Headspace solid-phase microextraction for direct determination of volatile phenols in cider

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

    Universidad de La Rioja

    Logroño, España

    GRID grid.119021.a

Journal of Separation Science

ISSN: 1615-9306

Year of publication: 2009

Volume: 32

Issue: 21

Pages: 3746-3754

Type: Article

Export: RIS
DOI: 10.1002/jssc.200900347 SCOPUS: 2-s2.0-76649107392 WoS: 000273993400023 GOOGLE SCHOLAR


Cited by

  • Scopus Cited by: 16 (14-07-2021)

Journal Citation Reports

  • Year 2009
  • Journal Impact Factor: 2.551
  • Best Quartile: Q2
  • Area: CHEMISTRY, ANALYTICAL Quartile: Q2 Rank in area: 22/70 (Ranking edition: SCIE)

SCImago Journal Rank

  • Year 2009
  • SJR Journal Impact: 1.401
  • Best Quartile: Q1
  • Area: Analytical Chemistry Quartile: Q1 Rank in area: 14/96
  • Area: Filtration and Separation Quartile: Q1 Rank in area: 2/18


A headspace solid-phase microextraction coupled to gas chromatography- tandem mass spectrometry (GC-MS/MS) method was optimised and validated for the determination of 4-ethylguaiacol, 4-ethylphenol, 4-vinylguaiacol and 4-vinylphenol, involved in the presence of Brett character, in ciders. The influence of different parameters on extraction efficiency (fibre coating, salt addition, exposure time, extraction temperature and sample volume/ total volume ratio) was evaluated. Divinylbenzene/carboxen/PDMS was selected as extraction fibre and the other optimised parameters were as follows: 10 mL of cider, temperature 70°C, extraction time 60 min and addition of 0.4 g/mL of NaCl. The proposed method showed satisfactory linearity. The detection limits obtained were 0.01 μg/L for 4-ethylguaiacol, 0.02 μg/L for 4-ethylphenol, 0.08 μg/L for 4-vinylguaiacol and 0.03 μg/L for 4-vinylphenol. These detection limits were lower than those obtained in previous studies on the determination of volatile phenols in other alcoholic beverages. Good recoveries of over 95% were observed for all compounds, and the repeatability obtained was considered acceptable, ranging between 4 and 10%. To demonstrate the feasibility of the procedure, the method was applied to the analysis of commercial ciders. To our knowledge, this is the first time that the headspace solid-phase microextraction procedure has been optimised to determine specifically the Brett character responsible compounds in cider. © 2009 Wiley-VCH Verlag GmbH & Co. KGaA.