Laboratorio Arbitral Agroalimentario, Ministerio de Medio Ambiente y Medio Rural y Marino, 28023 Madrid, Spain.
J Agric Food Chem. 2010 Jan 27;58(2):722-8. doi: 10.1021/jf9029095.
A novel procedure was established for the simultaneous characterization of wine glycerol and ethanol (13)C/(12)C isotope ratio, using liquid chromatography/isotope ratio mass spectrometry (LC-IRMS). Several parameters influencing separation of glycerol and ethanol from wine matrix were optimized. Results obtained for 35 Spanish samples exposed no significant differences and very strong correlations (r = 0.99) between the glycerol (13)C/(12)C ratios obtained by an alternative method (gas chromatography/isotope ratio mass spectrometry) and the proposed new methodology, and between the ethanol (13)C/(12)C ratios obtained by the official method (elemental analyzer/isotope ratio mass spectrometry) and the proposed new methodology. The accuracy of the proposed method varied from 0.01 to 0.19 per thousand, and the analytical precision was better than 0.25 per thousand. The new developed LC-IRMS method it is the first isotopic method that allows (13)C/(12)C determination of both analytes in the same run directly from a liquid sample with no previous glycerol or ethanol isolation, overcoming technical difficulties associated with complex sample treatment and improving in terms of simplicity and speed.
建立了一种新的方法,用于同时对葡萄酒甘油和乙醇的(13)C/(12)C 同位素比值进行特征描述,采用液相色谱/同位素比质谱法(LC-IRMS)。优化了从葡萄酒基质中分离甘油和乙醇的几个参数。对 35 个西班牙样品的结果表明,用替代方法(气相色谱/同位素比质谱法)和新提出的方法获得的甘油(13)C/(12)C 比值之间,以及用官方方法(元素分析仪/同位素比质谱法)和新提出的方法获得的乙醇(13)C/(12)C 比值之间没有显著差异和非常强的相关性(r=0.99)。所提出的方法的准确度在 0.01 到 0.19/千之间变化,分析精度优于 0.25/千。这种新开发的 LC-IRMS 方法是第一个允许在同一次运行中直接从液体样品中同时测定两种分析物的同位素方法,无需预先分离甘油或乙醇,克服了与复杂样品处理相关的技术困难,并在简单性和速度方面得到了提高。