Development of an Ultrasound-Assisted Emulsification Microextraction Method for the Determination of Volatile Compounds in Wines

Abstract

A fast and simple method based on ultrasound-assisted emulsification microextraction (USAEME) was developed for the analysis of volatile compounds in wines. A full factorial 24 screening design was built to investigate the main factors affecting the extraction of volatile components, namely the volume of extraction solvent, sonication time, salt content, and pH. Then, the factors with significant effects were optimized using an I-optimal design. The optimal value for all the variables studied was reached under the following experimental conditions: volume of extraction solvent 200 μL and salt content 5% m/v. The suitability of the optimized method was evaluated, resulting in very good linearity with coefficients of determination (R2) higher than 0.995 in all cases, while repeatability was lower than 8.4% except for d-limonene and p-cymene. Recoveries higher than 82% were observed for the groups of ethyl esters, acetate esters, alcohols, and terpenoid alcohols (linalool, α-terpineol). The recovery of acids ranged from 70.5% to 88.9%, whereas the three monoterpenes studied (d-limonene, γ-terpinene, p-cymene) were not extracted satisfactorily. The proposed method was effectively applied for the analysis of volatile compounds in laboratory-scale fermentations with selected strains of Saccharomyces cerevisiae.

Keywords

• ultrasound-assisted emulsification microextraction
• GC-FID
• experimental design
• response surface methodology
• volatile compounds
• wine