Journal of Pharmaceutical and Biomedical Analysis 2014-05-01

Using high-performance ¹H NMR (HP-qNMR®) for the certification of organic reference materials under accreditation guidelines--describing the overall process with focus on homogeneity and stability assessment.

Michael Weber, Christine Hellriegel, Alexander Rueck, Juerg Wuethrich, Peter Jenks

Index: J. Pharm. Biomed. Anal. 93 , 102-110, (2014)

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Abstract

Quantitative NMR spectroscopy (qNMR) is gaining interest across both analytical and industrial research applications and has become an essential tool for the content assignment and quantitative determination of impurities. The key benefits of using qNMR as measurement method for the purity determination of organic molecules are discussed, with emphasis on the ability to establish traceability to "The International System of Units" (SI). The work describes a routine certification procedure from the point of view of a commercial producer of certified reference materials (CRM) under ISO/IEC 17025 and ISO Guide 34 accreditation, that resulted in a set of essential references for (1)H qNMR measurements, and the relevant application data for these substances are given. The overall process includes specific selection criteria, pre-tests, experimental conditions, homogeneity and stability studies. The advantages of an accelerated stability study over the classical stability-test design are shown with respect to shelf-life determination and shipping conditions. Copyright © 2013 The Authors. Published by Elsevier B.V. All rights reserved.