| Abstract
| - A headspace solid-phase microextraction (HS-SPME) procedure at 30 °C with a 100 μm PDMS fiberof a saturated NaCl solution stirred at 1100 rpm combined to GC-ECD for the 2,4,6-trichloroanisol(TCA) determination in wines has been developed. Due to the matrix complexity and ethanol absorptioninto the fiber, the internal standard selection was crucial to obtain unbiased results. Thus, matrixeffects were observed when analyzing different types of Spanish wines (white, early, and vintagered wines) spiked with TCA at low concentration levels (i.e., <40 ng L-1). In contrast, the use of2,4,6-tribromoanisole (TBA) as internal standard overcame these matrix effects, whereas the use of2,4,6-trichlorophenyl ethyl ether led to inconsistent results. The developed HS-SPME-GC-ECDmethodology reaches a limit of quantitation for TCA in wine within 2.9−18 ng L-1, with a relativestandard deviation of 2.5−13.4%, depending on the TCA concentration level and wine characteristics.This analytical method is comparable to the existing methodologies based on HS-SPME followed byGC-MS in terms of accuracy, precision, length of determination, and length of quantification; however,analysis cost is reduced. Keywords: SPME-headspace; TCA; GC-ECD; internal standard selection; wine; matrix effect; mustyodor
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