Accreditation and Quality Assurance最新文献

A robust, precise, and environmentally friendly RP-HPLC method was developed and validated for the simultaneous quantification of netilmicin and benzyl alcohol in pharmaceutical formulations, with a specific focus on reducing reliance on ion-pairing agents. Traditional analytical methods for aminoglycosides often require high concentrations of such reagents to ensure adequate retention and separation. In this study, chromatographic parameters were systematically optimized to minimize the use of ion-pairing agents without compromising method performance. The method employed a Phenomenex C18 (250 mm × 4.6 mm, 5 µm) reversed-phase column under gradient elution, with UV detection at 205 nm. It demonstrated excellent linearity within 100 to 300 μg/mL for netilmicin and 10.0 to 30.0 μg/mL for benzyl alcohol, enabling accurate assay quantification in marketed product. Baseline resolution between netilmicin and its structurally related impurity, sisomicin, was achieved, confirming the method’s specificity. To establish stability-indicating capability, forced degradation studies were conducted under acidic, basic, oxidative, thermal, humidity, and photolytic stress conditions. Degradation products were well separated from the active components, affirming the method’s suitability for stability testing. The green chemistry approach focused on minimizing solvent use and waste. The results revealed adherence of the described method to the green analytical chemistry principles. Method validation was carried out according to ICH Q2(R1) guidelines, demonstrating compliance with criteria for specificity, linearity (R² > 0.999), system suitability, precision (RSD < 2 %), accuracy (98 to 102 %), recovery, and robustness. This validated method offers a reliable, sustainable analytical tool for routine quality control and stability assessment of netilmicin formulations, aligned with modern quality assurance practices and regulatory expectations.

Background

This study reported simultaneous estimation of kaempferol and vanillin in a binary mixture and formulation using Vierordt’s method, which is a cost-effective, precise, and accurate analytical method. Although vanillin and kaempferol have individually demonstrated strong therapeutic potential, no formulation has yet been developed. Moreover, a validated analytical method for their simultaneous estimation is currently lacking. This gap presents an opportunity to develop safer, more effective, and well-optimized therapeutic solutions through strategic advancements in both formulation design and analytical methodology.

Result

The procedure was validated as per the “International Council for Harmonization of Technical Requirements for Pharmaceuticals for Human Use (ICH)” guidelines. The method demonstrated linearity for vanillin (R² = 0.9973) and kaempferol (R² = 0.9960), with low LOD/LOQ values confirming high sensitivity, enabling accurate simultaneous estimation of both compounds in a binary mixture using Vierordt’s method. Excellent accuracy with recovery values confirming reliability of the method for precise quantification. The method demonstrated excellent intraday and interday precision for both vanillin and kaempferol with %RSD values below 2%, confirming its reproducibility. Strong robustness with %RSD values below 0.65% under slight wavelength variations indicated consistent absorbance response and accuracy across tested concentrations. Excellent ruggedness with %RSD values below 2% was recorded for both the drugs, confirming reliability of the method under varied analytical conditions. Average percentage recovery of 100.012% for kaempferol and 98.884% for vanillin, confirming its applicability for simultaneous estimation in varied ratio combinations.

Conclusion

Based on the clear spectral separation, absence of interfering substances, and successful method validation, the selection of Vierordt’s method was considered scientifically justified and suitable for the intended purpose. Thus, the developed system can accurately identify vanillin and kaempferol in a binary mixture or formulation.

A novel HPTLC method was designed and validated for the simultaneous quantification of Aceclofenac and Febuxostat, a newer pharmaceutical combination. The method incorporates green analytical chemistry principles. Chromatographic separation was performed on pre-coated silica gel 60 F₂₅₄ plates. Wavelength, chamber saturation time, volume of ethyl acetate, and solvent front were studied critically and optimized. Robustness was assessed by applying 2^4–1 fractional factorial design. The greenness of the method was assessed using four tools: Analytical Eco-scale, Blue Applicability Grade Index, Complementary Green Analytical Procedure Index, and Analytical Greenness Metric Approach. Further, RGB tool was used to assess the whiteness of the method. The optimized mobile phase (ethyl acetate: toluene: glacial acetic acid, 7:3:0.1) provided sharp peaks at R_f 0.47 and 0.71, respectively. Linearity was observed between 150 and 900 ng/band for Aceclofenac and 100–600 ng/band for Febuxostat, with correlation co-efficients of 0.9931 and 0.9788. The method was precise (%RSD < 2 %), accurate (92.7–96.9 % recovery), and robust (DoE-based fractional factorial design showed non-significant variation). Greenness was confirmed using Eco-Scale (84), AGREE (0.8), and BAGI tools. The method is simple, economical, and suitable for routine quality control of Febuxostat and Aceclofenac in topical formulations. The developed HPTLC method is efficient, precise, and adheres to green analytical chemistry principles. It provides a reliable and environmentally friendly approach for the simultaneous quantification of Aceclofenac and Febuxostat in ufasomal gel.

