通过带选择性HSQC NMR测量Tripterygium属的基胺类化合物的量化
Youwen Chen1, Yadan Wang2, Jiangong Yan2
1National Institutes for Food and Drug Control, Beijing, 102629, PR China; School of Chinese Materia Medica, Beijing University of Chinese Medicine, Beijing, 100102, PR China.
Analytica chimica acta
|July 16, 2023
概括
带选择性HSQC核磁共振成功分离了类胺类化物 (SPA),使得23个SPA的识别和量化成为可能. 这种新的方法为分析复杂的植物提取物提供了可靠的方法.
科学领域:
- 自然产品化学 自然产品化学
- 分析化学 分析化学
- 频谱学是一种光谱学.
背景情况:
- 来自Tripterygium属的塞斯基二烯胺类化合物 (SPA) 具有抗炎和抗风湿的特性.
- 类似的基结构导致1D NMR和HPLC的显著峰值重叠,阻碍了SPA的识别和量化.
研究的目的:
- 开发一种新的NMR方法,以更好地识别和量化复杂混合物中的SPA.
- 为含有SPA的植物提取物建立可靠和快速的分析方法.
主要方法:
- 应用带选择性HSQCNMR来选择性地激发SPA的H-3区域,实现信号分离.
- 测量合常数和放松时间,以评估HSQC信号的统一性.
- 使用wilforgine标准曲线方法和基于脉冲长度的度确定方法 (PULCON) 的量化.
- 根据USP<761>标准验证开发的方法.
主要成果:
- 带选择性HSQCNMR成功地解决了SPA的重叠信号.
- 从高分辨率带选择性HSQC频谱中确定了23个SPA.
- 通过标准曲线和PULCON方法进行量化,结果一致.
- 开发的方法证明了SPA分析的可靠性和效率.
结论:
- 带选择性HSQC核磁共振是一种强大的工具,可以克服复杂化物混合物的光谱重叠.
- 开发的量化方法得到了验证,并且适用于植物来源中SPA的快速分析.
- 这种方法提高了在天然产品中识别和量化生物活性化合物的能力.
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