The current investigation reports an effective adsorption of anionic species on [Zn-Al-CO3] and [Mn-Al-CO3] hydrotalcite-like compounds, as novel, inexpensive available alternative to the commercial hydrotalcite. LDH [Zn-Al-CO3] and [Mn-Al-CO3] were synthesized by co-precipitation at constant pH with a molar ratio of 2:1. Their calcinations lead to the formation of mixed oxides exhibiting fine dispersion of metal cations and high surface area. The structural characterization of materials was carried out by X-ray diffraction, infrared spectroscopy (FTIR) and DTA/GT. The assay of the solutions was monitored by UV-Vis spectrometry. The removal of Trypan blue from aqueous solutions by adsorption onto hydrotalcite particles was investigated using batch rate experiments. The sorption process was also found to be influenced by contact time and solution pH. A comparative study of calcined and uncalcined LDH was performed. The adsorption kinetics study showed that the Pseudo-second-order kinetic model could be used to describe the adsorption of Trypan blue satisfactorily.