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Survey and qualification of internal standards for quantification by 1H NMR spectroscopy
Uppsala universitet, Medicinska och farmaceutiska vetenskapsområdet, Farmaceutiska fakulteten, Institutionen för läkemedelskemi, Avdelningen för analytisk farmaceutisk kemi.
Uppsala universitet, Medicinska och farmaceutiska vetenskapsområdet, Farmaceutiska fakulteten, Institutionen för läkemedelskemi, Avdelningen för analytisk farmaceutisk kemi.
Vise andre og tillknytning
2010 (engelsk)Inngår i: Journal of Pharmaceutical and Biomedical Analysis, ISSN 0731-7085, E-ISSN 1873-264X, Vol. 52, nr 5, s. 645-651Artikkel i tidsskrift (Fagfellevurdert) 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.

sted, utgiver, år, opplag, sider
2010. Vol. 52, nr 5, s. 645-651
Emneord [en]
Nuclear magnetic resonance spectroscopy, Quantification, Internal reference standard, Absolute purity
HSV kategori
Forskningsprogram
Analytisk farmaceutisk kemi; Kemi med inriktning mot polymerkemi
Identifikatorer
URN: urn:nbn:se:uu:diva-122025DOI: 10.1016/j.jpba.2010.02.007ISI: 000276785400001OAI: oai:DiVA.org:uu-122025DiVA, id: diva2:308117
Tilgjengelig fra: 2010-04-06 Laget: 2010-04-06 Sist oppdatert: 2018-01-12bibliografisk kontrollert

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