References of "Boulanger, Bruno"
     in
Bookmark and Share    
See detailAnalysis of several analytical method validation strategies
Rozet, Eric ULg; Bouabidi, A.; Bouklouze, A. et al

Poster (2009)

Detailed reference viewed: 36 (4 ULg)
Full Text
Peer Reviewed
See detailTotal Error for the Valildation of Bioanalytical methods
Rozet, Eric ULg; Boulanger, Bruno ULg; Rudaz S et al

in Annales de Toxicologie Analytique (2009), 21(S1), 35

Detailed reference viewed: 113 (27 ULg)
Full Text
Peer Reviewed
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 ▲]

Detailed reference viewed: 230 (30 ULg)
See detailShort Course on Methof Validation
Boulanger, Bruno ULg; Hubert, Philippe ULg

Conference (2009)

Detailed reference viewed: 24 (2 ULg)
Peer Reviewed
See detailDesign Space for analytical methods. A Bayesian perspective based on multivariate models and prediction
Lebrun, Pierre ULg; Boulanger, Bruno ULg; Jullion, Astrid et al

Conference (2008, September)

Detailed reference viewed: 34 (13 ULg)
Peer Reviewed
See detailThe Expected Design Space for analytical methods: a new perspective based on modeling and prediction
Lebrun, Pierre ULg; Boulanger, Bruno ULg; Debrus, Benjamin ULg et al

Conference (2008, June)

The Design Space (DS) of an analytical method is defined as the set of factor settings that provides satisfactory results, with respect to pre-defined constraints. The proposed methodology aims at ... [more ▼]

The Design Space (DS) of an analytical method is defined as the set of factor settings that provides satisfactory results, with respect to pre-defined constraints. The proposed methodology aims at identifying a region in the space of factors that will likely provide satisfactory results during the future use of the analytical method in routine, through an optimization process of this method. First, the DS is statistically defined as derived from the β-Expectation prediction interval. Second, multi-criteria perspective is added in this definition as it is often required for optimizing analytical method. Finally, a Monte-Carlo simulation is envisaged to numerically predict and identify the DS under uncertainty. Examples based on high-performance liquid chromatography (HPLC) methods will be given, illustrating the applicability of the methodology. [less ▲]

Detailed reference viewed: 66 (8 ULg)
See detailUse of Independent Component Analysis and clustering methods to find and identify relevant components in a matrix of UV-spectral data
Lebrun, Pierre ULg; Debrus, Benjamin ULg; Boulanger, Bruno ULg et al

Scientific conference (2008, May)

In the framework of the elaboration of new pharmaceutical formulations, statistical methodologies can accelerate and automate the development and optimization of quantitative methods. To fulfil this ... [more ▼]

In the framework of the elaboration of new pharmaceutical formulations, statistical methodologies can accelerate and automate the development and optimization of quantitative methods. To fulfil this objective, design of experiment (DOE) are widely used. In this context, the same mixture of analytes is injected while LC operating conditions are assessed. This gives plenty of very different chromatograms that can be tedious and time-consuming to interpret. Recently, the independent component analysis (ICA) has shown its usefulness to interpret chromatogram, i.e. to separate numerical signals from a matrix containing data provided by liquid chromatography system equipped with ultra violet diode array detector (LC-UV DAD). A matrix containing peaks corresponding to different analytes is then obtained. A brief summary of the ICA algorithm, applied to this problem, will be first given. The aim of the current work is to show that an automated methodology can be used to match together ICA-identified peaks that correspond to the same analytes in different chromatograms. In this way, this task, attributed to analytical experts, can be quickened and easier. This methodology uses classical hierarchical agglomerative clustering with special dissimilarity measures between spectra. [less ▲]

Detailed reference viewed: 33 (16 ULg)
Full Text
Peer Reviewed
See detailEmpirical Relationship between Precision and Ultra-Trace Concentrations of Pcdd/Fs and Dioxin-Like Pcbs in Biological Matrices
Eppe, Gauthier ULg; Van Cleuvenbergen, Rudy; Smastuen Haug, Line et al

in Chemosphere (2008), 71(2), 379-87

Dioxin analysis in food and feed can be characterized as an analytical application where very high accuracy is required at very low levels of contamination. Gas chromatography (GC) in combination with (13 ... [more ▼]

