期刊
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
卷 52, 期 5, 页码 645-651出版社
ELSEVIER SCIENCE BV
DOI: 10.1016/j.jpba.2010.02.007
关键词
Nuclear magnetic resonance spectroscopy; Quantification; Internal reference standard; Absolute purity
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 H-1 chemical shift (delta) 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-d(6), CD3OD, CDCl3) wet e 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 (C) 2010 Elsevier B V All rights reserved
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