Development and validation of a simple analytical method for the determination of 2,4,6-trichloroanisole in wine by GC–MS

A novel method for the residue analysis of wine spoilage compound 2,4,6-trichloroanisole is reported. Wine (60 ml) was extracted with 2 ml toluene in presence of 24 g MgSO4 and 6 g NaCl. Cleanup of the toluene phase by dispersive solid phase extraction with mixture of 100 mg CaCl2, 25 mg primary secondary amine and 50 mg MgSO4 was effective in minimising co-extractives and matrix effects. Time-of-flight and tandem mass spectrometric parameters were optimised to achieve linearity over 0.25–500 ng ml−1 and method detection limit 0.0083 ng ml−1 which is well below the odour threshold of 0.04 ng ml−1. Recoveries at 0.04, 0.2 and 0.8 ng ml−1 were within 80–110% (±8%). The method was reproducible when tested for Argentinean wines with intra-laboratory Horwitz ratios being <0.20 in white and red wines at both the laboratories of India and Argentina. The method could be successfully applied for incurred wine samples.