In the manufacturing process of pesticide formulations, quality control plays a crucial part in ensuring its effectiveness and meeting requirements of regulatory for safe use. In this paper, a simplified HPLC-based method has been developed for simultaneous quantitative determination of Pyriproxyfen and Bifenthrin in 10% EC formulation using a C-18 analytical column (150 mmX4.6 mmX5 µm). Based on chromatographic separation with good resolution, acetonitrile: water (80:20, v/v) was selected as mobile phase in isocratic mode with a flow rate of 1.2 mL/min at a constant column temperature of 30 °C and UV detection at 220 nm. The method was validated in line with SANCO/3030/99 rev. 5 guidelines encompassing the key parameters system suitability, linearity, precision, recovery, LOD & LOQ. The validation parameters were found within acceptance criteria. The LOD and LOQ for Pyriproxyfen was 8.6 mg/L and 26.0 mg/L while that of Bifenthrin was 10.0 mg/L and 30.0 mg/L, respectively. Precision with acceptable %RSD of < 2% and recoveries ranging from 80 to 120% were obtained. Further escorting the decision making and confidence in the reliability of the produced data, measurement uncertainty using Eurachem/ CITAC procedure were obtained. The contributions to the uncertainty of measurement were from sample preparation, calibration standards preparation, calibration curve, and purity data. The contribution to the uncertainty of measurement from the analysis by HPLC were repeatability and intra-lab reproducibility. The combined expanded uncertainty of measurement was between 0.15% and 0.19%. The proposed analytical method is suitable for simultaneous quantitative determination of pyriproxyfen and bifenthrin in respective formulations.

Pulses are a common vegetable and grain in the human diet because of their high protein content. The use of pesticides for control is impacted by a variety of pests, which eventually leads to a residue issue in the finished goods. Considering the point, a field trial conducted to study the dissipation of residues of chlorantraniliprole and emamectin benzoate in/on cowpea pods showed initial accumulation of 1.69 and 0.15 mg/kg at the recommended doses of 18.50 SC @ 30 g a.i./ha and 5 SG @ 10 g a.i./ha, respectively. The residues of chlorantraniliprole and emamectin reached below the limit of quantitation (LOQ) of 0.01 mg/kg on the 7th and 5th day, respectively. Both the residues followed first-order kinetics with half-lives of 1.1 and 1.9 days, respectively. A pre-harvest interval (PHI) of 5 days is advised for both pesticides on cowpea when the green pods are to be utilized as human food in order to be safe, according to the current study. Based on theoretical maximum residue contribution (TMRC) and maximum allowed intake (MPI), risk evaluation revealed that TMRC < MPI in every instance.

This study presents the development and validation of a stability-indicating UPLC-MS/MS method for the simultaneous determination of trifluridine, tipiracil hydrochloride and their impurities. The chromatographic separation was achieved on a Waters UPLC using the Acquity BEH Phenyl column (100 mm ×2.1 mm, 1.7 µm) with a mobile phase comprising methanol and ammonium formate buffer (50:50, v/v) at a flow rate of 0.5 mL/min. The detection was carried out at the wavelength of 257 nm. The validation of the developed method adhered to ICH guidelines, evaluating parameters such as specificity, linearity, precision, accuracy, robustness and forced degradation. The method exhibited excellent linearity (R² > 0.999), high precision (%RSD < 1%) and recoveries ranging from 99.54% to 100.90%. The method was demonstrated to be robust against variations in flow rate and mobile phase composition, showing reproducibility across analysts. Forced degradation studies under acidic, alkaline, oxidative, thermal, photolytic and hydrolytic conditions confirmed the method’s stability-indicating capability. Degradation products were identified and characterized using LC–MS/MS, providing enhancing its application for stability testing, which is crucial for ensuring the quality, safety and efficacy of pharmaceutical  formulations. The developed method has been reported to be reliable and suitable for routine analysis of trifluridine, tipiracil hydrochloride and their impurities/related substances in both bulk drug and dosage forms.

The study presents method development, optimization, and validation of RP-HPLC technique to measure dobutamine, a cardiotonic agent utilized in the treatment of acute heart failure and cardiogenic shock. An Analytical Quality by Design was used to optimize chromatographic parameters, such as composition of the mobile phase, flow rate, and temperature of the column, applied Central Composite Design. The resulting optimized procedure showed superior system suitability, consisting of tailing factor 1.0, number of plates 12036 and similarity factor of 98.9 percent, which was very high in terms of resolution and reproducibility. The six repeated injections used to measure the system precision were 2106, 310.67 in terms of mean peak area and the low %RSD was 0.3 which indicated a high reproducibility. According to forced degradation studies, dobutamine was found to be stable when exposed to acidic conditions, basic conditions and peroxide conditions and also under thermal conditions; though these findings were accompanied by a high photolytic degradation (9%) and thus need to be stored under light protection. The technique also showed linearity over the broad concentration range (50 %, 150 %) with an R² of 0.99996 and at three different concentrations of 50 %, 100 %, and 150 %, the recovery studies have shown accurate results with low %RSD values (0.2, 0.4). The robustness assurance ensured that there is minimum change in USP tailing, plate counts and % similarity factor with different chromatographic conditions hence robustness of this methodology. The standardized AQbD-informed RP-HPLC method exhibits great precision, accuracy, and reliability in the analysis of dobutamine during the pharmaceutical quality control with the ICH compliance, contributing to the safety of patients by the guarantee of consistent therapeutic efficacy.

