G. Botelho1,2, C. Paulino1, A. Mendes-Faia2, M. C. Clímaco1
1INIA Estação Vitivinícola Nacional, 2565-191 Dois Portos. Portugal. E-mail: evn.mcclimaco@mail.net4b.pt
2Centro de Genética e Biotecnologia, Universidade de Trás-os-Montes e Alto Douro, 5000-911 Vila Real. Portugal.
(Manuscrito recebido em 04.06.07. Aceite para publicação em20.07.07.)
SUMMARY
]]> A method to study the glycosidically bound fractions in red grape juice was developed. Bound fractions were fractionated by solid-liquid chromatography on LiChroprep RP-18. The release of free aglycones was achieved by acid hydrolysis. In a preliminary approach the acid hydrolysis was performed at pH 1.0 and pH 3.0 levels. The pH 3.0 was selected in this study mainly due to its similarity with the pH levels that occur naturally in juices and grapes. Nine extractions of the same juice sample were carried out to study the repeatability of the method at pH 3.0. All the extracts were analysed by GC-MS and GC-FID. The repeatability found in the various quantified components in all extracts of the bound fraction of juice is expressed by their coefficient of variation, which varied in the range between 11.5% and 24.7%. Four aglycones, trans-furan linalool oxide, cis-furan linalool oxide, vitispirane, and ß-damascenone were quantified after pH 3.0 hydrolysis.Key words: glycosidically bound compounds, LiChroprep RP-18, acid hydrolysis, red grape juice
RESUMO
Um método para dosear os componentes ligados do aroma em sumos de uvas tintas não aromáticas
Desenvolveu-se um método para estudar as fracções ligadas glicosidicamente em sumos de uva tintas. As fracções ligadas foram fraccionadas por cromatografia sólido-líquido utilizando resina RP-18. A libertação das aglíconas foi realizada por hidrólise ácida. Numa abordagem preliminar a hidrólise ácida foi efectuada a pH 1.0 e pH 3.0. Seleccionou-se o pH 3.0, principalmente, devido à sua similaridade com os valores de pH que ocorrem naturalmente nos sumos e nas uvas. No estudo da repetibilidade do método com hidrólise a pH 3.0 realizaram-se nove extracções de uma amostra de sumo. Todos os extractos foram analisados por GC-MS e GC-FID. A repetibilidade, expressa pelo coeficiente de variação, encontrada nos diversos compostos quantificados, em todos os extractos da fracção ligada do sumo, variou entre 11.5% e 24.7%. Após hidrólise a pH 3.0, foram quantificadas quatro aglíconas: trans-óxido furânico de linalol, cis-óxido furânico de linalol, vitispirano e ß-damascenona.
Palavras-chave: compostos ligados glicosidicamente, LiChroprep RP-18, hidrólise ácida, sumo de uva tinta
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