References of "Lebrun, Pierre"
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See detailQuantitative determination of salbutamol sulfate impurities using achiral supercritical fluid chromatography
Dispas, Amandine ULg; Desfontaine, Vincent; Andri, Bertyl ULg et al

in Journal of Pharmaceutical & Biomedical Analysis (2017), 134

In the last years, supercritical fluid chromatography has largely been acknowledged as a singular and performing technique in the field of separation sciences. Recent studies highlighted the interest of ... [more ▼]

In the last years, supercritical fluid chromatography has largely been acknowledged as a singular and performing technique in the field of separation sciences. Recent studies highlighted the interest of SFC for the quality control of pharmaceuticals, especially in the case of the determination of the active pharmaceutical ingredient (API).Nevertheless, quality control requires also the determination of impurities. The objectives of the present work were to i) demonstrate the interest of SFC as a reference technique for the determination of impurities in salbutamol sulfate API and ii) to propose an alternative to a reference HPLC method from the European Pharmacopeia (EP) involving ionpairing reagent. Firstly, a screening was carried out to select the most adequate and selective stationary phase. Secondly, in the context of robust optimization strategy, the method was developed using design space methodology. The separation of salbutamol sulfate and related impurities was achieved in 7 minutes, which is seven times faster than the LC-UV method proposed by European Pharmacopeia (total run time of 50 minutes). Finally, full validation using accuracy profile approach was successfully achieved for the determination of impurities B, D, F and G in salbutamol sulfate raw material. The validated dosing range covered 50 to 150 % of the targeted concentration (corresponding to 0.3 % concentration level), LODs close to 0.5 μg/mL were estimated. The SFC method proposed in this study could be presented as a suitable fast alternative to EP LC method for the quantitative determination of salbutamol impurities. [less ▲]

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See detailChapter 11 - Validation of Supercritical Fluid Chromatography Methods
Dispas, Amandine ULg; Lebrun, Pierre ULg; Hubert, Philippe ULg

in Poole, Colin (Ed.) Supercritical Fluid Chromatography - Handbook in Separation Science (2017)

Method validation is the process of proving that an analytical method is acceptable for its intended purpose. The present chapter defines the validation criteria described in regulatory documents. Despite ... [more ▼]

Method validation is the process of proving that an analytical method is acceptable for its intended purpose. The present chapter defines the validation criteria described in regulatory documents. Despite the abundance of guidelines, the conclusion about method validity remains confused. In this context, the state-of-the-art validation methodology named total error approach is briefly explained as the methodology that should be followed for all method validations. Finally, a review of literature presents quantitative development and validation of supercritical fluid chromatography (SFC) methods considering a wide range of applications and analytical fields. [less ▲]

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See detailOptimization and validation of a fast Supercritical Fluid Chromatography method for the quantitative determination of vitamin D3 and its related impurities.
Andri, Bertyl ULg; Lebrun, Pierre ULg; Dispas, Amandine ULg et al

in Journal of Chromatography. A (2017)

In the uprising context of green analytical chemistry, Supercritical Fluid Chromatography (SFC) is often suggested as an alternative to Normal Phase Liquid Chromatography. Indeed, SFC provides fast ... [more ▼]

In the uprising context of green analytical chemistry, Supercritical Fluid Chromatography (SFC) is often suggested as an alternative to Normal Phase Liquid Chromatography. Indeed, SFC provides fast, efficient and green separations. In this report, the quantitative performances of SFC were challenged on a real-life case study: the Quality Control (QC) of vitamin D3. A rapid and green SFC method was optimized thanks to the Design of Experiments–Design Space (DoE–DS) methodology. It provided robust and high quality separation of the compounds within a 2 min timeframe, using a gradient of ethanol as co-solvent of the carbon dioxide. The analytical method was fully validated according to the total error approach, demon- strating the compliance of the method to the specifications of U.S. Pharmacopeia (USP: 97.0–103.0%) and European Pharmacopeia (EP: 97.0–102.0%) for an interval of [50–150%] of the target concentration. In order to allow quantification of impurities using vitamin D3 as an external standard in SFC-UV, correction factors were determined and verified during method validation. Thus, accurate quantification of impu- rities was demonstrated at the specified levels (0.1 and 1.0% of the main compound) for a 70.0–130.0% dosing range. This work demonstrates the validity of an SFC method for the QC of vitamin D3 raw material and its application to real samples. Therefore, it supports the switch to a greener and faster separative technique as an alternative to NPLC in the pharmaceutical industry. [less ▲]

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See detailScreening study of SFC critical method parameters for the determination of pharmaceutical compounds
Dispas, Amandine ULg; Lebrun, Pierre ULg; Sacre, Pierre-Yves ULg et al

in Journal of Pharmaceutical & Biomedical Analysis (2016), 125

Nowadays, supercritical fluid chromatography is commonly presented as a promising alternative technique in the field of separation sciences. Nevertheless the selection of chromatographic conditions and ... [more ▼]

