References of "Bouklouze, A"
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See detailARE CAPABILITY INDICES USEFULL TO ASSESS ANALYTICAL METHODS VALIDITY ?
Rozet, Eric ULg; Bouabidi, Abderrahim ULg; Talbi, M. et al

Poster (2012, February)

Analytical methods 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 ... [more ▼]

Analytical methods 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 ( ) 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 covering applications commonly encountered in the pharmaceutical industry. Finally a methodology to determine the optimal sample size required to validate analytical methods is also given using the proposed capability metric. [less ▲]

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See detailTransfer of drug dissolution testing by statistical approaches: Case Study
AL-Kamarany, M. A.; EL Karbane, M.; Ridouan, K. et al

in Saudi Pharmaceutical Journal (2012), 20(1), 93101

The analytical transfer is a complete process that consists in transferring an analytical procedure from a sending laboratory to a receiving laboratory. After having experimentally demonstrated that also ... [more ▼]

The analytical transfer is a complete process that consists in transferring an analytical procedure from a sending laboratory to a receiving laboratory. After having experimentally demonstrated that also masters the procedure in order to avoid problems in the future. Method of transfers is now commonplace during the life cycle of analytical method in the pharmaceutical industry. No official guideline exists for a transfer methodology in pharmaceutical analysis and the regulatory word of transfer is more ambiguous than for validation. Therefore, in this study, Gauge repeatability and reproducibility (R&R) studies associated with other multivariate statistics appropriates were successfully applied for the transfer of the dissolution test of diclofenac sodium as a case study from a sending laboratory A (accredited laboratory) to a receiving laboratory B. The HPLC method for the determination of the percent release of diclofenac sodium in solid pharmaceutical forms (one is the discovered product and another generic) was validated using accuracy profile (total error) in the sender laboratory A. The results showed that the receiver laboratory B masters the test dissolution process, using the sameHPLC analytical procedure developed in laboratory A. In conclusion, if the sender used the total error to validate its analytical method, dissolution test can be successfully transferred without mastering the analytical method validation by receiving laboratory B and the pharmaceutical analysis method state should be maintained to ensure the same reliable results in the receiving laboratory. [less ▲]

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See detailDevelopment and Validation of LC Method for the Diclofenac Sodium Release Determination Using Accuracy Profile Concept
Al-Kamarany, M.A.; El Karbane, M; Belomaria, M et al

in Asian Journal of Chemistry (2012), 24(10), 4393-4400

The article presents a rapid and sensitive RP-HPLC method with UV detection, using the diclofenac sodium release determination in solid pharmaceutical formulations. A novel validation strategy based on ... [more ▼]

The article presents a rapid and sensitive RP-HPLC method with UV detection, using the diclofenac sodium release determination in solid pharmaceutical formulations. A novel validation strategy based on accuracy profiles was used to select the most appropriate regression model with highest accuracy within well defined acceptance limits. Furthermore, the strategy was used to determine the limits of quantification as well as the suitable concentration range. The validation phase was completed by investigating of the risk profiles of various acceptable regression models in order to avoid obtaining measurements outside the acceptance limits fixed a priori. On the other hand, the present study shows how the LC method can be used more accurately to assess the kinetic dissolution profiles, instead the UV-visible method required by monographs of the USP. Robustness study was also performed in order to demonstrate the capability of this method to remain unaffected by a small and deliberate variation in method parameters. The LC method was validated using the total error approach, as a decision tool, guarantees that each of the future results that will be within the acceptance limits settled at ± 5 %. The UV spectrophotometric method based on the USP monograph, gives rise of impurities from diclofenac sodium in acidic condition (HCl 0.1 N). These impurities absorb at the same wave length (276 nm) as the active principal ingredient, which will yield some significant error in the per cent release during the dissolution test study. Described analytical method is a simple, sensitive, specific and more accurate indicating that this LC method is useful for manufacturing and quality control assay. [less ▲]

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See detailFlexibility and Applicability of β-expectation tolerance interval approach to assess the fitness of purpose of pharmaceutical analytical methods
Bouabidi, Abderrahim; Talbi, M.; Bourichi, H. et al

in Drug Testing and Analysis (2012), 4(12), 1014-1027

An innovative versatile strategy using Total Error has been proposed to decide about the method’s validity that controls the risk of accepting an unsuitable assay together with the ability to predict the ... [more ▼]

