This research aimed to measure the impact of provenance on the yield, chemical profile and antimicrobial activity of Rosmarinus officinalis essential oil (EO) collected from cultivated and wild plants from two different regions in Morocco (Fez and Figuig). The chemical composition analysis was...
Background: Analytical validation is a sequence of operations aiming to evaluate the accuracy, reliability, and cost of analytical results for making informed decisions in method selection and meeting the requirements of regulatory institutions. Objective: This study aims to perform an analytical validation by comparing three different approaches: the accuracy profile, the uncertainty profile, and the conventional validation to assess the capability of each method in confirming the robustness of the results. Methods: The accuracy profile offers a comprehensive assessment of analytical performance and integrates systematic and random errors to determine if future results will satisfy the predefined acceptance limits. Meanwhile, the uncertainty profile, which is complementary and innovative, allows uncertainty estimation from validation data. These approaches were developed after conventional validation that relies on statistical methodologies based on separate evaluations of method criteria to provide a comparative framework for evaluating new methods. Results: This comparison will give recommendations for best practices related to analytical validation. The uncertainty profile is a graphical decision-making tool for determining full validation by integrating analytical validation and the estimation of measurement uncertainty, evaluating two statistical methods: β-expectation tolerance intervals and β-content, γ-confidence tolerance intervals, using a formula introduced by Saffaj and Ihssane, predicting that 95% of future results will fall within the acceptance limits of ±5%, revealing that the tolerance intervals for β-expectation are smaller than β-content, γ-confidence. Conclusion: The total error approaches offer robust recommendations for optimal methods for routine application. Highlights: This study highlights the critical need for appropriate analytical validation and the challenges arising from the absence of clear guidelines for that purpose. Different approaches emphasize the significant impact of the choice of an adequate method, which remains pivotal for providing accurate results in real-world scenarios. Concrete examples and simulations illustrate the viewpoints associated with different approaches to making decisions.
The phytochemical profiles, antioxidant capacities, mineral composition, and antibacterial activities of Zingiber officinale (Z. officinal) and Piper nigrum (P. nigrum) were explored through aqueous, ethanolic, and methanolic extractions. The extracts were analyzed for polyphenols, flavonoids, and tannins, and their antioxidant potential was assessed using the DPPH assay. UPLC-HRMS identified major bioactive compounds, including 6-gingerol and shogaol in Z. officinale, and piperine and piperlonguminine in P. nigrum. Mineral analysis showed that P. nigrum was particularly rich in essential elements, including calcium (Ca), magnesium (Mg), and iron (Fe). In antibacterial testing, P. nigrum demonstrated wider zones of inhibition against E. coli, whereas Z. officinale was more active at lower concentrations, showing MICs as low as 3.91 µg/mL against Salmonella and S. aureus. PCA analysis revealed strong correlations between phenolic content and biological effects. These results underscore the potential of both spices as effective natural agents for use in food preservation and health-promoting applications.
Four aromatic and therapeutic plants, Thymus vulgaris, Rosmarinus officinalis, Pimpinella anisum, and Foeniculum vulgare, were examined in this comparative study. The objectives were to assess its phytochemical composition; polyphenol, flavonoid, and tannin content; antioxidant and antibacterial activity; bioactive molecule identification; and critical trace element quantification. Its aqueous and organic extracts were examined, focusing on ethanolic extracts. The ethanolic extract’s ability to neutralize free radicals was validated by phytochemical studies and antioxidant tests, underscoring their role in preventing oxidative stress. An Ultra-Performance Liquid Chromatography—High-Resolution Mass Spectrometry Orbitrap Exploris 120 (UPLC–HRMS Orbitrap) was used to identify the bioactive chemicals, and the results showed a variety of compounds having antibacterial and antioxidant properties. The important trace elements found in these plants were also measured using a Graphite Furnace-Atomic Absorption Spectrometer (GF-AAS). These components are essential to the biological characteristics of the plants, especially their antioxidant and antibacterial capacities. Among the aqueous extracts, it was observed that Rosmarinus officinalis and Foeniculum vulgare exhibited a MIC of 3.91 µg/mL against Staphylococcus. Additionally, R. officinalis also demonstrated a MIC of 3.91 µg/mL against Escherichia coli. All of the data were interpreted and shown using principal component analysis. The results were grouped and explained using this statistical method, which revealed a strong association between the abundance of antibacterial and antioxidant chemicals in the four plants under investigation.
Background: Azithromycin is a complex molecule derived from erythromycin. The control of its dosage in conventional release tablets requires the analytical validation of its method to ensure accurate quantification and provide confidence in the reliability of the results for informed decision-making. Objective: This study aims to validate an innovative method for azithromycin quantification using the accuracy profile. Additionally, a comparison is made between the uncertainty measurements calculated from the validation data using two formulas proposed by Feinberg et al. and Saffaj and Ihssane and contrasted with the ISO GUM approach. Methods: A liquid chromatography system intended for azithromycin analysis equipped with a reversed-phase C18 stationary phase consisting of octadecyl silyl vinyl polymer in a UV detector operating at 210 nm at a temperature of 40°C in isocratic elution using a mobile phase of acetonitrile and dipotassium hydrogen phosphate buffer (6.7 g/L), in the fraction of (60:40, v/v) at pH = 8. Results: The various accuracy profiles are illustrated to ensure that a known quantity of anticipated findings acquired through the method stand inside the tolerance interval of 95% and remain within the previously set acceptance limits of ±5%. Measurement uncertainty provides comparable values using both formulas of the total error approach. However, it was observed that the ISO-GUM approach tends to overestimate the expanded uncertainty. Specifically, while the ISO-GUM approach provides a rigorous framework, the use of the validation data offers a more empirical uncertainty estimation. Conclusion: The approach based on the total error grants the ability to accurately close the routine uncertainty, emphasizing a complete validation. Highlights: The proposed method is robust for pharmaceutical application, demonstrating good accuracy, with 95% of tolerance and uncertainty limits falling within the predefined acceptance limits of ±5%.
This study was designed to evaluate antioxidant and antibacterial activities of essential oils from Rosmarinus officinalis obtained by three different extraction methods: DA: Artisanal distillation; the essential oils were obtained directly from small cooperatives using a very traditional (nonindustrial) method and based on the technique of Steam distillation; DI: Industrial distillation which is also based on steam distillation; and DC: hydrodistillation through Clevenger apparatus laboratory. The chemical analyses were carried out with gas chromatography/mass spectrometry (GC/MS); they identified 16 components representing more than 99.89% of the essential oil and indicate that the chemotype is 1,8-Cineole and varies according to the method used (DI: 49.09%, DA: 42.12%, and DC: 53.21%). The antioxidant activity was evaluated by the β-carotene bleaching test measuring percent inhibition of peroxidation in linoleic acid system. The disc diffusion and modified resazurin microtiter-plate assays were used, respectively, to evaluate the inhibition zones (IZ) and minimum inhibitory concentration (MIC) of Rosmarinus officinalis essential oil. In general, Rosmarinus officinalis L. essential oil showed a lower antioxidant and antimicrobial activity than 1,8-Cineole the major component of the essential oil.