Abstract:

The objective of this study was to develop an analytical method for the determination of 2,4,6-trichloroanisole
(TCA) in wine by headspace solid-phase microextraction combined with gas chromatography-mass spectrometry (HSSPME-
GC-MS). Important extraction parameters such as fiber type, sample volume, extraction temperature, equilibration
time and extraction time were optimize using response surface method with the software Design Expert 7.0. The results
indicated that when polydimethylsiloxane/divinylbenzene (PDMS/DVB, 65 μm) was selected as the extraction fiber, and
optimised parameters for SPME were 9.8 mL of wine, 2 g of NaCl, temperature 33 ℃, equilibration time 10 min and
extraction time 90 min, followed by analysis by GC-MS and quantification using TCA-d5 as internal standard. The presented
method was shown to be adequate for the purpose, with a correlation coefficient R2 of 0.999 9, RSD of 1.03%, and recovery
rates between 95.7% and 106.1%. The limit of detection (LOD) and the limit of quantification (LOQ) were 0.3 and 1 ng/L,
respectively. This method was applied to analyze 7 commercial wine samples and the results revealed that the content of
TCA varied between 0 and 7.6 ng/L, lower in dry white red than in dry red wine. This method is simple and reliable, and can
be applied to the determination of TCA in wine.

Key words: response surface method, headspace solid-phase microextraction, GC-MS, 2,4,6-trichloroanisole, wine