| 反门控去耦技术在定量1H NMR测定苯乙醇胺A纯度中的应用 |
| 点此下载全文 |
|
| 基金项目:中国农业科学院创新工程；农产品质量安全风险评估标准物质研制与质量控制规范研究(2015)(GJFP201501503) |
|
| 中文摘要:采用定量核磁中反门控去耦的方法对苯乙醇胺A的纯度进行测定。通过对氘代溶剂和内标物、定量峰的选择，以及弛豫延迟时间(D1)，采样次数和采样温度等定量核磁条件的优化，最终确定测试条件为：激发脉冲角度30°，时间域数据点32 K，测定温度293 K，脉冲的弛豫延迟为33.64 s，采样次数64，线宽0.3 Hz。在此实验条件下，稳定性可达24 h，耐用性良好。以样品和内标的峰面积比对其摩尔比绘制标准曲线，结果显示，两者的摩尔比在0.333~3.333范围内线性关系良好，相关系数(r2)为0.999 9。该方法专属性强，准确，简便，适用于该类型化合物含量的测定。 |
| 中文关键词:苯乙醇胺A 定量核磁 反门控去耦 纯度 |
| |
| Application of Inverse Gated Decoupling Technique in Quantitative 1H NMR Determination of Purity of Phenylethanolamine A |
|
|
| Abstract:A high accuracy method of qNMR with inverse gated decoupling technique was established to determine the content of phenylethanolamine A.Considering the choice of deuterated solvents,internal standards and quantitative peaks,and the optimization of relaxation delay,aquisition number and temperature,the final measurement conditions of qNMR spectra were as follows:flip angle:30°,date point:32 K,detection temperature:293 K,a relaxation delay:33.64 s,acquisition times:64 times,line broadening:0.3 Hz.The experimental results showed that the stability of this condition could be maintained for 24 h.A good linear relationship was obtained between peak area ratio and molar ratio in the range of 0.333-3.333,and the correlation coefficient (r2) was 0.999 9.The established method is specific,accurate and simple,and could be used for the content determination of this kind of compounds. |
| Key Words:phenylethanolamine A qNMR inverse gated decoupling purity |
| 引用本文：宋印清，王敏*，王彤彤，周剑，杨梦瑞.反门控去耦技术在定量1H NMR测定苯乙醇胺A纯度中的应用[J].分析测试学报,2017,36(7):933-936. |
| 摘要点击次数: 2097 |
| 全文下载次数: 954 |
| 查看全文 下载PDF阅读器 |
|
|
