定量核磁共振波谱法测定3种低聚果糖的含量  

Determination of 3 Fructo-Oligosaccharides by Quantitative Nuclear Magnetic Resonance Spectroscopy

作　　者：陈新启 吴少辉 乐胜锋 张梅[1] 霍金洪 王尉[1,3] CHEN Xinqi;WU Shaohui;LE Shengfeng;ZHANG Mei;HUO Jinhong;WANG Wei(Institute of Analysis and Testing,Beijing Academy of Science and Technology(Beijing Center for Physical and Chemical Analysis),Beijing 100089,China;Quantum Hi-Tech(Guangdong)Biological Co.,Ltd.,Jiangmen 529081,China;Specialistic Group on Natural Product of National Technical Committee on ReferenceMaterials,Beijing100094,China)

机构地区：[1]北京市科学技术研究院分析测试研究所(北京市理化分析测试中心),北京100089 [2]量子高科(广东)生物有限公司,江门529081 [3]全国标准样品技术委员会天然产物标准样品专业工作组,北京100094

出　　处：《理化检验（化学分册）》2023年第6期637-642,共6页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家重点研发计划项目(2019YFE0197100)。

摘　　要：以蔗糖为内标物,氘代水为溶剂,采用氢-1核磁共振波谱法(1H-NMR)测定蔗果七糖、蔗果八糖、蔗果九糖等3种低聚果糖(FOS)的含量。优化后的1H-NMR参数如下:温度25℃,谱宽(2~14)×10^(-6),脉冲角度45°,脉冲延迟时间5 s,采样时间3 s,扫描次数16次。对蔗果七糖、蔗果八糖和蔗果九糖样品进行了仪器精密度和重复性试验,测定值的相对标准偏差(n=6)均小于0.50%。方法用于测定3种样品含量,测定结果与质量平衡法所得结果进行了比较,经F检验法评估,两种方法具有显著性差异。但由于定量核磁共振波谱法作为绝对含量的测定方法,仅需常见的化学品即可直接对待测成分进行测定,可以佐证质量平衡法的赋值结果。Three fructo-oligosaccharides(FOS),including fructo-oligosaccharide DP7,DP8 and DP9,were determined by 1H nuclear magnetic resonance spectroscopy(1H-NMR),using sucrose as the internal standard substance and deuterium oxide as the solvent.The optimized 1H-NMR parameters were as follows:temperature at 25℃,spectral width of(2-14)×10^(-6),pulse angle at 45°,pulse delay time of 5 s,sampling time of 3 s,and scanning 16 times.Tests for instrument precision and repeatability of fructo-oligosaccharide DP7,DP8 and DP9 samples were made,with RSDs(n=6)of the determined values less than 0.50%.The contents of three samples were determined by this method,and the results were compared with those obtained by the mass balance method.After evaluation by the F-test,there was a significant difference between the two methods.However,as quantitative nuclear magnetic resonance spectroscopy was usually used for determining absolute content,it could directly determine the components to be tested with only common chemicals,which could support the assignment results of the mass balance method.

关 键 词：低聚果糖(FOS) 氢-1核磁共振波谱法(1H-NMR) 内标 

分 类 号：O657.61[理学—分析化学]