Innovative high-performance liquid chromatography method development for the screening of 19 antimalarial drugs based on a generic approach, using design of experiments, independent component analysis and design space

Debrus, Benjamin; Lebrun, Philippe; Kindenge, Jérémie Mbinze; Lecomte, Frédéric; Ceccato, Attilio; Caliaro, Gabriel; Mbay, J. Mavar Tayey; Boulanger, Bruno; Marini, R.D.; Rozet, Eric; Hubert, Ph.

doi:10.1016/j.chroma.2011.05.102

Cited by 94 publications

(49 citation statements)

References 30 publications

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“…As suggested in ICH Q8 (R2) and previously successfully tested by Debrus et al [8] [9], a combining design of experiments (DoE) and Design Space (DS) was exploited to simultaneously optimize the separation based on predictive modeling technique using retention time-based responses [10]. Thereafter, a geometric transfer was performed for the HPLC developed methods in order to evaluate the robustness and improved gain of analysis time that is a challenge in the framework of fighting against counterfeit medicines.…”

Section: Introductionmentioning

confidence: 78%

“…The separation between the peaks of the critical pair has been chosen as a critical quality attribute (CQA) for the evaluation of quality chromatogram [8]. As proposed by Lebrun et al [8] [10] we used in this work the separation criterion (S) defined as the difference between the beginning of the second eluting peak (t RB ) and the end of the first eluting peak (t RE ) of the critical peak pair. Over the experimental domain, as shown on Figure 4, the probability of peak separation P (S > 0) was low: 0.4%.…”

Section: Prediction Of Optimal Separationsmentioning

confidence: 99%

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Fighting Poor Quality Medicines: Development, Transfer and Validation of Generic HPLC Methods for Analyzing Two WHO Recommended Antimalarial Tablets

Mbinze

Yemoa

Lebrun

et al. 2015

AJAC

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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 developed 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; 10 mM) (82.5:17.5, v/v) * These authors have equally contributed to this article. # Corresponding author. J. K. Mbinze et al.128 at 0.6 ml/min through a C18 column (100 mm × 3.5 mm, 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.

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Section: Introductionmentioning

confidence: 78%

Section: Prediction Of Optimal Separationsmentioning

confidence: 99%

Fighting Poor Quality Medicines: Development, Transfer and Validation of Generic HPLC Methods for Analyzing Two WHO Recommended Antimalarial Tablets

Mbinze

Yemoa

Lebrun

et al. 2015

AJAC

View full text Add to dashboard Cite

show abstract

“…The methods were developed through design of experiment and design space (DoE/DS) methodology [6][7][8] . Focusing on rapid and affordable aspects, a short column (RP18, 100 mm x 4.6 mm (ID), 3.5µm (dp)) and low cost organic solvent (methanol) were used in gradient mode with 10 mM ammonium dihydrogen carbonate buffer or ammonium formate buffer as mobile phase.…”

Section: Methodsmentioning

confidence: 99%

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

Habyalimana

Mbinze

Yemoa

et al. 2017

Journal of Pharmaceutical and Biomedical Analysis

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“…However, in a few cases, the coeluting peaks were seriously overlapped, and the spectra of the coeluting compounds were too similar to acquire accurate elution profiles for each compound, which was similar to the situation reported in the literature. 11 For these cases, the standard substances of the coeluting compounds were analyzed individually to acquire their elution profiles. It was found that in the elution profiles acquired by MCR-ALS, the biases in tR were small and acceptable while the biases in tB and tE were relatively large, compared with the chromatograms of the standard solutions.…”

Section: Resolution Of Coeluting Peaks and Peak Matchingmentioning

confidence: 99%

“…[9][10][11][12][13][14][15][16][17] In the AQbD approach, the relationships between the analytical parameters and the quality of the analytical methods are systematically investigated using risk assessment and the design of experiments (DoE) methodologies, and are then quantitatively represented in the form of mathematical models using multivariate statistical modeling methods. The AQbD approach is introduced in this work to acquire retention rules, i.e., to construct models relating the analytical parameters to the chromatographic parameters.…”

mentioning

confidence: 99%

Rapid HPLC Analytical Method Development for Herbal Medicine Formulae Based on Retention Rules Acquired from the Constituting Herbs

et al. 2018

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Herbal medicines (HMs), which offer a plethora of treatment options for complex diseases, have become increasingly popular worldwide in recent years. HM formulae, which are the combinations of two or more types of herbs, and therefore contain chemical compounds from each of the individual herbs, are the main form of HMs used in clinic. In this work, this type of sample matrix is regarded as a compound matrix, which is a mixture of their constituting ingredients. Similarly, a dietary supplement can also be regarded as a compound matrix if it is composed of multiple nutrients and/or extracts from several types of foods/plants. HPLC is the most commonly used method to analyze compound matrices in various fields. [1][2][3][4][5][6][7][8] However, due to the complexity of the matrices, chromatographic separation for these samples is challenging. Comprehensive pre-experiments to optimize the analytical parameters (e.g., gradient and pH of the mobile phase) are often needed to achieve good separation performance, which makes HPLC method development complicated and time-consuming. In the commonly used approach, the analytical parameters are optimized one by one in a process that is dependent on the experience of the researchers.Although many HPLC experiments are conducted and large amounts of raw data are acquired during method development, the rules of how the analytical parameters impact chromatographic separation are not effectively summarized and recorded. Consequently, when the composition of the compound matrix changes, a new analytical method must be developed from the very beginning if the performance of the original method becomes undesirable.An efficient approach to develop HPLC methods for compound matrices is needed.Since a compound matrix is the combination of its constituting ingredients, and HPLC methods for the individual ingredients have usually been developed before method development for the compound matrix, a question is raised: Are there any mutual retention rules between the compound matrix and its ingredients? If the answer is yes, then based on the retention rules acquired from the constituting ingredients, the impacts of the analytical parameters on the chromatographic separation of the compound matrix are predictable, which will enable rapid optimization of the analytical parameters for the compound matrix. When analyzing compound matrices and their constituting ingredients with the same HPLC analytical parameters, the same chemical compounds in these different samples have the same chromatographic parameters like retention time (tR) and peak width. Therefore, the relationships between the analytical parameters and these chromatographic parameters can be defined as the mutual retention rules between the compound matrices and their constituting ingredients. By effectively acquiring and utilizing the retention rules, the HPLC method development efficiency can be increased.In recent years, the analytical quality by design (AQbD) approach was proposed and has been successfully applied in the develo...

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Innovative high-performance liquid chromatography method development for the screening of 19 antimalarial drugs based on a generic approach, using design of experiments, independent component analysis and design space

Cited by 94 publications

References 30 publications

Fighting Poor Quality Medicines: Development, Transfer and Validation of Generic HPLC Methods for Analyzing Two WHO Recommended Antimalarial Tablets

Fighting Poor Quality Medicines: Development, Transfer and Validation of Generic HPLC Methods for Analyzing Two WHO Recommended Antimalarial Tablets

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

Rapid HPLC Analytical Method Development for Herbal Medicine Formulae Based on Retention Rules Acquired from the Constituting Herbs

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