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11.
Danel C Chaminade P Odou P Bartélémy C Azarzar D Bonte JP Vaccher C 《Electrophoresis》2007,28(15):2683-2692
An analytical method for the enantioseparation of the 9-hydroxyrisperidone, main metabolite of the antipsychotic risperidone (Risp), was developed by CD-EKC in the dual CDs mode using anionic and neutral CDs at acidic pH 2.5. Preliminary experiments allowed us to select the more suitable couple of CDs composed of sulfated-alpha-CD and hydroxypropylated-beta-CD. The optimization of the main experimental parameters (concentrations of both CDs and concentration of the phosphate buffer) was based on a central composite design through the response surface methodology. Then, the influence of the voltage and the temperature on the enantioseparation was studied using the classical univariate approach. The final method permits to resolve the enantiomers of the 9-hydroxyrisperidone with a resolution of 3.13 and an analysis time of about 13 min. Finally, this method was successfully applied for the simultaneous determination of Risp and the enantiomers of 9-hydroxyrisperidone (9-OHRisp). 相似文献
12.
Noiret I. Schamps J. Danede F. Odou G. Lamiot J. 《The European Physical Journal B - Condensed Matter and Complex Systems》2004,41(1):23-30
Structural properties of two RbCdCl3 samples grown either from the melt or from aqueous solution are studied via X-ray diffraction over a closed temperature cycle between 20
C and 300
C. During cooling step (300
C), the crystal grown from the melt undergoes a phase transition at 110
C that drives it from the cubic structure into a tetragonal structure that still persists at 20
C. It undergoes exactly the reverse phase transition at the same temperature during the heating (
C) step that immediately follows. The other crystal grows from aqueous solution at 20
C in an orthorhombic structure (i.e. not tetragonal as that of the crystal grown from the melt and cooled down to this temperature). During the heating (
C) step, it undergoes a direct orthorhombic-cubic phase transition at 240
C (without passing through the tetragonal phase) whereas, during subsequent cooling (300
C), it does not exhibit the corresponding reverse phase transition but rather exhibits exactly the same cubic-tetragonal phase transition at 110
C as the crystal grown from the melt. However, for both crystals, this tetragonal phase observed at room temperature is unstable and slowly converts into an orthorhombic phase over the course of time. Complementary Differential Scanning Calorimetry (D.S.C.) and Thermo Gravimetric Analysis (T.G.A.) measurements have been carried out over the range (
)
C in order to interpret diffraction experiments.Received: 19 May 2004, Published online: 30 September 2004PACS:
61.10.Nz X-ray diffraction - 64.70.Kb Solid-solid transitions - 65.40.Ba Heat capacity 相似文献
13.
Cécile Danel Nathalie Azaroual Albane Brunel Damien Lannoy Pascal Odou Bertrand Décaudin Gaston Vermeersch Jean-Paul Bonte Claude Vaccher 《Tetrahedron: Asymmetry》2009,20(10):1125-1131
The configurational stability of 9-hydroxyrisperidone, an atypical antipsychotic, was studied under acidic, basic and physiological conditions. The analysis of 9-hydroxyrisperidone was performed using a recently validated chiral capillary electrophoretic method developed using a dual cyclodextrin mode (hydroxypropylated-β-CD and sulfated-α-CD). The kinetic parameters (rate constants, half-lives, and apparent free energy barriers) of the racemization were calculated through a mathematical model of the first-order reaction. The influences of the pH, the temperature, the nature and the concentration of the buffer, and the presence of an organic co-solvent were investigated. The fastest racemizations were observed under acidic conditions with high phosphate buffer concentrations and high temperatures. Under these conditions, the cyclodextrins (β-CD, methyl- β-CD, or hydroxypropylated-β-CD) added to both enantiomers in various molar ratios were not able to retard the racemization. Finally, the mechanism of racemization was investigated using nuclear magnetic resonance (NMR) and the proton–deuterium exchange of the proton H9 borne by the chiral carbon has proven the presence of an imine–enamine tautomerism. 相似文献