Available online at www.sciencedirect.com Journal of Chromatography A, 1185 (2008) 23–30 Determination of phenolic compounds in wines by novel matrix solid-phase dispersion extraction and gas chromatography/mass spectrometry Lucio Minuti ∗ , Roberto Pellegrino Dipartimento di Chimica, Universit` a degli Studi di Perugia, Via Elce di Sotto 8, 06123 Perugia, Italy Received 20 November 2007; received in revised form 14 January 2008; accepted 17 January 2008 Available online 20 January 2008 Abstract A novel matrix solid-phase dispersion (MSPD) extraction method was developed to extract simultaneously 23 phenolic compounds from wine samples prior to determination by gas chromatography with mass spectrometric detection in the selected ion monitoring mode. Different parameters of the MSPD technique such as dispersant solid-phase, eluting solvent, and sample ionic strength and pH were optimized. The optimized MSPD procedure requires a small volume of wine (1 mL), commercial silica gel (1.5 g) as dispersant solid-phase and a small volume of ethyl acetate (5 mL) as eluting solvent. Under these conditions, the extraction of the studied compounds was almost complete (mean values of recoveries between 87 and 109%) in a short time (15 min). Moreover, satisfactory standard deviations of repeatability (RSD < 9% in most cases), linear regression coefficients (r 2 > 0.993) and detection limits (<8 g/L) confirm the usefulness of the methodology for routine monitoring of the concentration of individual phenolic antioxidants in wines. Application was illustrated by analysis of different wine samples. © 2008 Elsevier B.V. All rights reserved. Keywords: GC/MS–SIM; Extraction method; Phenols; Wines; Analysis 1. Introduction Polyphenols are a group of compounds that are widespread in both raw and processed foods [1–3]. Grapes and grape prod- ucts such as wine, particularly red wine, contain large amounts of phenolic compounds, especially flavonoids and hydroxybenzoic and hydroxycinnamic acids. Some phenolic compounds have been reported to have health benefits in view of their antioxidant activity, which may help to reduce the risk of cardiovascular dis- eases. Others, such as resveratrol, gallic acid and quercitin have been claimed to have activity against allergies, inflammation, hypertension, arthritis and carcinogens [4–15]. Phenolic compounds also contribute to wine characteristics such as the sensory properties, color stability, astringency and bitterness. Furthermore, due to their structure, which include ∗ Corresponding author at: Dipartimento di Chimica, Sezione di Chimica Organica, Universit` a degli Studi di Perugia, Via Elce di Sotto 8, 06123 Perugia, Italy. Tel.: +39 075 5785545; fax: +39 075 5785560. E-mail address: lucio@unipg.it (L. Minuti). OH groups, phenolic compounds are responsible for oxidation processes and other chemical reactions and play an important role in the whole winemaking technology from grape to wine [16–21]. Therefore, it is very important to have a rapid, sensitive and accurate analytical method to assay both qualitatively and quan- titatively a large number of phenolic compounds in wine. Reversed-phase, high-performance liquid chromatography (RP-HPLC) with diode array detection (DAD), fluorescence detection (FD) and electrochemical detection (ED) [22–32] and gas chromatography (GC) with mass spectrometry (MS) detec- tion [33–40] are the most widely employed analytical methods for detecting and quantifying these compounds in wines. Whereas, recent HPLC methods are based mostly on direct injection of the sample without any purification, the GC–MS methods require liquid–liquid extraction (LLE) or solid-phase extraction (SPE) to clean-up the sample followed by derivatiza- tion of the target compounds prior to the GC analyses. However, the high resolution and great sensitivity make the GC–MS meth- ods very attractive for the identification and quantification of individual phenolic compounds in wines. 0021-9673/$ – see front matter © 2008 Elsevier B.V. All rights reserved. doi:10.1016/j.chroma.2008.01.039