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

发布时间：2018-01-28 08:18

本文关键词： 苯乙醇胺A 定量核磁反门控去耦纯度　出处：《分析测试学报》2017年07期 　论文类型：期刊论文

【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(D_1),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307),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0.3Hz。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(r~2)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。
[Abstract]:The purity of phenylethanolamine A was determined by inverse gated decoupling method in quantitative nuclear magnetic field. The deuterium solvent and internal standard, the selection of quantitative peak and relaxation delay time were used to determine the purity of phenethanolamine A. The quantitative nuclear magnetic parameters such as sampling times and sampling temperature were optimized. The test conditions were determined as follows: excitation pulse angle 307 K, time domain data point 32 K, and measurement temperature 293 K. The relaxation delay of the pulse is 33.64 s, the sampling frequency is 64 and the linewidth is 0.3 Hz. Under the experimental conditions, the stability can reach 24 h. The standard curve was drawn with the peak area ratio of sample and internal standard. The results showed that the molar ratio of the two was linear in the range of 0.333 ~ 3.333. The correlation coefficient is 0.999 9. The method is specific, accurate and simple. It is suitable for the determination of this kind of compounds.
【作者单位】：中国农业科学院农业质量标准与检测技术研究所;
【基金】：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)
【分类号】：O657.2;S859.84
【正文快照】： 苯乙醇胺A又名克伦巴胺,是一种β-受体激动剂,具有β-受体激动剂的典型结构。它是一种人工合成的化学物质,是福莫特罗的同分异构体,其结构(见图1)与莱克多巴胺类似[1]。苯乙醇胺A是2010年新发现的一种瘦肉精,具有营养再分配的作用,添加到饲料中可加速脂肪的分解和转化,提高动

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