[en] Full text: From the combination of organic and inorganic materials hybrids with higher specific characteristics can be obtained, which makes it possible, for example, the application in pharmaceutical compositions due to the possibility of adjusting the control and evaluation of the effective concentration of drugs in organism through the controlled release. Chitosan, a biocompatible biopolymer, and phyllosilicates, minerals formed from silicates, are source examples that being used in pharmaceutical interests and which may prove even more interesting if their properties are combined. This work proposes the synthesis of magnesium phyllosilicate by the sol-gel route method with Tetraethyl Orthosilicate (TEOS) as source of Si and Magnesium Chloride Hexahydrate as source of Mg; obtaining the hybrid formed between this and the chitosan for evaluation the capacity of incorporation / release of amiloride as model drug. The systems were characterized by XRD, TG / DTG and FTIR. The release assay was performed on Hanson Research SR-8 Plus dissolver using apparatus I (basket), under stirring speed of 50 rpm and temperature of 37 ± 0.4 ° C, with a precisely weighed mass of samples containing the same drug content. 500 mL of phosphate buffer (0.1 mol L^-1, pH 7.4) was used as the dissolution medium, guaranteeing the sink conditions. The hybridization was successfully confirmed by the characterization techniques and the material obtained was shown a good adsorption capacity of amiloride, loading 55 mg g^-1, 49 mg g^-1 and 4 mg g^-1 for PhylQs, Phyl and Qs, respectively. The in vitro release tests of the developed systems showed a prolongation release rates of this drug for at least 4 h. This prolongation proposes the system developed as a system of sustained release of drugs, which implies in the slow and gradual release of the active substance favoring the maintenance of the plasma concentration within a therapeutic window. (author)