Accreditation and Quality Assurance最新文献

The current research focused on establishing a method for concurrently measuring teriflunomide (TFD) and querectin (QCN) accurately, precisely, and with simplicity. This method aims to be suitable for routine analysis purposes. The goal is to effectively utilize this combination effectively in the treatment of rheumatoid arthritis (RA) through a topical delivery approach. To date, there have been no reported UV-based methods for simultaneous estimation of TFD and QCN. The quantification was performed using the absorption factor method for multicomponent analysis. The developed method underwent validation in accordance with the guidelines set by the International Council for Harmonization of Technical Requirements for Pharmaceuticals for Human Use (ICH). The validated method demonstrated linearity within the concentration range of 2.0 to 12.0 μg/mL for both substances, exhibiting a regression coefficient of > 0.990. The developed method validated for accuracy and precision, demonstrating a recovery rate within the range and precision with an RSD of less than 2 % for both inter and intra-day measurements. Moreover, the developed method was effectively utilized for quantification in the prepared transferosomes using absorption factor method. The greenness of the proposed methods was assessed, showing their minimal environmental impact and low level of toxicity to the environment.

Green analytical methods have become an area of keen interest in the field of pharmaceutical analysis to safeguard both the operators’ health and the environment. The present work describes the systematic development of a green, simple, sensitive, and robust reversed-phase high-performance liquid chromatographic method for simultaneous quantitative analysis of pregabalin and duloxetine hydrochloride in capsules. The chromatographic separation was achieved on a Shim-pack Solar C₁₈ (250 mm × 4.6 mm, 5 µm) column. The proposed method used a mobile phase, comprising of di-potassium hydrogen phosphate buffer (pH 7.0; 20 mM) and acetonitrile delivered in a gradient mode. The separated analytes were monitored at 210 nm. Validation, as per the ICH Q2(R1) guidelines, endorsed the efficiency of the developed novel analytical method. Employing the optimized chromatographic conditions, pregabalin and duloxetine hydrochloride were well separated with retention times of 3.9 and 12.7 min, respectively. The linear ranges of duloxetine hydrochloride and pregabalin were between 10–40 µg/mL and 25–100 µg/mL, respectively. Greenness assessment of the developed method was evaluated using three different assessment tools viz. Analytical Eco-Scale, GAPI, and AGREE. This is the first analytical method to be developed for the simultaneous estimation of these drugs in pharmaceutical dosage form based on green chemistry principles. The developed method was applied for the simultaneous determination of pregabalin and duloxetine in capsule dosage form.

About 3.70 million tons of pesticides are consumed annually to improve agricultural revenues. Organophosphate (OP) is a significant pesticide class, representing approximately 40% of pesticides' global sales. Chlorpyrifos (CPF) has been an OP pesticide commonly used to prevent horticultural and domestic pests for the past 25 years. Although CPF was banned from household products by the United States Environmental Protection Agency (US-EPA) in the year 2000, its current sales in the US alone exceed 5,000 tons. Other authorities, such as European, Canadian and Egyptian, have also discontinued its use since 2020. Therefore, it is necessary to analyze CPF as a counterfeit pesticide in products and biological samples in the coming years. CPF has high toxicity, representing neurological and cardiovascular threats. The proposed research aims to develop a novel, fast, and cost-effective methodology to estimate CPF in pesticide products and biological human plasma using gas chromatography (GC) with a flame ionization detector (FID). Notably, only a few GC-FID methods were reported for CPF analysis in marketed products. Still, none has yet been reported for its determination in plasma using GC-FID despite being greener, cheaper, and simpler than GC-tandem mass spectrometry (MS/MS). Both procedures were validated according to the International Council for Harmonization (ICH) guidelines. The retention time was 13.3 min. Linearity was perceived in the concentration of 20.0–100.0 μg/mL, with a coefficient of determination of 0.9909 for analytical and 0.9905 for bio-analytical application, respectively. The detection (LOD) and quantification limits (LOQ) were 0.29 and 0.87 μg/mL. Further, the greenness of the developed technique was assessed and compared to some other reported methodologies. The validation and greenness results indicate that both methods are reliable and sensitive, making them suitable for routine quality control of CPF in marketed products and biological samples.

The concentration of trifluoroacetic acid in surface and groundwaters and drinking water is subject of increasing concern. Since there is no standardised procedure available, German standardisation body DIN has initiated the first draft standard using liquid chromatography with tandem mass spectrometry (LC–MS/MS) after direct injection for the concentration range between ≥ 0.1 and 3 µg/L. Herein, the interlaboratory comparison as final validation step involving 12 expert laboratories from Germany and Switzerland is described. Two groundwaters, two surface waters, a drinking water, a rainwater, and two fortified groundwater samples displayed relative repeatability standard deviations between 3 and 7% and relative reproducibility standard deviation between 6 and 20% and were included in the draft standard DIN 38407-53.

As of September 2024, 964 clinical laboratories in China have achieved ISO 15189 accreditation, demonstrating their adherence to internationally recognized standards in quality, technology, and management. However, in one such ISO 15189-accredited laboratories, discrepancies arose between β-human chorionic gonadotropin (β-hCG) test results and the clinical manifestations of pregnant women, following a change in the reagent batch number. An investigation revealed that although the laboratory had established internal quality control (IQC) procedures and performance verification protocols for reagents and consumables for β-hCG testing, and monitored the ongoing validity of test results according to established standards, the IQC sample concentrations of the IQC sample did not encompass the ‘threshold’ required for the automated dilution detection of the testing system, the IQC procedure could not effectively assess the accuracy of high-concentration β-hCG samples, failing to detect whether the automated dilution procedure was functioning correctly. More concerningly, after the β-hCG test results for high-concentration specimens in the laboratory falsely decreased, laboratory personnel failed to promptly recognize the inconsistency between the test results and the clinical manifestations of the pregnant women. This issue was only recognized after 4 days, when it was raised by the requesting doctor. Therefore, we present this case to as a cautionary example for quality management in other clinical laboratories. Laboratories should focus on the quality risks associated with the automated dilution procedure in testing systems and are advised to monitor system performance by retesting patient samples and developing IQC materials.

