Fedrizzi Bruno, Magno Franco, Moser Sergio, Nicolini Giorgio, Versini Giuseppe
IASMA Research Center, Agri-Food Quality Department, via Mach 1, 38010 San Michele all'Adige (TN), Italy.
Rapid Commun Mass Spectrom. 2007;21(5):707-14. doi: 10.1002/rcm.2893.
A new method based on headspace solid-phase microextraction coupled with gas chromatography/mass spectrometry (HS-SPME-GC/MS) to analyse 13 light and heavy volatile sulphur compounds in the same run was established. For the successful application of the procedure, various adsorption process parameters were optimised. In particular the nature of the adsorptive phase, the temperature, the ionic strength of the sample solutions and the equilibration time were considered. The best extraction conditions, in terms of the maximum signal obtainable for each compound, were obtained with a carboxen-polydimethylsiloxane-divinylbenzene (CAR-PDMS-DVB) 2 cm long coating fibre. The choice of suitable internal standards and the matrix effect were studied and the proposed method was validated by determining linearity, precision and accuracy, evaluating the critical, detection and quantification limits. This method is fast, sensitive and precise and easy to transfer to wine quality control. Finally, the proposed method was applied to the determination of the aforementioned sulphur compounds in 32 red and white wines.
建立了一种基于顶空固相微萃取结合气相色谱/质谱联用(HS-SPME-GC/MS)的新方法,可在一次运行中分析13种轻、重挥发性硫化合物。为使该方法成功应用,对各种吸附过程参数进行了优化。特别考虑了吸附相的性质、温度、样品溶液的离子强度和平衡时间。就每种化合物可获得的最大信号而言,使用2 cm长的羧基-聚二甲基硅氧烷-二乙烯基苯(CAR-PDMS-DVB)涂层纤维获得了最佳萃取条件。研究了合适内标的选择和基质效应,并通过测定线性、精密度和准确度、评估临界、检测和定量限对所提出的方法进行了验证。该方法快速、灵敏、精确且易于转移至葡萄酒质量控制。最后,将所提出的方法应用于32种红葡萄酒和白葡萄酒中上述硫化合物的测定。