Thesis defence

Title : Microfluidic approach to crystallize the different phases of an active pharmaceutical ingredient

The jury will be composed by :

Valérie DUPRAY, Rapporteuse

SMS – Université de Rouen Normandie (Rouen)

François PUEL, Rapporteur

CentraleSupélec – Université Paris Saclay (Gif-sur-Yvette)

Alexandra PEÑA REVELLEZ, Examinatrice

Institut Néel – CNRS (Grenoble)

Pierrette GUICHARDON, Présidente  du jury

Centrale Marseille (Marseille)

Stéphane VEESLERDirecteur de thèse

Aix-Marseille Univ, CNRS, CINAM (Marseille)

Nadine CANDONI, Codirectrice de thèse

Aix-Marseille Univ, CNRS, CINAM (Marseille)

Benoît ROBERT, Invité

Sanofi-Aventis R&D (Vitry-sur-Seine)

Romain GROSSIER, Invité

Aix-Marseille Univ, CNRS, CINAM (Marseille)

Abstract :

Most of the active pharmaceutical ingredients (API) can exist, in the solid state, under several crystalline phases (polymorphs, solvates, cocristals…). These phases have different physicochemical properties, which can affect the drug efficacy and its manufacturing process. In the pharmaceutical industry, a solid-state screening is thus carried out in the early stages of a drug development, to identify the existing phases and choose the one to develop. At this step, only a small amount of raw material is available, reducing the number of experiments. Droplet microfluidics is used to reduce the crystallization volumes to nanoliter scale, and thus the amount of product. This makes it possible to increase the number of experiments, bringing a statistical approach to address the stochasticity of nucleation. This thesis presents the development of a modular microfluidic platform, easy to use and compatible with most solvents, for solid-state screening of active pharmaceutical ingredients and fundamental nucleation studies. It enables to generate saturated solutions and droplets starting from powder and their characterization, to measure solubility, to crystallize API by cooling or non-solvent addition processes and to monitor nucleation in time and as a function of the temperature to establish global statistics on nucleation (all phases included). Lastly, the different phases are identified in situ by Raman spectroscopy to perform phase to phase statistics.