A rapid, one step preparation for measuring selected free plus SO2-bound wine carbonyls by HPLC-DAD/MS
A rapid, one step preparation for measuring selected free plus SO2-bound wine carbonyls by HPLC-DAD/MS
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DOI：
10.1016/j.talanta.2014.11.046
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发表时间：
2015-03-01
期刊：
影响因子：
6.1
通讯作者：
Waterhouse, Andrew L.
中科院分区：
文献类型：
--
作者：
Han, Guomin;Wang, Hua;Waterhouse, Andrew L.
羰基化合物是在酿酒和陈酿过程中的发酵和化学氧化过程中产生的，它们对葡萄酒的风味和颜色稳定性很重要。由于葡萄酒中还含有这些与二氧化硫反应而形成的α-羟基磺酸盐化合物，因此需要进行氧气排除的碱性预处理来释放这些结合的羰基以进行分析。通过改进在2,4-二硝基苯肼（DNPH）存在下加热和酸水解羟基磺酸盐的方法，羰基化合物同时快速释放和衍生，从而使方法更简单、更快速。此外，该方法通过添加二氧化硫避免了水解过程中的空气排除并发症。该方法针对温度、反应时间以及 DNPH、二氧化硫和酸的浓度进行了优化。腙在 10 小时内稳定，这对于 HPLC-DAD/MS 的色谱分析来说是足够的时间。该方法针对反应活性截然不同的 2-酮戊二酸、丙酮酸、乙偶姻和乙醛以及葡萄酒羰基化合物进行了验证，并且具有良好的特异性、高回收率和低检测限。这种快速、简单的新方法可用于测量不同年份和葡萄品种的一系列葡萄酒中的羰基化合物。 (C) 2014 Elsevier B.V. 保留所有权利。
Carbonyl compounds are produced during fermentation and chemical oxidation during wine making and aging, and they are important to wine flavor and color stability. Since wine also contains these compounds as alpha-hydroxysulfonates as a result of their reaction with sulfur dioxide, an alkaline pre-treatment requiring oxygen exclusion has been used to release these bound carbonyls for analysis. By modifying the method to hydrolyze the hydroxysulfonates with heating and acid in the presence of 2,4-dinitrophenylhydrazine (DNPH), the carbonyl compounds are simultaneously and quickly released and derivatized, resulting in a simpler and more rapid method. In addition, the method avoids air exclusion complications during hydrolysis by the addition of sulfur dioxide. The method was optimized for temperature, reaction time, and the concentrations of DNPH, sulfur dioxide and acid. The hydrazones were shown to be stable for 10 h, adequate time for chromatographic analysis by HPLC-DAD/MS. This method is demonstrated for 2-ketoglutaric acid, pyruvic acid, acetoin and acetaldehyde, wine carbonyls of very different reactivities, and it offers good specificity, high recovery and low limits of detection. This new rapid, simple method is demonstrated for the measurement of carbonyl compounds in a range of wines of different ages and grape varieties. (C) 2014 Elsevier B.V. All rights reserved.