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Development and validation of a reversed‐phase liquid chromatographic method for analysis of demeclocycline and related impurities
Author(s) -
Kahsay Getu,
Maxa Jaroslav,
Van Schepdael Ann,
Hoogmartens Jos,
Adams Erwin
Publication year - 2012
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201101071
Subject(s) - chromatography , detection limit , impurity , chemistry , volumetric flow rate , analytical chemistry (journal) , acetonitrile , resolution (logic) , materials science , physics , organic chemistry , quantum mechanics , artificial intelligence , computer science
A simple, robust, and rapid reversedphase high‐performance liquid chromatographic method for the analysis of demeclocycline and its impurities is described. Chromatographic separations were achieved on a S ymmetry S hield RP8 (75 mm × 4.6 mm, 3.5 μm) column kept at 40°C. The mobile phase was a gradient mixture of acetonitrile, 0.06 M sodium edetate (pH 7.5), 0.06 M tetrapropylammonium hydrogen sulphate (pH 7.5) and water, A (2:35:35:28 v/v/v/v) and B (30:35:35:0 v/v/v/v) pumped at a flow rate of 1 mL/min. UV detection was performed at 280 nm. The developed method was validated according to the ICH guidelines for specificity, limit of detection, limit of quantification, linearity, precision, and robustness. An experimental design was applied for robustness study. Results show that the peak shape, chromatographic resolution between the impurities, and the total analysis time are satisfactory and better than previous methods. The method has been applied for the analysis of commercial demeclocycline bulk samples available on the market.