Off-line coupling of two analytical methods: thin-layer chromatography (TLC) and atomic absorption spectrometry (AAS) was investigated for preliminary stability studies of zinc carboxylato complexes bound to nicotinic acid and their chromatographic separation on a Silufol layer. Zinc content, determined by an AAS method in fractions scrapped off the layers after zinc carboxylato complex (ZC) chromatographic analyses responds to ZC dissociation during chromatographic process. It was found that solute chromatographic stability is influenced substantially by the concentration of organic modifier in the eluent. To reveal relations between zinc distribution, corresponding solute retention and complex stability was the main aim of the presented paper.