Optimisation of a dispersive liquid-liquid microextraction method for the simultaneous determination of halophenols and haloanisoles in wines

A dispersive liquid-liquid microextraction (DLLME) method has been optimised for simultaneously extracting 2 4 6-trichloranisole (TCA) 2 3 4 6-tetrachloroanisole (TeCA) 24 6-tribromoanisole (TBA) pentachloroanisole (PCA) 2 4 6-trichlorophenol (TCP) 2 3 4 6-tetrachlorophenol (TeCP) 2 4 6-tribromophenol (TBP) and pentachlorophenol (PCP) from wine The haloanisoles and halophenols were automatically determined using a gas chromatography-electron capture detection (GC-ECD) system Derivatisation of halophenols was performed at the same time as DLLME Firstly disperser and extraction solvents salt addition and temperature conditions were selected Then the volume of disperser solvent extraction solvent and derivatisation agent and the percentage of base were optimised by means of a central composite design combined with desirability functions The optimal extraction-derivatisation conditions found were 1 3 mL of acetone 150 mu L of carbon tetrachloride 75 mu L of acetic anhydride and a percentage of base of 0 7% with no salt addition and at room temperature Under these conditions the proposed method showed satisfactory linearity (with correlation coefficients over 0 994) repeatability (below 9 7%) and reproducibility (below 9 9%) Moreover detection limits were lower than the olfactory threshold of the compounds The developed method was successfully applied to the analysis of red wine samples To our knowledge this is the first time that DLLME has been applied to determine cork taint responsible compounds in wine (C) 2010 Elsevier B V All rights reserved