Tavaborole (TVB), a benzoboroxole derivative, was approved for treating onychomycosis. Boron’s unique properties, such as variable oxidation states, and stability, require specialized analytical methods. The current RP-HPLC method was developed using eco-friendly solvents, maintaining pH, and providing a sharp peak at 5.7 min at 272 nm. A new NP-HPTLC technique was established employing a mobile phase composed of toluene and methanol, yielding an R_f value of 0.58 with a similar correlation coefficient of 0.9989 for both methods. The accuracy of TVB for both methods was evaluated at levels of 80 to 120%, providing the %RSD in the range of 0.42 to 0.86% (for HPLC) and 0.95 to 1.50% (for HPTLC). The reproducibility for the two methods was performed in triplicate (30–50 µg/ml) for HPLC and (4000 to 6000 ng/band) for HPTLC, and %RSD was evaluated. Replicates at 20 μg/ml for HPLC and 5000 ng/band for HPLTC show the %RSD of 1.42 and 0.65, respectively. Robustness parameters were evaluated by altering pH, wavelength, and flow rate for HPLC and mobile phase composition, plate saturation time, and development distance for HPTLC. The robustness was evaluated by altering the analyst to calculate a %RSD of 0.88 and 0.31 for HPLC and 0.12 and 0.22 for HPTLC. From the results, all the validation parameters are found within acceptable ranges. TVB showed stability in acidic and basic conditions, with degradation observed only under peroxide treatment. An attempt will be made to identify the probable and major degradants of TVB using LC–MS spectra, which was crucial considering the boron’s chemical properties. The RP-HPLC method was confirmed as environmentally sustainable using the AGREE program metrics. In contrast, the NP-HPTLC method met validation standards but was not considered eco-friendly due to solvent choice. Both methods are suitable for commercial applications.

Graphical abstract

ISO/IEC 17043:2015 specifies general requirements for the competence of providers and development and operation of proficiency testing schemes. As a requirement of ISO/IEC 17043:2015 accreditation, the Clinical Pharmacology Quality Assurance (CPQA) program uses ISO 17034 certified reference materials (CRMs) to produce proficiency testing materials in antiretroviral drug panels. CRMs that meet the ISO/IEC 17034 standard can be prohibitively expensive for CPQA participating laboratories (CPLs), requiring authentication of purity and identity by compendial testing. Here, to assist CPLs, we report on a compendial testing approach used to assess whether standard reference materials for bictegravir and cabotegravir, two commonly prescribed drugs used in combination regimens in the treatment of HIV-1 infection, for proficiency testing. Our approach uses high-performance liquid chromatography and thermogravimetric analysis to evaluate purity of the materials, and the combination of high-resolution mass spectrometry and proton nuclear magnetic resonance spectroscopy to establish molecular identity. Using this workflow, we identified standard reference materials for bictegravir and cabotegravir that are economical alternatives for CPLs.

The aim of this study was to develop a simple, accurate, and precise UV–Vis spectrophotometric method for the simultaneous determination of Andrographolide and Apocynin, bioactive compounds derived from Andrographis paniculata and Picrorhiza kurroa, respectively. These compounds are known for their hepatoprotective and antioxidant properties, and accurate quantification is essential for quality control of herbal formulations. A simultaneous equation method was developed based on the additive absorbances of Andrographolide and Apocynin at their respective λmax values (224 nm for Andrographolide and 274 nm for Apocynin). Linearity was established over a concentration range of 0.5 to 2.5 µg/mL for both compounds. Validation was conducted for parameters such as limits of detection (LOD), limits of quantification (LOQ), precision, and recovery. The method was applied to the analysis of three marketed herbal formulations. The method exhibited excellent linearity with correlation coefficients of 0.999 for Andrographolide and 0.998 for Apocynin. LODs were 0.012 µg/mL for Andrographolide and 0.066 µg/mL for Apocynin, with LOQs of 0.039 µg/mL and 0.202 µg/mL, respectively. Precision, confirmed by relative standard deviation (RSD) values below 2%, and recovery studies (98.66 %–102 % for Andrographolide, 98 %–101.60 % for Apocynin) demonstrated the method’s accuracy. The method successfully quantified the compounds in marketed herbal formulations, with results consistent with the label claims. The UV–Vis spectrophotometric method offers a reliable, precise, and cost-effective approach for the simultaneous quantification of Andrographolide and Apocynin in herbal formulations. Its simplicity and efficiency make it suitable for routine quality control in the pharmaceutical industry.

Recently, it has been shown that a probability distribution attributed to a constant, e.g. the true concentration of an analyte, cannot be used to accurately describe an objective set of information about the constant (Measurement Sensors 24, 2022, 100416;  Accreditation and Quality Assurance 29, 2024, 189–192). In this paper, that result is extended to show that such a distribution cannot always accurately describe subjective belief about it either. These results suggest that a logical system of uncertainty analysis in measurement can only be based on classical principles in which probability distributions describe patterns of measurements and errors under repetition. They call into question the premise underlying the approach to the evaluation of measurement uncertainty promoted in the supplements to the Guide to the Expression of Uncertainty in Measurement. The relevance of these results to the Eurachem/CITAC Guide Quantifying Uncertainty in Analytical Measurement (QUAM) is discussed, and QUAM is shown to be largely free of the problematic idea.