Mestres M, Busto O, Guasch J
Departament de Química, Escola d'Enologia, Universitat Rovira i Virgili, Spain.
J Chromatogr A. 1997 Jun 27;773(1-2):261-9. doi: 10.1016/s0021-9673(97)00188-x.
This study describes the development of a method for determining eleven sulphur compounds in wine, which takes into account that thiols are easily oxidizable. The equilibria of the analytes between air and aqueous ethanol were studied and optimised using static headspace gas chromatography in order to obtain the best sensitivities. The influences of parameters such as temperature, time, ionic strength, headspace volume and the volume of headspace injected were determined. A cryogenic trap was used to concentrate the headspace analytes and they were chromatographically analysed using GC temperature programming on a poly(ethylene glycol) capillary column with FPD detection at 394 nm. The power relationship was observed between the chromatography response and a concentration of sulphur compounds in the range 2-150 micrograms l(-1) in the sample. Recoveries were determined by the standard addition technique and were higher than 90% for sulphides and disulphides and close to 80% for thiols. The overall method was successfully used to determine the sulphur compounds in white and red wines.
本研究描述了一种测定葡萄酒中11种硫化合物的方法的开发过程，该方法考虑到硫醇易于氧化的特性。利用静态顶空气相色谱法研究并优化了分析物在空气和乙醇水溶液之间的平衡，以获得最佳灵敏度。确定了温度、时间、离子强度、顶空体积和进样顶空体积等参数的影响。使用低温捕集阱对顶空分析物进行浓缩，并在聚（乙二醇）毛细管柱上采用气相色谱程序升温，在394nm处用火焰光度检测器进行色谱分析。在2-150微克/升的样品硫化合物浓度范围内，观察到色谱响应与硫化合物浓度之间的幂关系。通过标准加入法测定回收率，硫化物和二硫化物的回收率高于90%，硫醇的回收率接近80%。该方法成功地用于测定白葡萄酒和红葡萄酒中的硫化合物。
