Development of an ultrasound-assisted emulsification-microextraction method for the determination of the main compounds causing cork taint in wines

  1. Pizarro, C. 1
  2. Sáenz-González, C. 1
  3. Pérez-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: 2012

Volume: 1229

Issue: 1229

Pages: 63-71

Type: Article

Export: RIS
DOI: 10.1016/j.chroma.2012.01.033 SCOPUS: 2-s2.0-84857141286 WoS: 000301606600009 GOOGLE SCHOLAR


In this work, an ultrasound-assisted emulsification-microextraction method has been optimised for the determination in wine of haloanisoles (2,4,6-trichloranisole (TCA), 2,3,4,6-tetrachloroanisole (TeCA), 2,4,6-tribromoanisole (TBA) and pentachloranisole (PCA)) responsible for the so-called cork taint. Their halophenolic precursors (2,4,6-trichlorophenol (TCP), 2,3,4,6-tetrachlorophenol (TeCP), 2,4,6-tribromophenol (TBP) and pentachlorophenol (PCP)) have also been simultaneously determined. For this purpose, parameters affecting the USAEME-derivatisation procedure were exhaustively investigated. Firstly, extraction solvent, basic conditions and extraction time were selected to, subsequently, employ experimental design methodology for the simultaneous optimisation of the volumes of acetic anhydride and extraction solvent, temperature and ionic strength conditions. Once optimised, the evaluation of the analytical performance of the method confirmed its suitability for the determination of the studied compounds in wines. The proposed method showed satisfactory linearity (correlation coefficients over 0.981), repeatability (below 10.9%) and inter-day precision (below 11.0%). Detection limits obtained were similar or even lower than previously reported. In addition, the proposed method was successfully applied to the analysis of real samples. To our knowledge, this is the first time that USAME method has been optimised for the simultaneous determination of haloanisoles and halophenols in wine. © 2012 Elsevier B.V.