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 (60ml) was extracted with 2ml toluene in presence of 24g MgSO4 and 6g NaCl. Cleanup of the toluene phase by dispersive solid phase extraction with mixture of 100mg CaCl2, 25mg primary secondary amine and 50mg MgSO4 was effective in minimising co-extractives and matrix effects. Time-of-flight and tandem mass spectrometric parameters were optimised to achieve linearity over 0.25–500ngml−1 and method detection limit 0.0083ngml−1 which is well below the odour threshold of 0.04ngml−1. Recoveries at 0.04, 0.2 and 0.8ngml−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. [ABSTRACT FROM AUTHOR]