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

Abstract

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 ml1 and method detection limit 0.0083 ng ml1 which is well below the odour threshold of 0.04 ng ml1 . Recoveries at 0.04, 0.2 and 0.8 ng ml1 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.