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Survey and qualification of internal standards for quantification by 1H NMR spectroscopy
Uppsala University, Disciplinary Domain of Medicine and Pharmacy, Faculty of Pharmacy, Department of Medicinal Chemistry, Analytical Pharmaceutical Chemistry.
Uppsala University, Disciplinary Domain of Medicine and Pharmacy, Faculty of Pharmacy, Department of Medicinal Chemistry, Analytical Pharmaceutical Chemistry.
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2010 (English)In: Journal of Pharmaceutical and Biomedical Analysis, ISSN 0731-7085, E-ISSN 1873-264X, Vol. 52, no 5, p. 645-651Article in journal (Refereed) Published
Abstract [en]

In quantitative NMR (qNMR) selection of an appropriate internal standard proves to be crucial. In this study, 25 candidate compounds considered to be potent internal standards were investigated with respect to the ability of providing unique signal chemical shifts, purity, solubility, and ease of use. The 1H chemical shift (δ) values, assignments, multiplicities and number of protons (for each signal), appropriateness (as to be used as internal standards) in four different deuterated solvents (D2O, DMSO-d6, CD3OD, CDCl3) were studied. Taking into account the properties of these 25 internal standards, the most versatile eight compounds (2,4,6-triiodophenol, 1,3,5-trichloro-2-nitrobenzene, 3,4,5-trichloropyridine, dimethyl terephthalate, 1,4-dinitrobenzene, 2,3,5-triiodobenzoic acid, maleic acid and fumaric acid) were qualified using both differential scanning calorimetry (DSC) and NMR spectroscopy employing highly pure acetanilide as the reference standard. The data from these two methods were compared as well as utilized in the quality assessment of the compounds as internal standards. Finally, the selected internal standards were tested and evaluated in a real case of quantitative NMR analysis of a paracetamol pharmaceutical product.

Place, publisher, year, edition, pages
2010. Vol. 52, no 5, p. 645-651
Keywords [en]
Nuclear magnetic resonance spectroscopy, Quantification, Internal reference standard, Absolute purity
National Category
Medicinal Chemistry Polymer Chemistry
Research subject
Analytical Pharmaceutical Chemistry; Chemistry with specialization in Polymer Chemistry
Identifiers
URN: urn:nbn:se:uu:diva-122025DOI: 10.1016/j.jpba.2010.02.007ISI: 000276785400001OAI: oai:DiVA.org:uu-122025DiVA, id: diva2:308117
Available from: 2010-04-06 Created: 2010-04-06 Last updated: 2018-01-12Bibliographically approved

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Bowden, Tim

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