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

  1. Pizarro, C. 1
  2. Sáenz-González, C. 1
  3. Perez-del-Notario, N. 1
  4. González-Sáiz, J.M. 1
  1. 1 Universidad de La Rioja

    Universidad de La Rioja

    Logroño, España

    GRID grid.119021.a

Journal of Chromatography A

ISSN: 0021-9673

Year of publication: 2010

Volume: 1217

Issue: 49

Pages: 7630-7637

Type: Article

Export: RIS
DOI: 10.1016/j.chroma.2010.10.032 PMID: 21035812 SCOPUS: 2-s2.0-78249254256 WoS: 000284672500002 GOOGLE SCHOLAR


Cited by

  • Scopus Cited by: 47 (12-11-2021)

JCR (Journal Impact Factor)

  • Year 2010
  • Journal Impact Factor: 4.194
  • Best Quartile: Q1
  • Area: CHEMISTRY, ANALYTICAL Quartile: Q1 Rank in area: 7/73 (Ranking edition: SCIE)
  • Area: BIOCHEMICAL RESEARCH METHODS Quartile: Q1 Rank in area: 17/71 (Ranking edition: SCIE)

SCImago Journal Rank

  • Year 2010
  • SJR Journal Impact: 2.234
  • Best Quartile: Q1
  • Area: Analytical Chemistry Quartile: Q1 Rank in area: 8/103
  • Area: Biochemistry Quartile: Q1 Rank in area: 50/393
  • Area: Organic Chemistry Quartile: Q1 Rank in area: 13/174
  • Area: Medicine (miscellaneous) Quartile: Q1 Rank in area: 101/2905


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 μL of carbon tetrachloride, 75 μL 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. © 2010 Elsevier B.V.