High-Throughput, Sub ng/L Analysis of Haloanisoles in Wines Using HS-SPME with GC-Triple Quadrupole MS

Haloanisole contamination causes development of “cork taint,” a musty off-aroma in affected wines. Cork taint results in significant economic loss for the wine and allied industries every year, therefore extensive quality-control procedures have been established at wineries and cork production facilities to monitor levels of haloanisoles in cork products. Because of the extremely low human sensory thresholds for these compounds (~1 to 4 ng/L for 2,4,6-trichloroanisole in wine), highly sensitive analytical methods are needed to detect the haloanisoles at threshold concentrations or lower. We present a method for the simultaneous analysis of four haloanisoles in wine—2,4,6-trichloroanisole (TCA); 2,3,4,6-tetrachloroanisole (TeCA); 2,3,4,5,6-pentachloroanisole (PCA); and 2,4,6-tribromoanisole (TBA)—that have been frequently associated with cork taint aromas in wines. Headspace solid-phase microextraction (HS-SPME) coupled to a GC-triple quadrupole MS was used to obtain limits of quantification that were ≤1.0 ng/L and below sensory threshold levels. The method is fully automated, requires no sample preparation other than the addition of internal standards, and is high throughput, with a 10-min extraction time and a 5-min incubation prior to extraction. This method can be readily adapted to screen for haloanisoles in cork extracts.