Dioxin analysis in food and feed can be characterized as an analytical application where very high accuracy is required at very low levels of contamination. Gas chromatography (GC) in combination with (13)C-label isotope dilution (ID) high resolution mass spectrometry (HRMS) is the reference congener-specific technique characterized by pronounced selectivity, precision and trueness at parts-per-trillion (ppt) and sub-parts-per-trillion (sub-ppt) levels. The quality of the analytical data produced routinely by a laboratory should be adequate for its intended purpose, i.e., one will seek a compromise between the cost and time needed and the consequences of incorrect decisions due to erroneous results. The requirements for reproducibility are usually dependent on the analyte concentrations and have been expressed in various empirical functions. While Horwitz or modified functions are widely useful for many purposes, it would be difficult to expect these functions to cover every analytical problem. This study reports on precision characteristics achieved by the GC-ID-HRMS reference method for polychlorinated dibenzo-p-dioxins (PCDDs), polychlorinated dibenzofurans (PCDFs) and dioxin-like polychlorinated biphenyls (DL-PCBs) in food and feed in two interlaboratory method-performance studies among expert laboratories with long-standing experience in this field. Striking linear functions in log scale between reproducibility standard deviation and congener's level over a concentration range of 10(-8)-10(-14)g per g fresh weight are observed. The data fit very well to a Horwitz-type function of the form s(R)=0.153c(0.904), where s(R) and c are dimensionless mass ratios expressed in pgg(-1) on fresh weight, regardless of the nature of the toxic congeners, food and feed matrices, or sample preparation methods. We demonstrate that the proposed function is suitable for use as a fitness-for-purpose criterion for proficiency assessment in interlaboratory comparisons on dioxins and related compounds in food. [less ▲]

Detailed reference viewed: 80 (6 ULg)
Full Text
Peer Reviewed
See detailHarmonization of strategies for the validation of quantitative analytical procedures: a SFSTP proposal part IV. Examples of application.
Hubert, Philippe ULg; Nguyen-Huu, J.-J.; Boulanger, Bruno ULg et al

in Journal of Pharmaceutical & Biomedical Analysis (2008), 48(3), 760-71

A harmonized approach for the validation of analytical methods based on accuracy profile was introduced by a SFSTP commission on the validation of analytical procedure. This fourth and last document aims ... [more ▼]

A harmonized approach for the validation of analytical methods based on accuracy profile was introduced by a SFSTP commission on the validation of analytical procedure. This fourth and last document aims at illustrating this methodology and the statistics used. Therefore the validation of real case methods are proposed such as methods for the quality control of drugs, for the quantitation of impurities in drug substances, for bioanalysis or for the determination of nutriments. Furthermore, different types of analytical methods are used in order to demonstrate the applicability of the proposed approach to a wide range of methods such as liquid chromatography (LC-UV, LC-MS), spectrophotometry or ELISA. [less ▲]

Detailed reference viewed: 133 (31 ULg)
Full Text
Peer Reviewed
See detailRisk-Based Approach for the Transfer of Quantitative Methods: Bioanalytical Applications
Rozet, Eric ULg; Dewé, Walthère ULg; Morello, R. et al

in Journal of Chromatography. A (2008), 1189

The transfer of analytical methods from a sending laboratory to a receiving one requires to guarantee that this last laboratory will obtain accurate results. Undeniably method transfer is the ultimate ... [more ▼]

The transfer of analytical methods from a sending laboratory to a receiving one requires to guarantee that this last laboratory will obtain accurate results. Undeniably method transfer is the ultimate step before routine implementation of the method at the receiving site. The conventional statistical approaches generally used in this domain which analyze separately the trueness and precision characteristics of the receiver do not achieve this. Therefore, this paper aims first at demonstrating the applicability of two recent statistical approaches using total error-based criterion and taking into account the uncertainty of the true value estimate of the sending laboratory, to the transfer of bioanalytical methods. To achieve this, they were successfully applied to the transfer of two fully automated liquid chromatographic method coupled on-line to solid-phase extraction. The first one was dedicated to the determination of three catecholamines in human urine using electrochemical detection, and the second one to the quantitation of N-methyl-laudanosine in plasma using fluorescence detection. Secondly, a risk-based evaluation is made in order to understand why classical statistical approaches are not sufficient to provide the guarantees that the analytical method will give most of the time accurate results during its routine use. Finally, some recommendations for the transfer studies are proposed. [less ▲]

Detailed reference viewed: 86 (17 ULg)
Full Text
Peer Reviewed
See detailDevelopment of a new predictive modelling technique to find with confidence equivalence zone and design space of chromatographic analytical methods
Lebrun, Pierre ULg; Govaerts, Bernadette; Debrus, Benjamin ULg et al

in Chemometrics and Intelligent Laboratory Systems (2008), 91

A new method for modelling chromatographic responses is presented as a critical piece for the achievement of automated development of analytical methods. This methodology is based on four parts. First, we ... [more ▼]

A new method for modelling chromatographic responses is presented as a critical piece for the achievement of automated development of analytical methods. This methodology is based on four parts. First, we propose to use a very little set of statistical equations to create predictive models for retention time based responses as the apex, the width and the asymmetry of peaks. Second, an experimental design is set up to realize experiments. Third, using grid search over the domain, multi criteria decision is taken with respect to different local or global optimization criteria, used as desirability functions. This allows finding an optimal chromatogram. Fourth, we advice to investigate how the predictive error of the models propagates around optimal solution. This allows to give confidence in the optimal solution, in finding a set of zones that presumably will give an acceptable solution. Design spaces can be derived with a similar technique. The approach is exemplified with a real case and predictions of models at optimal analytical conditions are validated through new experiments. Flexibility is left over all the presented methodology. [less ▲]

