Luan Jiaqi, Feng Rui, Yu Chen, Wu Xuri, Shen Wenbin, Chen Yijun, DI Bin, Su Mengxiang
Key Laboratory on Protein Chemistry and Structural Biology, China Pharmaceutical University.
Department of Pharmaceutical Analysis, China Pharmaceutical University.
Anal Sci. 2018;34(9):1093-1098. doi: 10.2116/analsci.18P095.
Quantitative nuclear magnetic resonance (qNMR) has emerged as an easy, rapid and reproducible method for various pharmaceuticals. In the current study, a general qNMR approach for calibrating the purity of the thiopeptcin reference standard (also known as nocathiacin I) was developed using sulfadoxine as an internal standard. Experimental conditions, such as the relaxation delay time and number of scans, were systematically optimized, and the method was validated with different analytical parameters, including selectivity, stability, linearity, precision and robustness. To examine the reliability and feasibility of the present qNMR method, there was no significant difference in the quantification of this complex cyclic peptide compared to the mass balance method. The present study further exemplified that qNMR is a reliable and valuable approach for the assessing of absolute purity of small-molecule pharmaceuticals, which provides a useful tool for drug discovery and development.
定量核磁共振（qNMR）已成为一种用于各种药物的简便、快速且可重复的方法。在本研究中，开发了一种以磺胺多辛为内标物校准硫肽霉素参考标准品（也称为诺卡硫霉素I）纯度的通用qNMR方法。对弛豫延迟时间和扫描次数等实验条件进行了系统优化，并通过不同的分析参数（包括选择性、稳定性、线性、精密度和稳健性）对该方法进行了验证。为检验本qNMR方法的可靠性和可行性，与质量平衡法相比，该复杂环肽定量分析无显著差异。本研究进一步证明，qNMR是评估小分子药物绝对纯度的可靠且有价值的方法，为药物发现和开发提供了有用工具。
