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Merck
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  • Thin-layer chromatography-densitometric measurements for determination of N-(hydroxymethyl)nicotinamide in tablets and stability evaluation in solutions.

Thin-layer chromatography-densitometric measurements for determination of N-(hydroxymethyl)nicotinamide in tablets and stability evaluation in solutions.

Journal of AOAC International (2008-11-05)
Urszula Hubicka, Jan Krzek, Justyna Luka
摘要

A thin-layer chromatography (TLC)-densitometric method was developed to determine N-(hydroxymethyl)nicotinamide in tablets and basic solutions along with nicotinic acid. Analysis was performed on silica gel F254 plates using chloroform-ethanol (2 + 3, v/v) mobile phase. The densitometric observations were made at 260 nm. The results showed good precision and accuracy; relative standard deviation was 2.37%, and recovery ranged from 97.60 to 100.82%. The limit of detection was 0.1 microg/spot, while the linearity range was from 0.2 to 1.75 microg/spot. Applicability of the newly developed method was tested for determination of N-(hydroxymethyl)nicotinamide in the preparation Cholamid. Densitometric measurements were used to evaluate stability of N-(hydroxymethyl)nicotinamide in basic solutions. It was found that decomposition corresponded to first-order reaction kinetics. The computed kinetic and thermodynamic parameters at 30 degrees C were as follows: k = 0.00675/min, t0,5 = 1.71 h, t0,1 = 0.26 h, and Ea = 44.75 kJ/mol.