Biomethane is expected to be important in meeting Europe’s greenhouse gas reduction target. The composition of biomethane varies, therefore, depending on the feedstock and process parameters. The European standards EN 16723 specify requirements for injecting biomethane into natural gas networks and its use as vehicle fuel. Ensuring that biomethane composition complies with the requirements set in the standards requires rigorous quality control processes and validated analytical methods. Method validation for parties lacking practical experience or training can be a complex process involving numerous steps and requires adequate guidelines, which were lacking for biomethane. The BiometCAP project has, therefore, developed a standardized protocol for evaluating gas analyzers in biomethane applications with detailed procedures for assessing instrument performance and ensuring accurate and reliable measurements. This article describes how to use the validation protocol with practical applications for evaluating the limit of detection and limit of quantification, the working range and linearity, the precision, the bias and finally to calculate the measurement uncertainties using the analytical method described in ISO 2620:2024 as an example. This method based on TD-CG/MS-FID can therefore be considered fit-for-purpose, providing reliable, precise and sensitive measurements for the analysis of VOCs as demonstrated for 3-carene, dichloromethane and hexamethyldisiloxane. Finally, the article also summarizes the measurement uncertainties obtained during an extensive evaluation exercise organized between seven NMIs across Europe. For any future validation work, measurement uncertainties of 1 to 10% relative for any regulated compounds can be used as reference.

The goal is to create an RP-HPLC technique that is easy to utilize, quick, and specific enough to measure Abiraterone and Niraparib in bulk and prescription dose forms using Box–Behnken response surface design with application to dissolution studies. Optimization was performed by Box–Behnken design with selecting mobile phase ratio of volume of acetonitrile, volume of trifluoroacetic acid, and flow rate as factors and evaluating responses, namely, retention time and tailing factor through Symmetry C18 column (150 × 4.6 mm, 3.5 µm) with a mobile phase of acetonitrile: 0.1% TFA (40:60 v/v) at a flow rate of 1 mL/min, detection at 257 nm, and a runtime of 6 min. Box–Behnken design compared the effect of flow rate, ratio of acetonitrile, and volume of TFA on retention time and tailing factor, and optimized conditions for increased sensitivity. Retention times were 2.013 min for Abiraterone and 3.655 min for Niraparib. The technique was found to be excellent in linearity with correlation coefficients (R²) of 0.999 for both drugs. Validation parameters such as system suitability, accuracy, precision, linearity, specificity, robustness, LOD, and LOQ were in compliance with ICH guidelines. Forced degradation and dissolution studies established the stability-indicating nature of the method and applicability for release profiling. This technique is an important improvement in the field of pharmaceutical analysis, providing a robust platform for antineoplastic drug development research and quality control.

Graphical abstract

The contemporary development of the society is characterized by a rapid and intensive development of technology and industry, which leads to the appearance of an increasing amount of different products, but also to environmental pollution as product of their work. In everyday life, before placing products on the market, it is necessary to test them. These tests are conducted by testing laboratories in accordance with the relevant specifications for the given products. In case these tests are performed in laboratories accredited to ISO/IEC 17025:2017 ‘General requirements for the competence of testing and calibration laboratories’, by an accreditation body in a country that is a signatory to the ILAC Mutual Recognition Arrangement, their results will be recognized internationally. The basic goal of this paper is to present the current state of accredited laboratories in the Republic of Serbia, i.e., the analysis of the first accreditations granted, the distribution of laboratories by cities in Serbia, the number of testing methods in accredited laboratories, as well as the subject of testing/calibration in them. In addition, statistical multivariate analyses—Pearson’s correlation matrix and principal component analysis—were performed to determine the correlation between accredited laboratories and socio-political parameters, as well as the similarity in the distribution of accredited organizations in Serbia. The results show that the Republic of Serbia has a fairly developed area of quality infrastructure, that there is a certain relation between the granting of initial accreditation and certain socio-political events, as well as that there is a linear dependence between the number of accredited testing and calibration laboratories and the socio-economic parameters of the city. In Serbia, a largest number of accredited testing laboratories analyze media from the environment; however, a large number of those that deal with the testing of materials, food and industrial equipment are also present.