923 (2001) 205–214 Journal of Chromatography A, www.elsevier.com / locate / chroma Fast analysis of important wine volatile compounds Development and validation of a new method based on gas chromatographic–flame ionisation detection analysis of dichloromethane microextracts * ´ Catalina Ortega, Ricardo Lopez, Juan Cacho, Vicente Ferreira Department of Analytical Chemistry, Faculty of Sciences, University of Zaragoza, 50009 Zaragoza, Spain Received 20 March 2001; received in revised form 8 May 2001; accepted 10 May 2001 Abstract A method for the simultaneous determination of major (10–200 mg/l) and minor (0.1–10 mg/l) volatile compounds from wine has been optimised and validated. A 3-ml volume of wine is diluted with water (7 ml), salted with 4.5 g of ammonium sulfate and extracted with 0.2 ml of dichloromethane. The extract is injected in the split mode in a GC system, separated on a Carbowax 20M capillary column and detected by flame ionisation detection.Volatiles from wine are divided into four groups according to their behaviour in the extraction, and a specific internal standard has been selected for each group. The method allows satisfactory determination of more than 30 volatile compounds of wine. Compounds analysed include acetaldehyde, diacetyl, acetoine (3-hydroxy butanone), fusel alcohols and their acetates, and fatty acids and their ethyl esters. The linear dynamic range of the method covers the normal range of occurrence of analytes in wine and extends from at least one 2 magnitude order to more than two, with typical r between 0.9938 and 0.9998. Reproducibility ranges from 3.1 to 10% (as RSD) with 5.5% as the average. The analysis of spiked samples has shown that matrix effects do not significantly affect method performance.  2001 Elsevier Science B.V. All rights reserved. Keywords: Wine; Food analysis; Volatile organic compounds 1. Introduction extremely complex and expensive. The best example of such analysis can be found in the work by Guth The gas chromatographic analysis of volatile [8] who, by using isotopomers, complex sample compounds in wine is a very important tool useful preparation schemes, and more than eight gas chro- for wine classification [1–3], for quality control [4– matography–mass spectrometry (GC–MS) runs, was 7] or for understanding wine sensory properties [8,9]. able to accurately quantify 43 odor-active com- The complete analysis of wine aroma is, however, pounds from wine. There is no need to carry out such a complex analysis to gain a big deal of information. A single GC–flame ionisation detection *Corresponding author. Tel.: 134-976-762-067; fax: 134-976- (FID) chromatogram from a wine extract can pro- 761-292. E-mail address: vferre@posta.unizar.es (V. Ferreira). vide quantitative data on compounds formed in 0021-9673 / 01 / $ – see front matter  2001 Elsevier Science B.V. All rights reserved. PII: S0021-9673(01)00972-4