合超临界流体染色学与内部标准校正定量NMR用于快速准确的纯度评估
Huan Yao1, Ting Huang1, Zhifang Li2
1National Institute of Metrology, Beijing 100029, P.R.China.
Analytical chemistry
|July 14, 2025
概括
一种新的可追溯量化方法,超临界流体染色学-内部标准校正-定量核磁共振 (SFC-ISC-qNMR),可以快速准确地评估活性药物成分 (API) 的纯度,而不需要针对特定目标的参考材料.
科学领域:
- 分析化学 分析化学
- 药品分析 药品分析
- 频谱学是一种光谱学.
背景情况:
- 纯度评估对于药品活性成分 (API) 质量控制至关重要.
- 现有的方法通常需要针对特定目标的认证参考材料 (CRM),这限制了它们的适用性.
- 需要快速,准确和独立于CRM的纯度评估技术.
研究的目的:
- 开发和验证用于API纯度评估的可追溯量化方法.
- 为了能够准确的定量确定低纯度的API.
- 为药物评估和研究建立一个独立于CRM的方法.
主要方法:
- 提出了一种新的超临界流体染色学-内部标准校正-定量核磁共振 (SFC-ISC-qNMR) 方法.
- 利用超临界流体染色学 (SFC) 进行分析物收集和分离.
- 使用定量核磁共振 (qNMR) 与内部标准校正 (ISC) 进行SI可追溯量化.
主要成果:
- 使用SFC.实现了高纯度的数字毒素隔离 (>99.87%) .
- 证明了该方法在测量混合物中数字毒素的可行性和可靠性.
- 确定商业数字毒素试剂的纯度为94.17%±0.15%,与高分辨率的qNMR一致.
- 与重力测量值相比,显示了高的一致性 (偏差<0.13%) 来确定尖端数字毒素含量.
- 在这种情况下,强调了直接的qNMR和HPLC在准确测量方面的局限性.
结论:
- SFC-ISC-qNMR方法为API纯度评估提供了一个强大而准确的方法.
- 该方法独立于特定目标的CRM,提供更广泛的适用性.
- 这种技术显示出药物评估,质量控制和研究的巨大潜力.
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