Articulo Determinación De Volátiles En Bebidas

Journal of Chromatography A, 1216 (2009) 2881–2890

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Journal of Chromatography A
journal homepage: www.elsevier.com/locate/chroma

Determination of volatile compounds in Brazilian distilled cachaca by using ¸ comprehensive two-dimensional gas chromatography and effects of production pathways
Patterson P. de Souza a , Zenilda de L. Cardeal a,∗ ,Rodinei Augusti a , Paul Morrison b , Philip J. Marriott b,∗∗
a b

Chemistry Department, ICEx, Federal University of Minas Gerais, Av. Antônio Carlos 6627, Belo Horizonte 31270-901, MG, Brazil Australian Centre of Research Separation Science, RMIT University, School of Applied Sciences, GPO Box 2476 V, Melbourne 3001, Australia

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Comprehensivetwo-dimensional gas chromatography (GC × GC) was applied to the study of cachaca pro¸ duction. Effects of bidistillation, and the use of charcoal filtration in the production of artisan cachaca, ¸ as well as the effects of multi-distillation on volatile products in commercial cachaca were investigated. ¸ Volatile compounds were collected and concentrated onto a polyacrylate solid-phase microextractionfibre, and analyzed using GC × GC on a non-polar (BPX5)–polar (BP20) column set. More than 100 compounds, comprising various homologous series were tentatively identified using MS library matching and comparison with retention indices. Phthalate organic contamination following the use of ion exchange resin for removal of copper ion was evident. Charcoal successfully removes this contamination product.Prediction of compounds within particular homologous series aids component identification. © 2008 Elsevier B.V. All rights reserved.

Article history: Available online 19 October 2008 Keywords: Cachaca ¸ Comprehensive two-dimensional gas chromatography TOF-MS SPME Retention index Phthalate contamination

1. Introduction Cachaca, which is obtained from sugarcane, is the third most ¸ consumeddistilled alcoholic beverage (after vodka and soju) in the world. Whilst approximately 1.3 billion litres of cachaca is pro¸ duced per year in Brazil [1,2], only 0.5% is exported. In the past, due to the poor quality of the cachaca product, it was sold at a low ¸ price. However in recent times, it may command close to US$120/L for the more elaborate cachaca brands, due to improved produc¸ tiontechnology. To increase the quality as well as the aggregate value of the beverage, modifications in the steps of production or post-production procedures have been incorporated following the experience of production of other beverages, such as whisky or vodka. Usually, manufacturers of artisan cachaca use physical filters to ¸ remove solid impurities from the casks. In addition, use of an ion exchangeresin after the alembic distillation to reduce copper content and a charcoal filter to reduce the acid content is reported in the industry.

∗ Corresponding author. ∗∗ Corresponding author. Tel.: +61 3 99252632. E-mail addresses: zenilda@ufmg.br (Z.d.L. Cardeal), philip.marriott@rmit.edu.au (P.J. Marriott). 0021-9673/$ – see front matter © 2008 Elsevier B.V. All rights reserved.doi:10.1016/j.chroma.2008.10.061

In a typical production, each 100 L of heart portion (the main distillation objective), accompanies 30 L of other less valuable fractions (the head + tail portions). In the final production, the total amount of (head + tail) is too large a volume to be simply discarded. One possible solution is to re-distill the (head + tail) fractions and combine this with product from the heartfraction and thereby increase the overall production yield. Distilled beverages – whisky, tequila, cachaca and others – ¸ consist of exceedingly complex mixtures of many different compounds. For whisky samples, more than 1000 compounds were reportedly identified [3] and other authors suggest 800 volatile compounds, several tens of which can have odour-impact [4]. This large number of compounds...