Rocha Sílvia M, Coutinho Paula, Barros António, Delgadillo Ivonne, Coimbra Manuel A
Departamento de Química, Universidade de Aveiro, 3810-193 Aveiro, Portugal.
J Chromatogr A. 2006 May 12;1114(2):188-97. doi: 10.1016/j.chroma.2006.03.107. Epub 2006 Apr 18.
This work describes a novel methodology for the rapid distinction of wines by headspace solid-phase microextraction coupled to gas chromatography-mass spectrometry, followed by principal component analysis of the data (HS-SPME-GC-MS-PCA). Headspace SPME is used to extract and concentrate the volatile and semi-volatile fractions. A DB-FFAP fused silica GC capillary column of 30 m at 220 degrees C was used acting as a transfer line of the components sorbed by the Carbowax-divinylbenzene coating fibre to the mass spectrometer, which acts as a sensor (30<m/z<300). In this methodology, which does not require any pre-treatment of the sample, the global volatile signature of the wine headspace (chromatographic profile and m/z pattern of fragmentation in each scan) is evaluated without complete chromatographic separation of its components. In order to retrieve from the data as much chemical information as possible and to extract m/z fragments (markers) for the characterisation and distinction of the wines varieties, a PCA was applied to the data resultant from the unresolved volatile fraction. In the present study, two different monovarietal white wines (Vitis vinifera L. var. Fernão-Pires and Arinto) were tested. Associated to the fast character of the proposed methodology and robustness taking into account the extraction time, it is also important to focus the higher sensibility and the lower effect of the sample moisture of the MS sensor response when compared to the conventional e-noses.
本研究描述了一种通过顶空固相微萃取结合气相色谱 - 质谱联用，随后对数据进行主成分分析（HS - SPME - GC - MS - PCA）来快速区分葡萄酒的新方法。顶空固相微萃取用于提取和浓缩挥发性和半挥发性成分。使用一根30 m、220℃的DB - FFAP熔融石英气相色谱毛细管柱，作为将被聚乙二醇 - 二乙烯基苯涂层纤维吸附的组分传输至作为传感器的质谱仪的传输线（30 < m/z < 300）。在该方法中，无需对样品进行任何预处理，在不完整分离葡萄酒顶空各组分的情况下，评估其整体挥发性特征（每次扫描中的色谱图和碎片的m/z模式）。为了从数据中尽可能多地获取化学信息，并提取用于表征和区分葡萄酒品种的m/z碎片（标记物），对未解析挥发性组分产生的数据应用了主成分分析。在本研究中，测试了两种不同的单一品种白葡萄酒（酿酒葡萄品种费尔南多皮雷斯和阿林托）。考虑到所提出方法的快速特性以及提取时间方面的稳健性，与传统电子鼻相比，聚焦于质谱传感器响应的更高灵敏度和更低的样品水分影响也很重要。
