Perestrelo Rosa, Caldeira Michael, Rodrigues Freddy, Câmara José S
Centro de Química da Madeira, Departamento de Química, Universidade da Madeira, Campus Universitário da Penteada, Funchal, Portugal.
J Sep Sci. 2008 Jun;31(10):1841-50. doi: 10.1002/jssc.200700568.
A suitable analytical procedure based on static headspace solid-phase microextraction (SPME) followed by thermal desorption gas chromatography-ion trap mass spectrometry detection (GC-(ITD)MS), was developed and applied for the qualitative and semi-quantitative analysis of volatile components of Portuguese Terras Madeirenses red wines. The headspace SPME method was optimised in terms of fibre coating, extraction time, and extraction temperature. The performance of three commercially available SPME fibres, viz. 100 mum polydimethylsiloxane; 85 mum polyacrylate, PA; and 50/30 mum divinylbenzene/carboxen on polydimethylsiloxane, was evaluated and compared. The highest amounts extracted, in terms of the maximum signal recorded for the total volatile composition, were obtained with a PA coating fibre at 30 degrees C during an extraction time of 60 min with a constant stirring at 750 rpm, after saturation of the sample with NaCl (30%, w/v). More than sixty volatile compounds, belonging to different biosynthetic pathways, have been identified, including fatty acid ethyl esters, higher alcohols, fatty acids, higher alcohol acetates, isoamyl esters, carbonyl compounds, and monoterpenols/C(13)-norisoprenoids.
开发了一种基于静态顶空固相微萃取（SPME），随后进行热脱附气相色谱 - 离子阱质谱检测（GC - （ITD）MS）的合适分析方法，并将其应用于葡萄牙马德拉土壤红葡萄酒挥发性成分的定性和半定量分析。顶空SPME方法在纤维涂层、萃取时间和萃取温度方面进行了优化。评估并比较了三种市售SPME纤维的性能，即100μm聚二甲基硅氧烷；85μm聚丙烯酸酯（PA）；以及50/30μm二乙烯基苯/碳分子筛涂覆在聚二甲基硅氧烷上的纤维。在用NaCl（30%，w/v）使样品饱和后，在750 rpm的恒定搅拌下，于30℃萃取60分钟，使用PA涂层纤维时，就总挥发性成分记录的最大信号而言，提取量最高。已鉴定出六十多种属于不同生物合成途径的挥发性化合物，包括脂肪酸乙酯、高级醇、脂肪酸、高级醇乙酸酯、异戊酯、羰基化合物和单萜醇/C(13)-去甲异戊二烯类化合物。
