Development of a methodology based on headspace solid-phase microextraction coupled to gas chromatography-mass spectrometry for the analysis of esters in brandies.

A specific method for the simultaneous quantification of 28 esters in brandies using headspace solid-phase microextraction and gas-chromatography coupled to mass spectrometry (HS-SPME-GC-MS) was optimised and validated. First, the optimal extraction conditions were determined by using response surface methodology, which were obtained for an extraction temperature of 33 °C for 55 min and a sample dilution of 7.2 % v/v ethanol. Eight deuterated ethyl esters were used as internal standards to provide specificity for the method, which was successfully validated in terms of linearity (R² > 0.981), repeatability (1 % < RSD < 30 %), reproducibility (1 % < RSD < 18 %), sensitivity (1.1 μg/L < LOQ < 1878 μg/L), accuracy (81 % < recovery < 118 %), and matrix effect. Then, the optimised method was tested on Spanish sherry brandies matured through the traditional dynamic ageing system of Criaderas and Solera, observing an overall decrease in...