摘要
目的建立核磁氢谱内标法快速测定酒制品中酒精含量的定量分析方法。方法采用核磁共振氢谱(^(1)H nuclear magnetic resonance,^(1)H-NMR),以二甲亚砜为内标物,以无水乙醇为对照品,按照单点法确立了定量计算公式,并对多种酒制品进行了测定。核磁共振氢谱测定参数为:温度25℃,谱宽2~14 ppm,脉冲角度45度,脉冲延迟时间3s,采样时间2s,扫描次数16次。结果在优化的测试条件下,目标物与内标物定量特征峰面积比在1:8~3:1范围内,该方法表现出良好的线性关系(r=0.9998);精密度和重复性实验相对标准偏差(relative standard deviations, RSDs)分别为0.061%和0.35%;样品加标回收率为98.9%~104.3%,平均偏差为2.1%。研究表明,该方法同样适用于水峰压制的情况及对酒制品中其他物质的测定。结论该方法样品需求量小、试剂成本低、结果稳定可靠,是一种简便、快捷的酒精含量检测方法。
Objective To establish a quantitative analysis method for the rapid determination of alcohol content in wine products by internal standard method of;H nuclear magnetic resonance spectroscopy(;H-NMR). Methods The quantitative calculation formula was established by;H-NMR using dimethylsulfoxide as the internal standard and anhydrous ethanol as the reference substance according to the single point method, and a variety of wine products were determined. The measurement parameters of;H-NMR hydrogen spectrum were as follows: Temperature 25 ℃,spectrum width 2-14 ppm, pulse angle 45 degrees, pulse delay time 3 s, sampling time 2 s, and scanning times 16 times. Results Under the optimized test conditions, the quantitative characteristic peak area ratio of the target substance to the internal standard substance was in the range of 1:8-3:1, and the method showed a good linear relationship(r=0.9998);the relative standard deviations(RSDs) for the precision and repeatability experiments were 0.061% and 0.35%, respectively;the recoveries of spiked samples were 98.9%-104.3%, with the average deviation of 2.1%. The results showed that this method was also suitable for the determination of other substances in wine products under the condition of water peak compression. Conclusion This method has the advantages of small sample requirement, low reagent cost, stable and reliable results, and is a simple and rapid method for detecting alcohol content.
作者
甄少波
ZHEN Shao-Bo(School of Hotel Management,China University of Labor Relations,Beijing 100048,China)
出处
《食品安全质量检测学报》
CAS
北大核心
2022年第3期926-932,共7页
Journal of Food Safety and Quality
基金
教育部教育教学改革专项(JYJG202002)
中国劳动关系学院一般科研项目(20XYJS010)。
关键词
核磁共振氢谱
内标法
酒精度
1H nuclear magnetic resonance
internal standard method
alcohol content
