title: A simple and sensitive vortex assisted liquid-liquid microextraction method for the simultaneous determination of haloanisoles and halophenols in wines.
abstract: A vortex assisted liquid-liquid microextraction (VALLME) method was developed and optimised for the determination of the main compounds that can cause cork taint in wines, 2,4,6-trichloroanisole (TCA), 2,3,4,6-tetrachloroanisole (TeCA), 2,4,6-tribromoanisole (TBA) and pentachloroanisole (PCA); and their corresponding halophenolic precursors. Target compounds were determined by gas chromatography combined with a micro-electron capture detector (GC-µECD) system. Halophenol extraction and derivatisation processes were performed at the same time. To optimise the VALLME method, the extraction solvent was selected. Then, the other parameters of influence, such as volume of extraction solvent and derivatisation agent, salt addition and vortex time were optimised using a central composite design combined with desirability functions. Once the optimal conditions had been determined, the method was validated, showing satisfactory linearity (with correlation coefficients over 0.983), repeatability (below 10.0%) and reproducibility (below 11.2%). Detection limits obtained were lower than the olfactory threshold of the studied compounds, being similar or even lower than previously reported with the advantage of reducing the extraction time. The analysis of real wine samples demonstrated the applicability of the method. To our knowledge, this is the first time that VALLME has been applied for the simultaneous determination of haloanisoles and halophenols in wine.
authors: Department of Chemistry, University of La Rioja, C/ Madre de Dios 51, 26006 Logroño, La Rioja, Spain. Electronic address: consuelo.pizarro@unirioja.es.
authors: C
authors: C
authors: Pizarro
authors: Department of Chemistry, University of La Rioja, C/ Madre de Dios 51, 26006 Logroño, La Rioja, Spain. Electronic address: nuria.perez-del-notario@unirioja.es.
authors: N
authors: N
authors: Pérez-Del-Notario
authors: Department of Chemistry, University of La Rioja, C/ Madre de Dios 51, 26006 Logroño, La Rioja, Spain. Electronic address: alfonso.saenz@alum.unirioja.es.
authors: A
authors: A
authors: Sáenz-Mateo
authors: Department of Chemistry, University of La Rioja, C/ Madre de Dios 51, 26006 Logroño, La Rioja, Spain. Electronic address: josemaria.gonzalez@unirioja.es.
authors: J M
authors: JM
authors: González-Sáiz
mesh_terms: D000840:Anisoles / Q000032:analysis* / Q000302:isolation & purification; D002733:Chlorophenols / Q000032:analysis* / Q000302:isolation & purification; D002849:Chromatography, Gas; D059627:Liquid Phase Microextraction / Q000379:methods*; D015203:Reproducibility of Results; D014920:Wine / Q000032:analysis*
chemical_list: D000840:Anisoles; D002733:Chlorophenols; C015421:pentachloroanisole; C110228:2,4,6-trichloroanisole; C060998:anisole; C484217:2,4,6-tribromoanisole; C024564:2,4,6-trichlorophenol
keywords: Cork taint; Experimental design; Haloanisoles; Halophenols; Vortex assisted liquid–liquid microextraction; Wine