Multivariate optimization of headspace solid-phase microextraction coupled to gas chromatography-mass spectrometry for the analysis of terpenoids in sparkling wines

• Published in: Talanta (Oxford) 2020-02, Vol.208, p.120483-120483, Article 120483
• Main Authors: Muñoz-Redondo, José Manuel, Ruiz-Moreno, María José, Puertas, Belén, Cantos-Villar, Emma, Moreno-Rojas, José Manuel
• Format: Article
• Language: English
• Subjects: Box-Behnken design; GC-MS; Response surface methodology; Sparkling wine; Terpenes; Variable selection
• ISSN: 0039-9140; 1873-3573
• DOI: 10.1016/j.talanta.2019.120483

A headspace solid-phase microextraction coupled to gas-chromatography and mass spectrometry (HS-SPME-GC-MS) was developed and validated for the determination of 26 terpenes in sparkling wines. The use of a Box-Behnken experimental design, together with the desirability function D, allowed the extraction conditions of the method to be optimized. The optimal extraction conditions were found at a dilution ratio of 2:3, the addition of 3.5 g of NaCl, an extraction temperature of 46 °C and an extraction time of 52 min, using the DVB/CAR/PDMS fibre. Afterwards, the analytical method was successfully validated in terms of linearity, matrix effect, limit of detection and quantification, precision and accuracy. To test the developed method, 35 commercial sparkling wines from different grape varieties, geographical regions and ageing times were analysed and their terpenoid profile was monitored. The use of multivariate statistical tools made it possible to highlight differences in the samples related to the terpene profile. Finally, the most important compounds involved in the discrimination of the samples were identified by means of iterative variable selection procedures. [Display omitted] •A HS-SPME-GC-MS was developed for quantification of terpenes in sparkling wines.•Response Surface Methodology was used for optimization of the HS-SPME methodology.•The method was validated in terms of linearity, LOD, LOQ, precision and accuracy.•Andalusian sparkling wines displayed higher contents of terpenes.•Potentiality of Andalusian region was highlighted for the elaboration of sparkling wines.