Godelmann Rolf, Kost Christian, Patz Claus-Dieter, Ristow Reinhard, Wachter Helmut
Chemical and Veterinary Investigation Office Karlsruhe, Weissenburger Strasse 3, D-73187 Karlsruhe, Germany.
WineSpin Analytics GmbH & Co. KG, Germaniastrasse 63, D-55459 Aspisheim, Germany.
J AOAC Int. 2016 Sep;99(5):1295-304. doi: 10.5740/jaoacint.15-0318. Epub 2016 Jul 20.
To examine whether NMR analysis is a suitable method for the quantitative determination of wine components, an international collaborative trial was organized to evaluate the method according to the international regulations and guidelines of the German Institute for Standardization/International Organization for Standardization, AOAC INTERNATIONAL, the International Union of Pure and Applied Chemistry, and the International Organization of Vine and Wine. Sugars such as glucose; acids such as malic, acetic, fumaric, and shikimic acids (the latter two as minor components); and sorbic acid, a preservative, were selected for the exemplary quantitative determination of substances in wine. Selection criteria for the examination of sample material included different NMR spectral signal types (singlet and multiplet), as well as the suitability of the proposed substances for manual integration at different levels of challenge (e.g., interference as a result of the necessary suppression of a water signal or the coverage of different typical wine concentration ranges for a selection of major components, minor components, and additives). To show that this method can be universally applied, NMR measurement and the method of evaluation were not strictly elucidated. Fifteen international laboratories participated in the collaborative trial and determined six parameters in 10 samples. The values, in particular the reproducibility SD (SR), were compared with the expected Horwitz SD (SH) by forming the quotient SR/SH (i.e., the HorRat value). The resulting HorRat values of most parameters were predominantly between 0.6 and 1.5, and thus of an acceptable range.
为了检验核磁共振（NMR）分析是否是定量测定葡萄酒成分的合适方法，组织了一项国际合作试验，以根据德国标准化研究所/国际标准化组织、美国官方分析化学师协会（AOAC INTERNATIONAL）、国际纯粹与应用化学联合会以及国际葡萄与葡萄酒组织的国际法规和指南对该方法进行评估。选择了葡萄糖等糖类；苹果酸、乙酸、富马酸和莽草酸（后两种为次要成分）等酸类；以及防腐剂山梨酸，用于葡萄酒中物质的示例性定量测定。样品材料检验的选择标准包括不同的NMR光谱信号类型（单峰和多重峰），以及所提议物质在不同挑战水平下进行手动积分的适用性（例如，由于必须抑制水信号而产生的干扰，或针对主要成分、次要成分和添加剂选择的不同典型葡萄酒浓度范围的覆盖情况）。为了表明该方法可以普遍应用，未严格阐明NMR测量和评估方法。15个国际实验室参与了合作试验，并对10个样品中的6个参数进行了测定。通过形成商SR/SH（即HorRat值），将这些值，特别是重现性标准差（SR）与预期的霍维茨标准差（SH）进行了比较。大多数参数的最终HorRat值主要在0.6至1.5之间，因此处于可接受范围内。