An innovative versatile strategy using Total Error has been 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. This strategy is based on the simultaneous combination of systematic (bias) and random (imprecision) error of analytical methods. Using validation standards both types of error are combined through the use of a prediction interval or β-expectation tolerance interval. Finally, an accuracy profile is built by connecting, on one hand all the upper tolerance limits, and on the other hand all the lower tolerance limits. This profile combined with pre-specified acceptance limits allows to evaluate the validity of any quantitative analytical method and thus their fitness for their intended purpose. In this work, the approach of accuracy profile was evaluated on several types of analytical methods encountered in pharmaceutical industrial field and also covering different pharmaceutical matrices. The four studied examples depicted the flexibility and applicability of this approach for different matrices ranging from tablets to syrups, different techniques such as liquid chromatography, or UV spectrophotometry and for different categories of assays commonly encountered in the pharmaceutical industry that are content assays, dissolution assays and quantitative impurity assays. The accuracy profile approach assesses the fitness of purpose of these methods for their future routine application,. It also allows to select the most suitable calibration curve, to evaluate adequately a potential matrix effect and propose efficient solution and to define correctly the limits of quantification of the studied analytical procedures. [less ▲]

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See detailDetermination of binary polymorphic mixtures of fluconazole using near infrared spectroscopy and X-ray powder diffraction: A comparative study based on the pre-validation stage results
Ziemons, Eric ULg; Bourichi, H.; Mantanus, Jérôme ULg et al

in Journal of Pharmaceutical & Biomedical Analysis (2011), 55

The aim of the present study was to develop near infrared (NIR) and X-ray powder diffraction methods (XRPD) able to determine pure crystalline form II of fluconazole in a binary polymorphic mixtures ... [more ▼]

The aim of the present study was to develop near infrared (NIR) and X-ray powder diffraction methods (XRPD) able to determine pure crystalline form II of fluconazole in a binary polymorphic mixtures containing form II and III. In order to give a first performance estimation of both methods, these latters were pre-validated using accuracy profiles, a statistical approach based on β-expectation tolerance intervals. Both methods showed a good trueness, precision and accuracy and their β-expectation tolerance intervals were fully included within the acceptance limits. The comparative study was carried out using statistical analysis based on the work of Bland and Altman. A good agreement between the two methods was demonstrated indicating the interchangeability of NIR method with XRPD method. [less ▲]

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See detailDO PLACEBO BASED VALIDATION STANDARDS MIMIC REAL BATCH PRODUCTS BEHAVIOUR? CASE STUDIES
Bouabidi, A.; Talbi, M.; Bouklouze, A. et al

in Journal of Pharmaceutical & Biomedical Analysis (2011), 55

Analytical methods validation is a mandatory step to evaluate the ability of developed methods to provide accurate results for their routine application. Validation usually involves validation standards ... [more ▼]

Analytical methods validation is a mandatory step to evaluate the ability of developed methods to provide accurate results for their routine application. Validation usually involves validation standards or quality control samples that are prepared in placebo or reconstituted matrix made of a mixture of all the ingredients composing the drug product except the active substance or the analyte under investigation. However, one of the main concerns that can be made with this approach is that it may lack an important source of variability that come from the manufacturing process. The question that remains at the end of the validation step is about the transferability of the quantitative performance from validation standards to real authentic drug product samples. In this work, this topic is investigated through three case studies. Three analytical methods were validated using the commonly spiked placebo validation standards at several concentration levels as well as using samples coming from authentic batch samples (tablets and syrups). The results showed that, depending on the type of response function used as calibration curve, there were various degrees of differences in the results accuracy obtained with the two types of samples. Nonetheless the use of spiked placebo validation standards was showed to mimic relatively well the quantitative behaviour of the analytical methods with authentic batch samples. Adding these authentic batch samples into the validation design may help the analyst to select and confirm the most fit for purpose calibration curve and thus increase the accuracy and reliability of the results generated by the method in routine application. [less ▲]

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See detailDoes placebo based validation standards mimic well real batch products behaviour? A case study
Bouabidi, Abderrahim ULg; Talbi, M.; Bouklouze, A. et al

Poster (2010, September)

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See detailCritical analysis of several analytical method validation strategies in the framework of the fit for purpose concept.
Rozet, Eric ULg; Bouabidi, A.; Fillet, Marianne ULg et al

in Journal of Chromatography. A (2010), 1217

Analytical method validation is a mandatory step at the end of the development in all analytical laboratories. It is a highly regulated step of the life cycle of a quantitative analytical method. However ... [more ▼]

Analytical method validation is a mandatory step at the end of the development in all analytical laboratories. It is a highly regulated step of the life cycle of a quantitative analytical method. However, even if some documents have been published there is a lack of clear guidance for the methodology to follow to adequately decide when a method can be considered as valid. This situation has led to the availability of several methodological approaches and it is therefore the responsibility of the analyst to choose the best one. The classical decision processes encountered during method validation evaluation are compared, namely the descriptive, difference and equivalence approaches. Furthermore a validation approach using accuracy profile computed by means of beta-expectation tolerance interval and total measurement error is also available. In the present paper all of these different validation approaches were applied to the validation of two analytical methods. The evaluation of the producer and consumer risks by Monte Carlo simulations were also made in order to compare the appropriateness of these various approaches. The classical methodologies give rise to inadequate and contradictory conclusions which do not allow them to answer adequately the objective of method validation, i.e. to give enough guarantees that each of the future results that will be generated by the method during routine use will be close enough to the true value. It is found that the validation methodology which gives the most guarantees with regards to the reliability or adequacy of the decision to consider a method as valid is the one based on the use of the accuracy profile. [less ▲]

