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甘油是酿酒过程中不可缺少的甜料与抑制剂,它对提高酒的质量具有重要作用。酒中甘油的分析一般采用氧化法、还原法或化学衍生法。采用直接进样气相色谱法,柱温要200℃以上,保留时间仍较长,色谱峰拖尾严重。本文采用色谱时间归一化技术,控制甘油的保留值一定,合理地调整固定液涂渍量与载气流速、柱长与柱温之间的关系。选定一根0.43%PEG-20M薄涂柱,使甘油在较低柱温下与其它细份有效、快速分离。甘油保留时间短,峰形较对称。该法用用于三种葡萄酒中甘油的测定,其相对标准偏差分别为±0.69%,±0.47%和±0.57%。回收率分别为94.4%,95.0%和95.9%。
Glycerin is indispensable in the brewing process of sweeteners and inhibitors, it is to improve the quality of the wine has an important role. Analysis of wine glycerol generally use the oxidation method, reduction method or chemical derivative method. Using direct injection gas chromatography, the column temperature to be above 200 ℃, the retention time is still long, severe tailing peak. In this paper, the chromatographic time normalization technique is used to control the retention of glycerol to a certain extent. The relationship between the amount of fixative solution and carrier gas flow rate, column length and column temperature should be adjusted reasonably. A 0.43% PEG-20M thin-coated column was selected to allow glycerol to be efficiently separated from other fractions at lower column temperatures and quickly separated. Short retention time of glycerol, peak shape more symmetrical. The method was applied to the determination of glycerol in three wines with relative standard deviations of ± 0.69%, ± 0.47% and ± 0.57%, respectively. The recoveries were 94.4%, 95.0% and 95.9%, respectively.