摘要
采用核磁共振碳谱(^(13)C Nuclear magnetic resonance,^(13)C-NMR)的脉冲序列,分别以苯磺酸钠和蔗糖为内标物和对照品,建立了蔗糖含量的直接定量分析方法,并对多种食品和药品中的蔗糖进行了测定。^(13)C-NMR测定参数为:谱宽–15-235 ppm,脉冲角度45°,温度25℃,脉冲延迟时间1 s,采样时间0.87 s,扫描次数为2000,氢宽带去耦。考察目标物加入量与定量特征峰面积比之间的相关性,得到回归方程Y=0.02415+0.03195X,r=0.9998,在测试范围内线性关系良好。精密度实验和重复性实验的相对标准偏差RSD分别为0.078%和0.520%。样本加标回收率95.50%-104.80%,平均98.60%。该方法不需要样品前处理,结果准确可靠,测定时间较短,是一种快捷简便的食品和药品中蔗糖含量的检测方法,也可用于其他糖类的测定。
A direct quantitative analysis method for sucrose content was established using pulse sequences of ^(13)C nuclear magnetic resonance(^(13)C NMR),with sodium benzenesulfonate and sucrose as internal standard and reference material,sucrose content in various food and drug products was determined.The ^(13)C-NMR measurement parameters were as follous:spectral width-15-235 ppm,pulse angle of 45 degrees,temperature at 25℃,pulse delay time of 1 s,sampling time of 0.87 s,and 2000 scan times,hydrogen broadband decoupling.The correlation between the amount of target substance added and the ratio of quantitative characteristic peak area was investigated,and the regression equation(Y=0.02415+0.03195X,r=0.9998)was obtained,the linear relationship was good within the testing range.The relative standard deviations(RSD)of precision and repeatability experiments was 0.078%and 0.52%,The recovery rate of spiked samples ranged from 95.50% to 104.80%,with an average of 98.60%.This method does not require sample pretreatment,and the results are accurate,reliable,and the determination time is short.It is a fast and convenient method for detecting sucrose content in food and drugs,and can also be used for the determination of other sugars.
作者
陈新启
杨作振
焦晓林
马博凯
张梅
王尉
CHEN Xinqi;YANG Zuozhen;JIAO Xiaolin;MA Bokai;ZHANG Mei;WANG Wei(Institute of Analysis and Testing,Beijing Academy of Science and Technology(Beijing Center for Physical and Chemical Analysis),Beijing 100089,China;Biomedicine School,Beijing City University,Beijing 100094,China)
出处
《食品科技》
CAS
北大核心
2023年第10期243-248,共6页
Food Science and Technology
基金
北京市科学技术研究院创新工程项目(23CA005-03)。
关键词
核磁共振碳谱
食品
药品
定量核磁
质量分数
^(13)C nuclear magnetic resonance
food
medicine
quantitative NMR
mass fraction
