Optimisation of a simple and reliable method based on headspace solid-phase microextraction for the determination of volatile phenols in beer

  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 Chromatography A

ISSN: 0021-9673

Year of publication: 2010

Volume: 1217

Issue: 39

Pages: 6013-6021

Type: Article

Export: RIS
DOI: 10.1016/j.chroma.2010.07.021 PMID: 20728896 SCOPUS: 2-s2.0-77956263551 WoS: 000282196700001 GOOGLE SCHOLAR


Cited by

  • Scopus Cited by: 39 (14-07-2021)

Journal Citation Reports

  • Year 2010
  • Journal Impact Factor: 4.194
  • Best Quartile: Q1
  • Area: BIOCHEMICAL RESEARCH METHODS Quartile: Q1 Rank in area: 17/71 (Ranking edition: SCIE)
  • Area: CHEMISTRY, ANALYTICAL Quartile: Q1 Rank in area: 7/73 (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 simple, accurate and sensitive method based on headspace solid-phase microextraction (HS-SPME) coupled to gas chromatography-tandem mass spectrometry (GC-MS/MS) was developed for the analysis of 4-ethylguaiacol, 4-ethylphenol, 4-vinylguaiacol and 4-vinylphenol in beer. The effect of the presence of CO2 in the sample on the extraction of analytes was examined. The influence on extraction efficiency of different fibre coatings, of salt addition and stirring was also evaluated. Divinylbenzene/carboxen/polydimethylsiloxane was selected as extraction fibre and was used to evaluate the influence of exposure time, extraction temperature and sample volume/total volume ratio (Vs/Vt) by means of a central composite design (CCD). The optimal conditions identified were 80°C for extraction temperature, 55min for extraction time and 6mL of beer (Vs/Vt 0.30). Under optimal conditions, the proposed method showed satisfactory linearity (correlation coefficients between 0.993 and 0.999), precision (between 6.3% and 9.7%) and detection limits (lower than those previously reported for volatile phenols in beers). The method was applied successfully to the analysis of beer samples. To our knowledge, this is the first time that a HS-SPME based method has been developed to determine simultaneously these four volatile phenols in beers. © 2010 Elsevier B.V.