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Survey and qualific...
Survey and qualification of internal standards for quantification by 1H NMR spectroscopy
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Rundlöf, Torgny (author)
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Mathiasson, Marie (author)
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- Bekiroglu, Somer (author)
- Uppsala universitet,Avdelningen för analytisk farmaceutisk kemi
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- Hakkarainen, Birgit (author)
- Uppsala universitet,Avdelningen för analytisk farmaceutisk kemi
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- Bowden, Tim (author)
- Uppsala universitet,Polymerkemi
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- Arvidsson, Torbjörn (author)
- Uppsala universitet,Avdelningen för analytisk farmaceutisk kemi
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(creator_code:org_t)
- Elsevier BV, 2010
- 2010
- English.
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In: Journal of Pharmaceutical and Biomedical Analysis. - : Elsevier BV. - 0731-7085 .- 1873-264X. ; 52:5, s. 645-651
- Related links:
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https://urn.kb.se/re...
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https://doi.org/10.1...
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Abstract
Subject headings
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- 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.
Subject headings
- MEDICIN OCH HÄLSOVETENSKAP -- Medicinska och farmaceutiska grundvetenskaper -- Läkemedelskemi (hsv//swe)
- MEDICAL AND HEALTH SCIENCES -- Basic Medicine -- Medicinal Chemistry (hsv//eng)
- NATURVETENSKAP -- Kemi -- Polymerkemi (hsv//swe)
- NATURAL SCIENCES -- Chemical Sciences -- Polymer Chemistry (hsv//eng)
Keyword
- Nuclear magnetic resonance spectroscopy
- Quantification
- Internal reference standard
- Absolute purity
- Pharmaceutical chemistry
- Farmaceutisk kemi
- Polymer chemistry
- Polymerkemi
- Analytical Pharmaceutical Chemistry
- Analytisk farmaceutisk kemi
- Chemistry with specialization in Polymer Chemistry
- Kemi med inriktning mot polymerkemi
Publication and Content Type
- ref (subject category)
- art (subject category)
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