respectively, and the recovery of diltiazem hydrochloride varied from 99 to 100 %. Method optimization was accomplished through the use of a Box–Behnken design with desirability functions, and the validation parameters satisfied the requirements specified in the ICH Q2 (R1) recommendations. The AGREE assessment of the proposed RP-HPLC technique resulted in a score of 0.68, indicating a good balance between analytical performance and environmental sustainability. This confirms its environmental sustainability and suitability as an eco-friendly analytical method.

In this research work, a robust, Box–Behnken design-assisted reversed-phase liquid chromatography (RPLC) has been optimized for the quantification of Amlodipine Besylate, Metoprolol Succinate and Telmisartan followed by validation of method. Method is developed by utilizing Shimadzu LC-2010C HT HPLC system, autosampler injector and photodiode array detector. The separation was attained utilizing C₁₈ (5 μm, 250 × 4.6 mm), Phenomenex column as stationary phase. Optimized mobile phase was methanol/50 mM ammonium phosphate buffer adjusted to pH 3.5 (65:35%v/v). Detection wavelength set for estimation was 230 nm, and flow rate of mobile phase optimized was 1 ml/min. Box–Behnken design as a part of Analytical Quality by Design approach was used for optimization considering the critically influencing method attributes, flow rate (ml/min), molar concentration of buffer (mM) and buffer solution volume (ml) that resulted in optimized chromatographic conditions. The linearity exhibited a linear response within a range of 2–10 µg/mL, 19–95 µg/mL and 16–80 µg/mL (correlation coefficient: 0.9988, 0.9983 and 0.9972) for Amlodipine Besylate, Metoprolol Succinate and Telmisartan, respectively. The analytical method exhibited appropriate precision and accuracy considering the RSD values as less than 2% and mean recoveries in the range of 99.99–101.00% for all three drugs. Validation was ensured in compliance with ICH Q2 (R1) in terms of method’s sensitivity, accuracy, robustness and appropriate linearity for Amlodipine Besylate, Metoprolol Succinate and Telmisartan. Environmental impact evaluation of the developed method was conducted through the utilization of various software such as complex GAPI, AGREE and BAGI confirming that the optimized method was ecologic and environmentally safe. The method has been efficient in every parameter with accurate sustainability, simplicity, sensitivity and reproducibility.

Vibegron is a beta-3 adrenergic agonist receptor used in the treatment of overactive bladder. Present study aims to develop and validate enviornmentally sustainable UV spectrophotometric and Chromatography methods for the quantitative analysis of the Vibegron in both bulk drug substances and products, addressing the current lack of established quantification methods. The UV spectrophotometric method was developed using Acetonitrile as the solvent at a wavelength of 248 nm. While the HPLC method contained, Kromasil Classic C18 (250 mm*4.6 mm*5 µm) column, detection wavelength 248 nm, mobile phase composition Acetonitrile and Ammonium Acetate buffer 4.5 pH 44:56 (v/v) atflow rate of 0.8 mL/min, and injection volume 10 µL. The ICH Q2 (R2) guideline is followed to validate developed methods, including parameters like specificity, linearity, range, accuracy, assay, precision, LOD, LOQ, and robustness. The UV spectrophotometric and HPLC methods demonstrated strong linearity with R² = 0.9993 and 0.9972, respectively. The percentage recovery for accuracy and assay at each level was between 98 and 101% for both methods. Results were found to be consistent with an RSD < 2 for both methods for precision and robustness parameters. LOD was found to be 0.6520 µg/mL and 0.5767 µg/mL, and the LOQ was found to be 1.9759 µg/mL and 1.7476 µg/mL, respectively, for the UV and HPLC method. Sustainability assessment using standard tools revealed that the UV spectrophotometric method is greener and more economical, whereas, HPLC offers higher precision with increased cost and environmental impact. The methods ensure quality control, regulatory compliance, and sustainable, cost-effective analysis.

Ensuring food safety remains a pressing public health and economic imperative in Iraq, a nation marked by rich agricultural traditions yet hindered by infrastructural challenges and inconsistent regulatory enforcement. Despite established legal frameworks, significant gaps in compliance have led to persistent contamination issues, including heavy metals in meats, pathogenic bacteria in dairy products, and adulteration across food commodities. Proficiency testing (PT) can serve as a catalyst to improve this situation by providing an external quality assurance mechanism that benchmarks laboratory performance and fosters accuracy and consistency. International standards underscore the importance of PT-ISO/IEC 17025:2017 and ISO/IEC 15189:2022 requires laboratories to regularly verify result accuracy via inter-laboratory comparisons, and ILAC’s 2024 policy (P9:01/2024) mandates that accreditation bodies utilize PT outcomes as part of the lab accreditation process. Implementing robust PT schemes in Iraq, however, faces barriers—from technical limitations (scarcity of trained personnel and accredited PT providers) and financial constraints to limited regulatory enforcement compelling labs to participate. This review critically examines these challenges and synthesizes strategies to integrate PT into Iraq’s food safety framework. Key recommendations include investing in laboratory capacity (modernizing equipment and training staff), establishing a national PT program (or partnerships with international PT providers) to cover priority contaminants, and strengthening governance by embedding PT participation into national food safety regulations and laboratory accreditation criteria. By institutionalizing proficiency testing, Iraq can enhance the reliability and comparability of laboratory results, improve the credibility of its food safety oversight, and align its practices with international standards of accreditation and quality assurance.

This evaluation focused on measurement uncertainty in determining the content of benzylpenicillin sodium in injections using acid–base titration. The process involved β-lactam ring hydrolysis and back-titration of excess alkali with hydrochloric acid (HCl). The study identified and quantified uncertainty sources including repeatability, weighing, volumetric measurements (burette), and titrant concentration. The combined standard uncertainty was calculated using a spreadsheet approach adhering to GUM principles, and the impact of room temperature variations and triple determinations was assessed. The average benzylpenicillin sodium content was determined to be 96.9% with an expanded uncertainty (k = 2) of ± 2.2%. Triple determination reduced the contribution from repeatability, but volumetric uncertainties and titrant concentration uncertainty remained substantial contributors. Correcting for a mean room temperature of 25 °C did not markedly alter the result. Incorporating all quantified uncertainty components provided a reliable estimate of benzylpenicillin sodium content with defined confidence intervals. However, the inherent limitation of titration's specificity and the need for full metrological traceability of titrants are important considerations.