Detailed reference viewed: 157 (35 ULg)
Full Text
Peer Reviewed
See detailHarmonization of strategies for the validation of quantitative analytical procedures - A SFSTP proposal - Part II
Hubert, Philippe ULg; Nguyen-Huu, J.-J.; Boulanger, Bruno ULg et al

in Journal of Pharmaceutical & Biomedical Analysis (2007), 45(1), 70-81

As reported in a previous paper[1], the main objective of the new commission of the Societe Francaise des Sciences et Techniques Pharmaceutiques (SFSTP) was the harmonisation of approaches for the ... [more ▼]

As reported in a previous paper[1], the main objective of the new commission of the Societe Francaise des Sciences et Techniques Pharmaceutiques (SFSTP) was the harmonisation of approaches for the validation of quantitative analytical procedures. In a series of meetings, members of this Commission have first tried to review the objectives of analytical methods and the objectives of validation methods and to recommend the use of two-sided beta-expectation tolerance intervals for total error of validation samples (accuracy profile) in the acceptance/rejection of analytical method in validation phase. In the context of the harmonization, the other objectives were: (i) to propose a consensus on the norms usually recognized, while widely incorporating the ISO terminology; (ii) to recommend to validate the analytical procedure accordingly to the way it will be used in routine; (iii) to elaborate a rational, practical and statistically reliable strategy to assure the quality of the analytical results generated. This strategy has been formalised in a guide and the three latter objectives made by the Commission are summarised in the present paper which is the second part of summary report of the SFSTP commission. The SFSTP guide has been produced to help analysts to validate their analytical methods. It is the result of a consensus between professionals having expertise in analytical and/or statistical fields. The suggestions presented in this paper should therefore help the analyst to design and perform the minimum number validation experiments needed to obtain all the required information to establish and demonstrate the reliability of its analytical procedure. (C) 2007 Elsevier B.V. All rights reserved. [less ▲]

Detailed reference viewed: 160 (23 ULg)
Full Text
Peer Reviewed
See detailUsing tolerance intervals in pre-study validation of analytical methods to predict in-study results - The fit-for-future-purpose concept
Rozet, Eric ULg; Hubert, Cédric ULg; Ceccato, Attilio ULg et al

in Journal of Chromatography. A (2007), 1158(1-2), 126-137

It is recognized that the purpose of validation of analytical methods is to demonstrate that the method is suited for its intended purpose. Validation is not only required by regulatory authorities, but ... [more ▼]

It is recognized that the purpose of validation of analytical methods is to demonstrate that the method is suited for its intended purpose. Validation is not only required by regulatory authorities, but is also a decisive phase before the routine use of the method. For a quantitative analytical method the objective is to quantify the target analytes with a known and suitable accuracy. For that purpose, first, a decision about the validity of the method based on prediction is proposed: a method is declared proper for routine application if it is considered that most of the future results generated will be accurate enough. This can be achieved by using the "beta-expectation tolerance interval" (accuracy profile) as the decision tool to assess the validity of the analytical method. Moreover, the concept of "fit-for-purpose" is also proposed here to select the most relevant response function as calibration curve, i.e. choosing a response function based solely on the predicted results this model will allow to obtain. This paper reports four case studies where the results obtained with quality control samples in routine were compared to predictions made in the validation phase. Predictions made using the "beta-expectation tolerance interval" are shown to be accurate and trustful for decision making. It is therefore suggested that an adequate way to conciliate both the objectives of the analytical method in routine analysis and those of the validation step consists in taking the decision about the validity of the analytical method based on prediction of the future results using the most appropriate response function curve, i.e. the fit-for-future-purpose concept. [less ▲]

Detailed reference viewed: 119 (28 ULg)
Full Text
Peer Reviewed
See detailImprovement of the decision efficiency of the accuracy profile by means of a desirability function for analytical methods validation - Application to a diacetyl-monoxime colorimetric assay used for the determination of urea in transdermal iontophoretic extracts
Rozet, Eric ULg; Wascotte, Valentine; Lecouturier, Nathalie et al

in Analytica Chimica Acta (2007), 591(2), 239-247

Validation of analytical methods is a widely used and regulated step for each analytical method. However, the classical approaches to demonstrate the ability to quantify of a method do not necessarily ... [more ▼]

Validation of analytical methods is a widely used and regulated step for each analytical method. However, the classical approaches to demonstrate the ability to quantify of a method do not necessarily fulfill this objective. For this reason an innovative methodology was recently introduced by using the tolerance interval and accuracy profile, which guarantee that a pre-defined proportion of future measurements obtained with the method will be included within the acceptance limits. Accuracy profile is an effective decision tool to assess the validity of analytical methods. The methodology to build such a profile is detailed here. However, as for any visual tool it has a part of subjectivity. It was then necessary to make the decision process objective in order to quantify the degree of adequacy of an accuracy profile and to allow a thorough comparison between such profiles. To achieve this, we developed a global desirability index based on the three most important validation criteria: the trueness, the precision and the range. The global index allows the classification of the different accuracy profiles obtained according to their respective response functions. A diacetyl-monoxime colorimetric assay for the determination of urea in transdermal iontophoretic extracts was used to illustrate these improvements. [less ▲]

Detailed reference viewed: 79 (9 ULg)