Accurate Determination of 2,4,6-Trichloroanisole in Wines at Low Parts Per Trillion by Solid-Phase Microextraction Followed by GC-ECD

Abstract

A headspace solid-phase microextraction (HS-SPME) procedure at 30 degrees C with a 100 microm PDMS fiber of 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 absorption into the fiber, the internal standard selection was crucial to obtain unbiased results. Thus, matrix effects were observed when analyzing different types of Spanish wines (white, early, and vintage red wines) spiked with TCA at low concentration levels (i.e., <40 ng L(-)(1)). In contrast, the use of 2,4,6-tribromoanisole (TBA) as internal standard overcame these matrix effects, whereas the use of 2,4,6-trichlorophenyl ethyl ether led to inconsistent results. The developed HS-SPME-GC-ECD methodology reaches a limit of quantitation for TCA in wine within 2.9-18 ng L(-)(1), with a relative standard 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 by GC-MS in terms of accuracy, precision, length of determination, and length of quantification; however, analysis cost is reduced.

Simultaneous headspace solid phase microextraction analysis of off‐flavour compounds from Quercus suber L. cork

“…These results are in agreement with previous studies 19,35 and may be due to the high Henry's constant of TCA (130 atm cm 3 mol −1 ). At 30…”

Optimisation of the derivatisation reaction and subsequent headspace solid-phase microextraction method for the direct determination of chlorophenols in red wine

“…Although SPME methods have also been applied to analyse various components, off-flavours and contaminants in wine samples (i.e. volatile components, sulphur aroma, diacetyl, methylisothiocyanate, pesticides, chloroanisoles) [42][43][44][45][46], to our knowledge, no SPME-based method has been applied in the analysis of chlorophenols in wine samples.…”

A rapid space-resolved solid-phase microextraction method as a powerful tool to determine contaminants in wine based on their volatility

“…In SPME, the extraction of target analytes from sample matrix to the fiber is conducted either directly, with the coated fiber directly immersed in the liquid sample (direct SPME), or in the headspace (HS-SPME), where the extracting fiber is suspended above the sample. Because of the high volatility of TCA, head space solid-phase microextraction (HS-SPME) (Alzaga, Ortiz, Sanchez-Baeza, Marco, & Bayona, 2003;Lizarraga, Irigoyen, Belsue, & Gonzalez-Penas, 2004;Ozhan et al, 2009;Riu, Mestres, Busto, & Guasch, 2002;Vlachos, Kampioti, Kornaros, & Lyberatos, 2007) has been used for the analysis of TCA in wine.…”