The effect of tube quality on externally calibrated quantitative nuclear magnetic resonance analysis: How bad can it be?

Author:

Ochoa Jessica L.1,Germann Stephan2,Conklin Breanna1,Kurita Kenji1,Russell David J.1,Yang Cassie2,Napolitano José G.1ORCID

Affiliation:

1. Synthetic Molecule Pharmaceutical Sciences (SMPS) Genentech Inc. South San Francisco California USA

2. Analytical Research and Development (ARD) AbbVie Inc. North Chicago Illinois USA

Abstract

AbstractExternally calibrated quantitative nuclear magnetic resonance (NMR) approaches offer practical means to simultaneously evaluate chemical identity and content without the addition of calibrants to the test sample. Despite continuous advances in external calibration over the last few decades, adoption of these approaches has been slower than expected. Variations in NMR tube geometry are a commonly overlooked factor that can have a substantial effect on externally calibrated quantitation methods. In this report, we investigate the extent to which tube‐to‐tube volume variability can affect quantitative NMR outcomes. The results highlight the importance of considering tube quality during the development stages of externally calibrated quantitative methods. In addition, we propose a simple, yet effective volume correction strategy using the residual protonated solvent signal that, based on experiments with mixed NMR tubes of varying quality, alleviates the effect of tube‐to‐tube variability.

Publisher

Wiley

Subject

General Materials Science,General Chemistry

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