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

Abstract

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.