Highly selective solid-phase extraction and large volume injection for the robust gas chromatography–mass spectrometric analysis of TCA and TBA in wines

A reliable solid-phase extraction (SPE) method for the simultaneous determination of 2,4,6-trichloroanisole (TCA) and 2,4,6-tribromoanisole (TBA) in wines has been developed. In the proposed procedure 50 mL of wine are extracted in a 1 mL cartridge filled with 50 mg of LiChrolut EN resins. Most wine...

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Bibliographic Details
Published in:Journal of Chromatography A 2005-09, Vol.1089 (1), p.235-242
Main Authors: Insa, S., Anticó, E., Ferreira, V.
Format: Article
Language:English
Subjects:
2,4,6-Tribromoanisole
2,4,6-Trichloroanisole
Anisoles - analysis
Biological and medical sciences
cork
Cork taint
Fermented food industries
Food industries
Fundamental and applied biological sciences. Psychology
gas chromatography
Gas Chromatography-Mass Spectrometry - methods
Large volume injection
mass spectrometry
odor compounds
odors
organobromine compounds
organochlorine compounds
phenolic compounds
Reproducibility of Results
Sensitivity and Specificity
Solid-phase extraction
taint
Wine
Wine - analysis
wines
Wines and vinegars
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Summary:A reliable solid-phase extraction (SPE) method for the simultaneous determination of 2,4,6-trichloroanisole (TCA) and 2,4,6-tribromoanisole (TBA) in wines has been developed. In the proposed procedure 50 mL of wine are extracted in a 1 mL cartridge filled with 50 mg of LiChrolut EN resins. Most wine volatiles are washed up with 12.5 mL of a water:methanol solution (70%, v/v) containing 1% of NaHCO 3. Analytes are further eluted with 0.6 mL of dichloromethane. A 40 μL aliquot of this extract is directly injected into a PTV injector operated in the solvent split mode, and analysed by gas chromatography (GC)–ion trap mass spectrometry using the selected ion storage mode. The solid-phase extraction, including sample volume and rinsing and elution solvents, and the large volume GC injection have been carefully evaluated and optimized. The resulting method is precise (RSD (%) < 6% at 100 ng L −1), sensitive (LOD were 0.2 and 0.4 ng/L for TCA and TBA, respectively), robust (the absolute recoveries of both analytes are higher than 80% and consistent wine to wine) and friendly to the GC–MS system (the extract is clean, simple and free from non-volatiles).
ISSN:0021-9673
DOI:10.1016/j.chroma.2005.06.061