Nowadays, supercritical fluid chromatography is commonly presented as a promising alternative technique in the field of separation sciences. Nevertheless the selection of chromatographic conditions and sample preparation of pharmaceutical compounds remain a challenge and peak distortion was previously highlighted. The main objective of the present work was to evaluate the impact of different critical method parameters (CMPs), i.e. stationary phase, mobile phase composition and injection solvent nature. The experiments were performed considering two groups of antimalarial molecules: one group with neutral/apolar compounds and the other one with salt form of polar compounds. In this context, another objective was to propose a suitable sample solvent for quantitative analysis. The interest of new generation stationary phase to obtain good peak shape and the interest to tune the mobile phase composition were demonstrated. During this study, design of experiments and desirability function approach enabled to highlight optimal chromatographic conditions in order to maximise peak capacity and to get acceptable value of symmetry factor. Regarding sample injection solvent composition, some counterintuitive results were observed: solvents closer to the mobile phase polarity (i.e heptane or 2-propanol/heptane mixture) did not provide best results in terms of peak symmetry. In addition, acetonitrile and short aliphatic alcohols offered an interesting alternative as injection solvent: toxicity of solvents used is clearly reduced and better quantitative performances could be expected while keeping high peak capacity and symmetric sharp peaks. Finally, the quantitative performances were evaluated by the method validation for the quantitative determination of quinine sulfate in a pharmaceutical formulation. These better understandings on critical method parameters led SFC to be an even more promising technique in the field of the analysis of pharmaceutical compounds. [less ▲]

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See detailImplementing principles of Quality by Design (QbD) in validation context
Hubert, Cédric ULg; Lebrun, Pierre ULg; Rozet, Eric et al

Conference (2016, May 10)

Analytical method performances have to be specified by the analyst trough the definition of the “Analytical Target Profile (ATP)”, as proposed by the regulatory bodies. In the specific context of the ... [more ▼]

Analytical method performances have to be specified by the analyst trough the definition of the “Analytical Target Profile (ATP)”, as proposed by the regulatory bodies. In the specific context of the pharmaceutical industry, regulatory authorities have recently imposed the assessment and management of risk throughout the entire product lifecycle. This includes the analytical procedure and consequently its own lifecycle. The development step of an analytical method is still largely addressed using a “Changing One Separate Factor a Time (COST)” approach (also known as the “Quality-by-Testing (QbT)” approach). This strategy can lead to a suitable method for assessing the risk of routine use, even where the experimental domain is not examined. However, in order to consider an experimental domain rather than a set of specific experimental conditions during the development phase, a multivariate approach must be considered: the “Quality-by-Design (QbD)” strategy. This strategy allows the definition of a “Design Space (DS)” by means of design of experiments (DoE). This DS, computed considering critical method parameters, allows the analyst to focus on the main objective of an analytical method: obtaining reliable results using a robust method. In the course of a specific case study, the benefits of the QbD strategy in terms of managing the qualitative part of the analytical process were highlighted. Working in the context of analytical procedure, the validation step is a major part of the analytical method lifecycle. Indeed, the objective of analytical method validation is to demonstrate that this method is suited for quantifying the target analytes with an established and suitable level of accuracy, as defined by the “ATP”. This is sometimes called the “fit-for-future-purpose” concept. The decision regarding the validity of a method based on prediction can be achieved by using the “β-expectation tolerance interval” (accuracy profile). The capability of this approach to manage the quantitative part of the analytical procedure is nowadays largely illustrated in scientific literatures. Considering the assessment and management of risk throughout the analytical lifecycle, a global strategy allowing the unification of the development and validation phases in a single step was considered. With this innovative approach, a strategy allowing the management of global analytical risk (i.e., for both qualitative and quantitative part of the analytical method) was proposed. Indeed, the developed strategy allows validating an entire experimental domain by means of the accuracy profile rather than a single set of specific experimental conditions. With this strategy, the DS is no longer simply the place where qualitative performances are obtained, but also the space where quantitative performances of the analytical procedure are assessed and managed. [less ▲]

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See detailValidation des méthodes analytiques: Approche basée sur l'erreur totale
Ziemons, Eric ULg; Hubert, Cédric ULg; Marini Djang'Eing'A, Roland ULg et al

Scientific conference (2015, May 12)

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See detailDesign Space for Analytical Methods: Why ? What ? How ?
Rozet, Eric ULg; Debrus, Benjamin ULg; Lebrun, Pierre ULg et al

Conference (2015, January 22)

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See detailFighting Poor Quality Medicines: Develop-ment, Transfer and Validation of Generic HPLC Methods for Analyzing two WHO Recommended Antimalarial Tablets
Mbinze Kindenge, Jérémie; Yemoa, Achille; Lebrun, Pierre ULg et al

in American Journal of Analytical Chemistry (2015), 6

As serious but neglected public health problems, poor quality medicines, i.e. for antimalarial medicines, urged to be fought. One of the approaches is to consider the analytical chemistry and separative ... [more ▼]

As serious but neglected public health problems, poor quality medicines, i.e. for antimalarial medicines, urged to be fought. One of the approaches is to consider the analytical chemistry and separative techniques. In this study, a generic liquid chromatographic method was firstly devel-oped for the purpose of screening 8 antimalarial active ingredients, namely amodiaquine (AQ), piperaquine (PPQ), sulfalene (SL), pyrimethamine (PM), lumefantrine (LF), artesunate (AS), artemether (AM) and dihydroartemisinine (DHA) by applying DoE/DS optimization strategy. Since the method was not totally satisfying in terms of peak separation, further experiments were undergone applying the same development strategy while splitting the 8 ingredients into five groups. Excellent prediction was observed prior to correlation between retention times of predicted and observed separation conditions. Then, a successful geometric transfer was realized to reduce the analysis time focusing on the simultaneous quantification of two WHO's recommended ACTs in anti-malarial fixed-dose combination (AM-LF and AS-AQ) in tablets. The optimal separation was achieved using an isocratic elution of methanol-ammonium formate buffer (pH 2.8; 10mM) (82.5: 17.5, v/v) at 0.6ml/min through a C18 column (100mm×3.5mm, 3.5 μm) thermostated at 25°C. After a successful validation stage based on the total error approach, the method was applied to determine the content of AM/LF or AS/AQ in seven brands of antimalarial tablets currently marketed in West, Central and East Africa. Satisfying results were obtained compared to the claimed contents. [less ▲]

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