Control of halophenol and haloanisole concentration in wine cellar environments, wines, corks and wood staves using gas chromatography with mass spectrometry

Background and Aims The presence of halophenol (HP) and haloanisole (HA) compounds in wine cellar environments, in products in contact with wine production, and consequently in wines is responsible for substantial economic losses to the industry. Their assessment is therefore of a great interest for wine producers. The aim of this study was to develop a rapid and sensitive analytical method for the simultaneous determination of 22 HPs and HAs in wine cellar atmospheres, as well as in corks, wooden staves and wines. Methods and Results A rapid solid liquid extraction method assisted by ultrasound was applied to isolate the analytes from solid samples, and dispersive liquid–liquid microextraction was used for preconcentration purposes. The enriched extracts were analysed by gas chromatography–mass spectrometry. Variables related with the dispersive liquid–liquid microextraction procedure and the derivatisation of HPs by in situ acetylation were optimised using multivariable approaches based on central composite designs. The optimised method provides a detection limit of between 0.006 and 0.05 ng/mL (0.02 and 0.2 ng/g, for solid samples) and enrichment factors in the 125- to 300-fold range. Conclusions The analytical characteristics of the method make it a valuable tool for the routine monitoring of HPs and HAs in wine cellar facilities. Significance of the Study The unequivocal quantification of the 22 analytes studied allows wine producers to control the appearance of cork taint and hence the quality of their products.