Analytical and semipreparative enantioseparation of 9-hydroxyrisperidone, the main metabolite of risperidone, using high-performance liquid chromatography and capillary electrophoresis. Validation and determination of enantiomeric purity.
作者： Cécile Danel , Christine Barthélémy , Dalila Azarzar , Hugues Robert , Jean-Paul Bonte
DOI: 10.1016/J.CHROMA.2007.06.023
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摘要: Abstract The HPLC semipreparative enantioseparation of 9-hydroxyrisperidone (9-OHRisp) was studied by optimizing various experimental conditions: the nature chiral stationary phase (CSP), mobile composition, temperature and analyte loading. This successfully completed using polysaccharide Chiralcel OJ a n-hexane/ethanol/methanol (50/35/15, v/v/v) ternary phase. To assess enantiomeric purity both isolated isomers, three analytical methods UV detection were developed validated: one CE method dual cyclodextrin mode two either CSP in normal-phase or α-acid glycoprotein (α-AGP) reversed-phase mode. make it possible to obtain excellent enantioseparations (Rs > 3) with analysis times lower than 15 min, calculated limits allow for determination minor impurities (0.1%). Enantiomeric obtained dextrorotatory levorotatory enantiomers superior 99.9% equal 98.9%, respectively, which proved success enantioseparation. A brief comparison performances completes this work.
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