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A simple and sensitive method was developed and validated to simultaneously separate and determine the 2‐Methoxy‐3,5‐dimethylpyrazine, 2‐Isopropyl‐3‐methoxypyrazine, guaiacol, 2‐Isobutyl‐3‐methoxypyrazine, 2‐Methylisoborneol, geosmin, 2,4,6‐Trichloroanisole, 2,3,4,6‐Tetrachloroanisole, 2,4,6‐Tribromoanisole and Pentachloroanisole in cork stoppers via headspace solid‐phase microextraction (HS‐SPME) coupled with gas chromatography tandem mass spectrometry (GC–MS/MS). The influence of the fibre coating used, the extraction times and temperatures, the sodium chloride additions and the desorption temperatures were investigated. Once done, the optimial HS‐SPME conditions established were divinylbenzene/carboxenpolydimethylsiloxane/polydimethylsiloxane (DVB/CAR/PDMS) fibres, a 50°C extraction temperature, 60‐min extraction time, an ionic strength of 3‐g sodium chlorid and a 290°C desorption temperature. The method showed a good linearity (R2 ≥ 0.994) within the tested range (from 0.1 to 50 ng L−1) for all the compounds. Using TCA‐d10 and MIB‐d3 as internal standards the precision, expressed as repeatability and reproducibility RSD, was <10% in both. Note that the limits of quantifications (LOQs) are below the sensory threshold levels for such compounds in water and wine. Good recoveries were obtained for cork macerates (from 100.4% to 126%) and when compared with other reported methods using HS‐SPME in water and cork stopper samples, the present method had more analytes with the lowest limit of detection for most of the targeted compounds, along with good precision and recovery.

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Compounds 2,4,6-trichloroanisole (TCA), 2,3,4,6-tetrachloroanisole (TeCA), 2,4,6-tribromoanisole (TBA) and pentachloroanisole (PCA), 2-methylisoborneol (2MIB) and geosmin (GSM) have been reported as being responsible for cork and wine taint. A sustainable method based on thermal desorption-gas chromatography–mass spectrometry (TD-GC/MS) has been developed and optimized, taking into account desorption parameters and chromatographic and mass spectrometric conditions. The combination of parameters that jointly maximized the compound detection was as follows: desorption temperature at 300 °C, desorption time at 30 min, cryo-temperature at 20 °C and trap high temperature at 305 °C. The proposed methodology showed a good linearity (R ≤ 0.994) within the tested range (from 0.1 to 2 ng) for all target compounds. The precision expressed as repeatability and reproducibility was RSD < 10% in both. The limits of quantification ranged from 0.05 to 0.1 ng. The developed methodology and the sampling rates (R-values) of all targeted compounds (from 0.013 to 0.071 m3 h−1) were applied to the air analysis of two wineries. The results showed that the developed methodology is a sustainable and useful tool for the determination of these compounds in air.