Optimisation of the derivatisation reaction and subsequent headspace solid-phase microextraction method for the direct determination of chlorophenols in red wine

An acetylation reaction for the derivatisation of the three chlorophenols involved in cork taint was optimised using a Doehlert design for direct application in wine samples. In this first step, the optimum reaction pH, by adding different amounts of KHCO 3, and the required quantity of derivatisati...

Descripción completa

Detalles Bibliográficos
Autores: Martínez-Uruñuela, A., González-Sáiz, J.M. [0000-0002-4463-8343], Pizarro, C. [0000-0001-6450-8741]
Tipo de recurso: artículo
Estado:Versión publicada
Fecha de publicación:2004
País:España
Institución:Universidad de La Rioja (UR)
Repositorio:RIUR. Repositorio Institucional de la Universidad de La Rioja
OAI Identifier:oai:portal.dialnet.es:doc/5bbc698fb750603269e81d76
Acceso en línea:https://investigacion.unirioja.es/documentos/5bbc698fb750603269e81d76
Access Level:acceso abierto
Palabra clave:Acetylation
Chlorophenols
Cork taint
Experimental design
Solid-phase microextraction
Wine
Descripción
Sumario:An acetylation reaction for the derivatisation of the three chlorophenols involved in cork taint was optimised using a Doehlert design for direct application in wine samples. In this first step, the optimum reaction pH, by adding different amounts of KHCO 3, and the required quantity of derivatisation reagent were fixed. Then a series of parameters relevant for the headspace solid-phase microextraction process, such as desorption conditions, salt addition and agitation sample were evaluated. A simultaneous study of the type of fibre and extraction temperature was performed at five levels and based on the results obtained the rest of factors (sample volume and exposition time) that could potentially affect the extraction yields were optimised by a central composite design. According to the validation of the method, we propose here, to our knowledge, the first application of solid-phase microextraction for the direct analysis of chlorophenols in red wine samples. © 2004 Elsevier B.V. All rights reserved.