Controle qualité de Tramadol à Kisangani: Developpement, Validation et Application d'une méthode par Spectroscopie dans l'Ultra-violet

peer reviewedSubstandard and falsified medicines are circulating in low-income countries mostly without any control. We availed a simple and not expensive UV-Vis spectroscopic method to evaluate the quality of tramadol in Kisangani before and during the Covid-19 period. Methods: For the analytical quantitative method, an experimental design was applied to set up the optimal levels of the selected factors, namely, pH of dissolution medium, type of cuvette, and wavelength. Taking into account the capsule pharmaceutical formulation within 80 - 120 μg·mL-1 concentration range, we analyzed 89 tramadol samples from pharmacies and hospitals of the six Kisangani municipalities. Results: pH showed a significant effect on absorbance, whereas quartz cuvette and wavelength did not. A typical 100 μg·mL-1 tramadol solution gave an absorbance of 0.64 at 272 nm. Validation highlighted a matrix effect observed with a 6% bias. A correction factor of 0.9372 allowed to improve the accuracy profile, which were then totally included within the 10% acceptance limits. Quality control revealed that 25 samples out of 89 were not compliant in terms of manufacturing license, registration status in DRC and content as well. Conclusion: This study showed that the strengthening of analytical strategy in Kisangani is a need

SMALL SAMPLE SIZE CAPABILITY INDEX FOR ASSESSING VALIDITY OF ANALYTICAL METHODS

peer reviewedaudience: researcher, professional, studentAnalytical method’s capability evaluation can be a useful methodology to assess the fitness of purpose of these methods for their future routine application. However, care on how to compute the capability indices has to be made. Indeed, the commonly used formulas to compute capability indices such as Cpk, will highly overestimate the true capability of the methods. Especially during methods validation or transfer, there are only few experiments performed and, using in these situations the commonly applied capability indices to declare a method as valid or as transferable to a receiving laboratory will conduct to inadequate decisions. In this work, an improved capability index, namely Cpk-tol and the corresponding estimator of proportion of non conforming results (tolCpk−π) is proposed. Through Monte-Carlo simulations, they have been shown to greatly increase the estimation of analytical methods capability in particular in low sample size situations as encountered during methods validation or transfer. Additionally, the usefulness of this capability index is illustrated through several case studies

Separation of aminoglutethimide enantiomers using single and dual cyclodextrin system in capillary electrophoresis

peer reviewedaudience: researcher, professional, student, popularizatio

Development and validation of an LC method for the determination of six corticosteroids, salicylic acid and parabens in different pharmaceutical formulations

peer reviewedaudience: researcher, professional, student, popularizationMise au point de méthodes d’analyse en vue de l’étude de stabilité des principes actifs dans des formes dermopharmaceutiques dans le cadre de l’établissement d’un Nouveau Formulaire Thérapeutique valid

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Interest of Raman spectroscopy for the detection and analysis of poor-quality medicines

editorial reviewedAccess to quality medicines is an essential right of the patients. However, in 2017, the World Health Organization estimated that 1 in 10 medical products circulating in low- and middle-income countries is either substandard or falsified. This reinforces the fact that post-marketing surveillance (PMS) of medical products by strong national regulatory authorities (NRA) is crucial. To achieve an efficient PMS, the NRA need analytical tools at the inspection, screening, confirmatory and forensics levels to control the physicochemical properties of the samples. Among the analytical tools available, Raman spectroscopy is particularly interesting because of its spectral specificity and the wide variety of acquisition modes available. Handheld devices may be used directly on the field to confirm the presence of a specific active pharmaceutical ingredient (API) in a formulation [1]. Thanks to databases of pure ingredients, it is also possible to identify the compound present when a wrong API is present [2]. Recent developments have extended the applicability of handheld devices to the analysis of fluorescent chemicals and the analysis through barriers [3]. The detection of substandard medicines is also made possible with the construction of regression chemometrics models [4]. Benchtop systems and among them imaging systems are particularly useful in the confirmatory and forensic steps. Indeed, the imaging systems enable the visualization and identification of a large range of both organic and inorganic compounds used as API or excipients [5]. In addition, thanks to the high spatial resolution, it allows the detection of trace contaminants. This information may be of particular interest during prosecutions and the clustering of criminal cases. Nevertheless, the extraction of the relevant information from the raw measurements requires once again intensive work by highly trained staff. In conclusion, Raman spectroscopy have particularly interesting features for the PMS of medicines

Universal applicability of Total Error for the validation of bioanalytical methods

An innovative universal strategy using Total Error is thus proposed to decide about the method’s validity that controls the risk of accepting an unsuitable assay together with the ability to predict the reliability of future results. Several examples of applications of this validation methodology to various types of assays [LC-MS, ELISA, Bio-Assays] will be presented

APPLICATION OF DESIGN SPACE OPTIMIZATION STRATEGY TO THE DEVELOPMENT OF LC METHODS FOR SIMULTANEOUS ANALYSIS OF 18 ANTIRETROVIRAL MEDICINES AND 4 MAJOR EXCIPIENTS USED IN VARIOUS PHARMACEUTICAL FORMULATIONS

peer reviewedtAs one of the world’s most significant public health challenges in low- and middle-income countries,HIV/AIDS deserves to be treated with appropriate medicines, however which are not spared from coun-terfeiting. For that, we developed screening and specific HPLC methods that can analyze 18 antiretroviralmedicines (ARV) and 4 major excipients. Design of experiments and design space methodology wereinitially applied for 15 ARV and the 4 excipients with prediction thanks to Monte Carlo simulations andfocusing on rapidity and affordability thus using short column and low cost organic solvent (methanol)in gradient mode with 10 mM buffer solutions of ammonium hydrogen carbonate. Two other specificmethods dedicated to ARV in liquid and in solid dosage formulations were also predicted and opti-mized. We checked the ability of one method for the analysis of a fixed-dose combination composedby emtricitabine/tenofovir/efavirenz in tablet formulations. Satisfying validation results were obtainedby applying the total error approach taking into account the accuracy profile as decision tool. Then, thevalidated method was applied to test two samples coded A and B, and claimed to contain the tested ARV.Assay results were satisfying only for sample B