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See detailEvaluation of decision methodologies for analytical method validation
Rozet, Eric ULg; Rudaz, S.; Bouabidi, A. et al

Poster (2009)

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See detailAnalysis of several analytical method validation strategies
Rozet, Eric ULg; Bouabidi, A.; Bouklouze, A. et al

Poster (2009)

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See detailMethodologies for the transfer of analytical methods: A review.
Rozet, Eric ULg; Dewé, Walthère ULg; Ziemons, Eric ULg et al

in Journal of Chromatography. B : Analytical Technologies in the Biomedical & Life Sciences (2009), 877

The transfer of a method from a laboratory to a production site is an important step in the development cycle of new pharmaceutical products. Method transfers are increasingly implemented due to the ... [more ▼]

The transfer of a method from a laboratory to a production site is an important step in the development cycle of new pharmaceutical products. Method transfers are increasingly implemented due to the economical pressure coming from the rationalization of production sites, analytical subcontracting and fusion of pharmaceutical groups. However, no official guidance regarding study design, data analysis, or decision procedures is present neither in FDA documents nor in ICH documents for method transfers. The experiments performed in such a transfer and the methodology used to accept or reject it should be fitted for purpose. In order to provide to analysts a global view of the problematic of analytical method transfer, this paper reviews the documentation available in the scientific literature about the design of transfer studies and the required sample size. Special focus is also made on the statistical methodologies available for decision making with particular emphasis on risk management. Examples of transfer of pharmaceutical, bio-pharmaceutical and biological methods published in the literature are reviewed in order to illustrate the various possibilities among the strategies for methods transfer. [less ▲]

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See detailRobustness testing of a chiral NACE method for R-timolol determination in S-timolol maleate and uncertainty assessment from quantitative data.
Marini Djang'Eing'A, Roland ULg; Rozet, Eric ULg; Vanderheyden, Yvan et al

in Journal of Pharmaceutical & Biomedical Analysis (2007), 44(3), 640-51

A robustness test of a capillary electrophoresis method for the chiral separation of timolol in nonaqueous acidified media was performed. A two-level Plackett-Burman design was applied in which one ... [more ▼]

A robustness test of a capillary electrophoresis method for the chiral separation of timolol in nonaqueous acidified media was performed. A two-level Plackett-Burman design was applied in which one qualitative and six quantitative factors were examined. Resolution, migration times and relative migration times to pyridoxine (selected as internal standard) were examined as qualitative responses to evaluate electrophoretic performance. A quantitative response, the content of R-timolol in S-timolol maleate sample, was also considered. Even though some significant factor effects were observed on the qualitative responses, it was still possible to quantify the R-timolol in the S-timolol maleate samples properly. The quantitative response was not significantly affected by the selected factors, demonstrating the robustness of the procedure. However, the use of different HDMS-beta-CD batches seemed to affect both types of responses necessitating to introduce a warning in the procedure. Since the experiments of the Plackett-Burman design can be assimilated to laboratories in an interlaboratory study, uncertainty can be evaluated using the robustness test data. The robustness test was set-up in such a way that the required variances could be estimated. [less ▲]

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See detailValidation of a potentiometric method using azithromycin selective electrode
Rachidi, Mohamed ULg; Cherra, Y.; Digua, K. et al

Poster (2006)

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See detailAnalytical validation of potentiometric method for cetirizinium ion
Rachidi, Mohamed ULg; Digua, K.; Hubert, Philippe ULg et al

in Analytical Letters (2006), 39(8), 1699-1708

Accuracy and reliability of the analytical results are crucial for ensuring quality, safety, and efficacy of pharmaceutical products. However, to ensure these criteria, analytical validation is required ... [more ▼]

Accuracy and reliability of the analytical results are crucial for ensuring quality, safety, and efficacy of pharmaceutical products. However, to ensure these criteria, analytical validation is required. In this matter, many official documents describing the criteria of validation are available. However, these concern mainly chromatography analysis and bio-analytical methods of pharmaceutical products, but they do not propose any experimental protocol for direct potentiometric methods using ion-selective electrodes applied in pharmaceutical analysis. In this work, we are proposing a validation strategy based on the normative and regulatory guidelines applied to a potentiometric method with a polymeric membrane selective to cetirizine dihydrochloride. The statistical analysis obtained from raw data is described for all steps of this protocol. Also this validated method was successfully applied to the determination of cetirizine in pharmaceutical preparations using direct potentiometry with a mean relative standard deviation of 0.57% and a mean recovery of 99.63%. [less ▲]

Detailed reference viewed: 163 (5 ULg)