收集后的纯度校正用于内部标准校正-高性能液体色谱-定量核磁共振
Xueyao Li1, Wei Zhang2, Ting Huang2
1College of Chemistry, Beijing University of Chemical Technology, Beijing 100029, China. tgs1803@163.com.
概括
一种新方法提高了复杂化合物的定量核磁共振 (qNMR) 精度. 采集后的纯度校正用于内部标准校正-HPLC-qNMR方法可以提高纯度的确定,特别是对于具有类似杂质的样品.
科学领域:
- 分析化学 分析化学
- 频谱学是一种光谱学.
- 染色体学 染色体学 是一种染色学.
背景情况:
- 定量核磁共振 (qNMR) 对低纯度的复杂有机化合物可能产生不准确的结果.
- 杂质信号与目标组件信号的不完全分离在qNMR分析中构成了重大挑战.
- 传统的质量平衡方法来确定杂质是艰苦的,耗时的,昂贵的.
研究的目的:
- 开发一种改进的方法,使用qNMR精确确定复杂有机化合物的纯度.
- 解决标准qNMR和HPLC-qNMR在处理具有低纯度和结构相似杂质的样本方面的局限性.
- 为了减少与杂质识别和量化相关的时间和成本.
主要方法:
- 开发采集后纯度校正用于内部标准校正-HPLC-qNMR (ISC-HPLC-qNMR).
- 将改进方法应用于纯度较低的复杂化合物 - - 氧化四环素.
- 引入一个校正因子来考虑不完整的HPLC净化.
主要成果:
- 通过ISC-HPLC-qNMR方法,氧基环素的纯度值为82.00%±0.82%.
- 常规的qNMR与解卷提供了81.70%±0.35%的可比纯度值.
- 结果表明,该方法在处理复杂的样本时具有有效性,在HPLC净化后残留杂质.
结论:
- 开发的ISC-HPLC-qNMR方法准确量化复杂化合物的纯度,即使具有具有挑战性的杂质概况.
- 这种方法将qNMR的适用性扩展到HPLC无法完全净化的样品.
- 该方法通过消除对杂质识别的需求,可以节省大量的时间和成本.
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