管质量对外部校准的定量核磁共振分析的影响:它有多糟糕?
Jessica L Ochoa1, Stephan Germann2, Breanna Conklin1
1Synthetic Molecule Pharmaceutical Sciences (SMPS), Genentech Inc., South San Francisco, California, USA.
定量核磁共振 (NMR) 方法可以在没有添加校准剂的情况下确定化学含量. 这项研究表明,NMR管的变化会影响准确性,但简单的溶剂信号校正方法可以解决这个问题.
科学领域:
- 分析化学 分析化学
- 频谱学是一种光谱学.
- 核磁共振是一种核磁共振.
背景情况:
- 定量核磁共振 (NMR) 可以同时进行化学识别和含量确定,而无需样本增量.
- 尽管取得了进展,但在定量NMR中外部校准方法的采用仍然有限.
- 在NMR管的几何变化是一个重要的,往往被忽视,影响定量结果的因素.
研究的目的:
- 研究NMR管到管体积变量的影响对外部校准的定量NMR结果的影响.
- 评估拟议的体积校正策略在缓解这些变化的有效性.
主要方法:
- 对定量NMR实验进行了外部校准.
- 管到管的体积变化被系统地引入使用不同质量的NMR管.
- 开发并测试了一种利用剩余的质子化溶剂信号的新型体积校正策略.
主要成果:
- 观察到NMR管体积变化的显著影响对定量NMR结果.
- 提出的基于溶剂信号的体积校正策略有效地减轻了管到管变量的影响.
- 该校正方法在使用混合质量的NMR管的实验中被证明是可靠的.
结论:
- 核磁共振管质量是开发可靠的外部校准定量核磁共振方法的关键考虑因素.
- 简单的溶剂信号校正策略提供了一个切实可行的解决方案,以克服管到管的变化.
- 这种方法提高了外部校准在定量NMR的稳定性和适用性.
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