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Background: Accurate determination of active pharmaceutical ingredients and impurities is essential for ensuring the safety and effectiveness of medications. This study focuses on the validation of a high-performance liquid chromatography (HPLC) method for quantifying atorvastatin and its impurities, addressing a critical aspect of pharmaceutical analysis., Objective: The primary objective is to conduct a comprehensive validation study for the HPLC method, covering specificity assessment, response function establishment, and a detailed analysis of precision, trueness, and tolerance intervals. The emphasis is on demonstrating the method's precision, accuracy, and stability-indicating capabilities across various concentrations and compounds., Methods: The HPLC method is validated through rigorous assessments, including specificity, response function establishment, and analyses of precision, trueness, and tolerance intervals. Induced degradation experiments are conducted to explore atorvastatin's behavior under extreme conditions. Insights into the compound's synthesis and degradation pathways are provided through a proposed mechanism for intramolecular esterification., Results: The results affirm the precision, accuracy, and stability-indicating capabilities of the validated HPLC method. The method effectively differentiates between atorvastatin and its impurities, showcasing its suitability for pharmaceutical quality control., Conclusions: The validated HPLC method emerges as a robust and reliable tool for atorvastatin analysis, contributing significantly to pharmaceutical research and quality control. Its application ensures the safety and efficacy of medications, reinforcing its role in pharmaceutical analysis., Highlights: This study not only validates a crucial HPLC method for atorvastatin analysis but also provides insights into the compound's behavior under extreme conditions and its synthesis and degradation pathways. The validated method serves as a cornerstone in pharmaceutical research and quality control, ensuring medication safety and efficacy., (© The Author(s) 2024. Published by Oxford University Press on behalf of AOAC INTERNATIONAL. All rights reserved. For permissions, please email: journals.permissions@oup.com.)

Background: Monitoring impurities in drug products is a principal requirement of pharmaceutical regulatory authorities all over the world to ensure drug safety. For this reason, there is a great need for analytical QC of dugs products., Objective: In this study, a simple, efficient, and direct HPLC method was developed for the determination of three impurities of diclofenac., Methods: The HPLC method was developed using a mobile phase which consisted of an HPLC grade mixture, acetonitrile-0.01M phosphoric acid adjusted to pH 2.3 (1 + 3, by volume)., Results: The separation was performed in 15 min. The calibration curves of the three impurities were linear; the correlation coefficients were 0.999 at concentrations of 0.00015-0.003 µg/mL., Conclusion: The validation of this method shows that it meets all validation criteria. This shows the reliability of this method for the routine control of diclofenac impurities., Highlights: The validation of a robust HPLC method for the determination of diclofenac impurities is of great importance for the pharmaceutical industry to control its products., (© The Author(s) 2023. Published by Oxford University Press on behalf of AOAC INTERNATIONAL. All rights reserved. For permissions, please email: journals.permissions@oup.com.)

Background: The authentication of the geographical origin of virgin olive oils (VOO) generally requires the use of sophisticated and time-consuming analytical techniques. There is a need for quick and simple analytical techniques to predict the origin of olive oils., Objective: This study aims to examine the physico-chemical data of olive oils collected in six regions of Morocco during two consecutive years 2020 and 2021, and also to evaluate the ability of FT-IR in combination with discrimination tools to study the geographical origin of Moroccan olive oils., Method: Fourier transform infrared spectroscopy (FTIR) was used in this study as an emerging analytical technique to express a unique "fingerprint." A preliminary processing of the ATR-FTIR spectral data was performed by preprocessing algorithm to reduce the noise and the effect of signal variation as well as to minimize the effects of light scattering to extract the maximum analytical information from the spectra. A multivariate statistical procedure based on principal component analysis (PCA) coupled with linear discriminant analysis (LDA) as well as partial least-squares discriminant analysis (PLS-DA) was developed to provide a powerful classification approach., Results: Based on the PCA, six clusters were identified. The application of PCA-LDA and PLS-DA procedures demonstrate a powerful capacity in predicting the geographic origin of olive oils; this capacity is shown by the high value of correct classification rate (CCR), varying between 84.09 and 100%., Conclusions: The suggested procedure has given reliable results for the classification of olive oils according to their geographical origin, with advantages such as being fast, inexpensive, and not requiring any prior separation process., Highlights: The performance of this approach is significantly faster and possesses a higher degree of selectivity and sensitivity. The implementation of this technique for routine analysis of olive oil would save significant time, resources, and solvents., (© The Author(s) 2022. Published by Oxford University Press on behalf of AOAC INTERNATIONAL. All rights reserved. For permissions, please email: journals.permissions@oup.com.)

Background: Hypertension is a critical health problem; it is a prevalent risk factor for cardiovascular disease. Many treatments to combat hypertension are available, however many patients are resistant to the standard therapeutic approaches. The association of two or more substances in a fixed-dose combination is effective and tolerated as a substitute for the standard therapeutic approach., Objective: The new ultra performance liquide chromatography method was developed and validated to assay a combination of eight antihypertensive drugs including a diuretic: hydrochlorothiazide, dihydropyridine calcium channel blocker: Amlodipine and angiotensin II type 1 receptor blockers (sartans): valsartan, candesartan, eprosartan, olmesartan, losartan, and irbesartan in the pharmaceutical matrix., Methods: Chromatographic separation was performed on an Acquity® UPLC C18 1.7 µm 2.1 × 100 mm column, with a gradient of buffer solution and acetonitrile, in the proportion of (80:20 v/v)., Results: Good resolution was obtained, and an optimal analysis time of less than 5 min was achieved. The method was validated according to the International Conference on Harmonization guidelines following the classical approach and accuracy profile, and it is shown to be suitable for intended applications. The method was successfully used for quality control laboratories and the determination of these drugs combinations in pharmaceutical dosage forms., (© AOAC INTERNATIONAL 2020. All rights reserved. For permissions, please email: journals.permissions@oup.com.)

Background: Counterfeit medicines are an increasing scourge that are difficult to identify and they have become industrialized and widespread through highly organized illegal channels., Objective: This research aims to develop a robust method to determine four phosphodiesterase type-5 inhibitors in counterfeit drugs based on ultra-performance liquid chromatography., Method: Experimental design methodology (DOE) and design space (DS) recommended by ICH Q8 were used side-by-side in the development phase to define the optimal parameters as well as the robustness of the chromatographic method. Moreover, both the uncertainty and risk profile derived from the β-content and γ-confidence tolerance interval were investigated during the validation phase to examine the performance of this method., Results: Successful chromatographic results, in a high resolution between the four active ingredients and an optimal analysis time of less than 1.6 min, were achieved at the end of the optimization phase. In addition, validation results show a low risk of future measurements outside acceptance limits set at 5%., Conclusions: Our procedure was successfully applied in the routine phase to identify 23 illicit formulations of an erectile dysfunction drug., Highlights: An efficient method for the characterization of 4 authorized phosphodiesterase in less than 1.6 min was established. A DS approach was applied to test the performance of this analytical method during analytical development. A risk profile was then carried out to approve the validity of the analytical method through the uncertainty profile approach., (© AOAC INTERNATIONAL 2020. All rights reserved. For permissions, please email: journals.permissions@oup.com.)