Multiple headspace solid-phase microextraction for eliminating matrix effect in the simultaneous determination of haloanisoles and volatile phenols in wines

• Published in: Journal of Chromatography A Vol. 1166; no. 1-2; pp. 1 - 8
• Main Authors: Pizarro, C., Pérez-del-Notario, N., González-Sáiz, J.M.
• Format: Journal Article
• Language: English
• Published: Amsterdam Elsevier B.V 28.09.2007; Elsevier
• Subjects: Anisoles - analysis; Biological and medical sciences; Brett; Cork taint; Ethylphenols; Fermented food industries; Food Contamination - analysis; Food industries; Fundamental and applied biological sciences. Psychology; Gas Chromatography-Mass Spectrometry - methods; Haloanisoles; Multiple headspace solid-phase microextraction (MHS-SPME); Phenols - analysis; Solid Phase Microextraction - methods; Solid-phase microextraction (SPME); Tandem Mass Spectrometry - methods; Vinylphenols; Volatilization; Wine; Wine - analysis; Wines and vinegars; Wine; Brett; Vinylphenols; Haloanisoles; Multiple headspace solid-phase microextraction (MHS-SPME); Cork taint; Ethylphenols; Solid-phase microextraction (SPME); Trace analysis; Chemical analysis; Coupled method; Volatile organic compound; Haloether; Off-flavours; Chemical enrichment; Solid phase microextraction; Gas chromatography; Sample preparation; Mass spectrometry MS/MS; Simultaneous measurement; Phenols; Headspace; Quantitative analysis
• ISSN: 0021-9673
• DOI: 10.1016/j.chroma.2007.08.031

This paper proposes a multiple headspace solid-phase microextraction (MHS-SPME) method coupled to gas chromatography–tandem mass spectrometry detection (GC/MS/MS) for the simultaneous determination of 2,4,6-trichloroanisole, 2,3,4,6-tetrachloroanisole, pentachloroanisole, 2,4,6-tribromoanisole, 4-ethylphenol, 4-ethylguaiacol, 4-vinylphenol and 4-vinylguaiacol in wines. These compounds are involved in the presence of “cork taint” and Brett character in wines. The MHS-SPME method is a modification of SPME developed for quantitative analysis that avoids possible matrix effects based on an exhaustive analyte extraction from the sample. After demonstrating the existence of matrix effect in the analysis of the target compounds by HS-SPME with a divinylbenzene/Carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fibre, the MHS-SPME method was developed and validated. The proposed method showed satisfactory linearity, precision and detection limits, all below the odour detection thresholds of the compounds in wine matrices. Good recoveries were observed for all compounds, always above 90%, and the repeatability obtained was considered acceptable, ranging between 2 and 11%. After checking the applicability of the method by comparing the results recorded with those obtained with the standard addition method, the method was applied successfully to the analysis of wine samples. To our knowledge, this is the first time that MHS-SPME combined with GC/MS/MS has been applied to simultaneously determine haloanisoles and volatile phenols in wine.