Supercritical fluid extraction of 2,4,6-trichloroanisole from cork stoppers.

2,4,6-Trichloroanisole (TCA) is the compound most often associated with cork taint in wines and has been shown to have a very low sensory threshold ( approximately 5 ng/L in wine). A supercritical fluid extraction (SFE) method for TCA in bark cork stoppers was developed with quantification via gas chromatography-mass spectrometry with selected ion monitoring. Supercritical carbon dioxide functioned as the extracting solvent, and temperature and pressure were optimized for the extraction. The method was validated using the stable isotope (2)H(5)-TCA as the internal standard. Recovery of TCA from spiked corks was found to be within 1-4% of the theoretical concentration with a coefficient of variation ranging from 2.6 to 9.7%. TCA levels in corks pulled from wines described as tainted by experienced judges ranged from 0.13 to 2.11 microg/g of cork. The SFE procedure offers a rapid, quantitative, nearly solvent-free, and automated method for the extraction of TCA from complex solid matrices such as cork.

Analysis of 2,4,6-trichloroanisole in wines using solid-phase microextraction coupled to gas chromatography-mass spectrometry.

Cork taint in wine is a serious problem which is exacerbated by the difficulty of its assessment. Current analytical procedures are costly, time consuming and require the use of large amounts of solvents. We developed and evaluated a rapid method for the detection of the cork taint compound, 2,4,6-trichloroanisole (TCA), in wine samples. The method employs solid-phase microextraction, a solventless, automated sampling procedure, coupled to GC-MS-selected ion monitoring analysis. Quantification is enabled by a fully deuterated [2H5]TCA analog used as an internal standard. Accuracy (+/- 8%), precision (R.S.D. 5-13%), and limit of quantification (5 ng/l) are comparable to existing methods.