What Is the Accuracy of Quantitative Analysis by Low-Field NMR Spectroscopy Using Internal Standard: Systematic Study of Finished Medicinal Products?

IF 1.3 4区物理与天体物理 Q4 PHYSICS, ATOMIC, MOLECULAR & CHEMICAL

Applied Magnetic Resonance Pub Date : 2025-09-26 DOI:10.1007/s00723-025-01804-w

Klaudia Adels, Yulia B. Monakhova

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Abstract

Quantitative nuclear magnetic resonance (qNMR) is considered as a powerful tool for measuring the absolute amount of small molecules in complex mixtures. In this study, the performance of quantitative analysis on low-field NMR (LF NMR) devices was evaluated for a representative set of 33 finished medicinal products. Sample preparation, critical acquisition, and processing parameters were systematically evaluated. Recovery rates varied between 97 and 103% were achieved by signal-to-noise ratio (SNR) equal to 300 using deuterated solvents. For non-deuterated solvents, the recovery rates between 95 and 105% were observed at this SNR value. Average bias values in comparison with the reference high-field NMR were found to be 1.4% and 2.6% for deuterated and non-deuterated solvents, respectively. Erroneous results can be obtained for non-deuterated solvents when the integrated signals are situated close to solvent suppression regions. Validation results in terms of precision and reproducibility demonstrate that the LF qNMR method is fit-for-purpose for the marketed pharmaceutical products.

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内标低场核磁共振光谱定量分析的准确性：成品药的系统研究？

定量核磁共振（qNMR）被认为是测量复杂混合物中小分子绝对数量的有力工具。本研究对具有代表性的33种成品药进行了低场核磁共振（LF NMR）定量分析。系统地评估了样品制备、关键采集和处理参数。采用氘化溶剂，信噪比（SNR）为300，回收率在97% ~ 103%之间。在此信噪比下，非氘化溶剂的回收率在95 ~ 105%之间。与参考高场NMR相比，氘化溶剂和非氘化溶剂的平均偏置值分别为1.4%和2.6%。对于非氘化溶剂，当积分信号位于溶剂抑制区附近时，可能会得到错误的结果。在精密度和可重复性方面的验证结果表明，LF qNMR方法适合于上市药品的目的。

本文章由计算机程序翻译，如有差异，请以英文原文为准。

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来源期刊

Applied Magnetic Resonance 物理-光谱学

CiteScore

1.90

自引率

10.00%

发文量

审稿时长

2.3 months

期刊介绍： Applied Magnetic Resonance provides an international forum for the application of magnetic resonance in physics, chemistry, biology, medicine, geochemistry, ecology, engineering, and related fields. The contents include articles with a strong emphasis on new applications, and on new experimental methods. Additional features include book reviews and Letters to the Editor.