Setup and validation of shake-flask procedures for the determinationof partition coefficients (log D) from low drug amounts

Several procedures based on the shake-flask method and designed to require a minimum amount of drug for octanol-water partition coefficient determination have been established and developed. The procedures have been validated by a 28 substance set with a lipophilicity range from -2.0 to 4.5 (logD7.4...

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Detalles Bibliográficos
Autores: Andrés Sanz, Axel, Rosés Pascual, Martí, Ràfols Llach, Clara, Bosch, Elisabeth, Espinosa Ferrer, Sonia, Segarra, Victor, Huerta Castaño, José María
Tipo de recurso: artículo
Estado:Versión aceptada para publicación
Fecha de publicación:2015
País:España
Institución:Universidad de Barcelona
Repositorio:Dipòsit Digital de la UB
OAI Identifier:oai:diposit.ub.edu:2445/143737
Acceso en línea:https://hdl.handle.net/2445/143737
Access Level:acceso abierto
Palabra clave:Lipofília
Química farmacèutica
Lipophilicity
Pharmaceutical chemistry
Descripción
Sumario:Several procedures based on the shake-flask method and designed to require a minimum amount of drug for octanol-water partition coefficient determination have been established and developed. The procedures have been validated by a 28 substance set with a lipophilicity range from -2.0 to 4.5 (logD7.4). The experimental partition is carried out using aqueous phases buffered with phosphate (pH 7.4) and n-octanol saturated with buffered water and the analysis is performed by liquid chromatography. In order to have accurate results, four procedures and eight different ratios between phase volumes are proposed. Each procedure has been designed and optimized (for partition ratios) for a specific range of drug lipophilicity (low, regular and high lipophilicity) and solubility (high and low aqueous solubility). The procedures have been developed to minimize the measurement in the octanolic phase. Experimental logD7.4 values obtained from different procedures and partition ratios show a standard deviation lower than 0.3 and there is a nice agreement when these values are compared with the reference literature ones