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  • 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.

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.

Journal of pharmaceutical and biomedical analysis (2013-11-05)
Michael Weber, Christine Hellriegel, Alexander Rueck, Juerg Wuethrich, Peter Jenks
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.

MATERIALS
Product Number
Brand
Product Description

Supelco
Methyl 3,5-dinitrobenzoate, Standard for quantitative NMR, TraceCERT®
Sigma-Aldrich
Potassium phthalate monobasic, puriss. p.a., ≥99.5% (T)
Supelco
Phosphonoacetic acid, TraceCERT®, 31P-qNMR Standard
Supelco
Triphenyl phosphate, TraceCERT®, 31P-qNMR Standard
Supelco
Dimethylmalonic acid, Standard for quantitative NMR, TraceCERT®
Supelco
Thymol, Standard for quantitative NMR, TraceCERT®
Supelco
Benzoic acid, Standard for quantitative NMR, TraceCERT®
Supelco
1,2,4,5-Tetrachloro-3-nitrobenzene, Standard for quantitative NMR, TraceCERT®
Supelco
Potassium phthalate monobasic, Standard for quantitative NMR, TraceCERT®
Supelco
L-Glutamic acid, certified reference material, TraceCERT®
Supelco
Duroquinone, Standard for quantitative NMR, TraceCERT®
Supelco
Ethylene carbonate, Standard for quantitative NMR, TraceCERT®
Supelco
Ethyl 4-(dimethylamino)benzoate, Standard for quantitative NMR, TraceCERT®
Supelco
1,2,4,5-Tetramethylbenzene, Standard for quantitative NMR, TraceCERT®
Supelco
Calcium formate, Standard for quantitative NMR, TraceCERT®
Supelco
Maleic acid, Standard for quantitative NMR, TraceCERT®
Supelco
Dimethyl terephthalate, Standard for quantitative NMR, TraceCERT®
Supelco
Dimethyl sulfone, Standard for quantitative NMR, TraceCERT®