Fifteen aroma compounds have been determined in their free and glycosylated forms in grapes using dispersive liquid-liquid microextraction with gas chromatography-mass spectrometry. The sample treatment includes a previous solid-liquid extraction stage and subsequent parallel microextraction approaches to preconcentrate total aroma content and the free fraction. Thus, the extraction of the total content of analytes requires previous enzymatic hydrolysis of the bound forms. For preconcentration, chloroform (250 μl) and acetonitrile (1.5 ml) were added to 10 ml of the sample extract in the presence of 0.5 g sodium chloride. The absence of matrix effect in the samples allowed quantification against aqueous external standards. Limits of detection ranged between 5 and 30 ng/g, depending on the compound. Method accuracy was studied through recovery assays, with recoveries in the 82-115% range being obtained. Relative standard deviations for repeatability studies were lower than 12%. Four different samples of grapes were analyzed, being quantified linalool in its free form at concentrations in the 359-470 ng/g range, and benzyl alcohol, 2-phenylethanol, and linalool oxide I and II in their bound forms between 52 and 464 ng/g.
Keywords: aroma compounds; dispersive liquid-liquid microextraction; gas chromatography-mass spectrometry; glycosides; grape.
© 2022 The Authors. Journal of Separation Science published by Wiley-VCH GmbH.