PMID- 21035812 OWN - NLM STAT- MEDLINE DCOM- 20110203 LR - 20151119 IS - 1873-3778 (Electronic) IS - 0021-9673 (Linking) VI - 1217 IP - 49 DP - 2010 Dec 3 TI - Optimisation of a dispersive liquid-liquid microextraction method for the simultaneous determination of halophenols and haloanisoles in wines. PG - 7630-7 LID - 10.1016/j.chroma.2010.10.032 [doi] AB - A dispersive liquid-liquid microextraction (DLLME) method has been optimised for simultaneously extracting 2,4,6-trichloranisole (TCA), 2,3,4,6-tetrachloroanisole (TeCA), 2,4,6-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 muL of carbon tetrachloride, 75 muL 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. CI - Copyright (c) 2010 Elsevier B.V. All rights reserved. FAU - Pizarro, C AU - Pizarro C AD - Department of Chemistry, University of La Rioja, C/Madre de Dios 51, 26006 Logrono, La Rioja, Spain. consuelo.pizarro@unirioja.es FAU - Saenz-Gonzalez, C AU - Saenz-Gonzalez C FAU - Perez-del-Notario, N AU - Perez-del-Notario N FAU - Gonzalez-Saiz, J M AU - Gonzalez-Saiz JM LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20101013 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Acetic Anhydrides) RN - 0 (Anisoles) RN - 0 (Chlorophenols) RN - 0 (Phenols) RN - 1364PS73AF (Acetone) RN - 2E48G1QI9Q (acetic anhydride) RN - 451W47IQ8X (Sodium Chloride) RN - CL2T97X0V0 (Carbon Tetrachloride) RN - YS6K3EU393 (2,4,6-tribromophenol) SB - IM MH - Acetic Anhydrides MH - Acetone MH - Anisoles/*analysis/chemistry MH - Carbon Tetrachloride MH - Chemical Fractionation/*methods MH - Chlorophenols/*analysis/chemistry MH - Chromatography, Gas MH - Models, Chemical MH - Phenols/*analysis/chemistry MH - Reproducibility of Results MH - Sodium Chloride MH - Temperature MH - Wine/*analysis EDAT- 2010/11/03 06:00 MHDA- 2011/02/04 06:00 CRDT- 2010/11/02 06:00 PHST- 2010/07/27 00:00 [received] PHST- 2010/10/04 00:00 [revised] PHST- 2010/10/05 00:00 [accepted] PHST- 2010/11/02 06:00 [entrez] PHST- 2010/11/03 06:00 [pubmed] PHST- 2011/02/04 06:00 [medline] AID - S0021-9673(10)01395-6 [pii] AID - 10.1016/j.chroma.2010.10.032 [doi] PST - ppublish SO - J Chromatogr A. 2010 Dec 3;1217(49):7630-7. doi: 10.1016/j.chroma.2010.10.032. Epub 2010 Oct 13.