Development and optimization of a HS-SPME-GC-MS methodology to quantify volatile carbonyl compounds in Port wines
Nathalie Moreira1, Ana Margarida Araújo2, Frank Rogerson3
1UCIBIO@REQUIMTE/Laboratório de Toxicologia, Departamento de Ciências Biológicas, Faculdade de Farmácia, Universidade do Porto, Rua Jorge Viterbo Ferreira, 228, 4050-313 Porto, Portugal; Universidade Católica Portuguesa, CBQF - Centro de Biotecnologia e Química Fina - Laboratório Associado, Escola Superior de Biotecnologia, Rua Arquiteto Lobão Vital 172, 4200-374 Porto, Portugal; LQAV/REQUIMTE/Departamento de Química e Bioquímica, Faculdade de Ciências, Universidade do Porto, Rua do Campo Alegre, 4169-007 Porto, Portugal.
Abstract:
A method based on headspace solid-phase microextraction (HS-SPME) coupled to gas chromatography-triple quadrupole/mass spectrometry detection (GC-TQ/MS) with a prior derivatization step with O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine hydrochloride (PFBHA) was developed to quantify carbonyl compounds in different categories of Port wines. Optimal extraction conditions were obtained incubating 2 ml of wine with 2.3 g/l of PFBHA for 10 min and extracted during 20 min at 32 °C. The method was validated for 38 carbonyl compounds (alkanals, alkenals, Strecker aldehydes, dialdehydes, ketones and furan aldehydes) with regard to linearity, repeatability, inter and intra-day precision and accuracy, showing that the method is suitable for the determination of carbonyl compounds in wines. Tawny wines with 'indication of age' (10-40 years old) presented the highest levels of some carbonyl compounds, such as propanal, pentanal, hexanal, Strecker aldehydes, diacetyl, methyl glyoxal, 3-pentanone and 2-furfural, whereas Ruby wines were characterized by the highest amounts of some unidentified compounds.
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