Layered double hydroxides (LDHs) can be structurally described as the stacking of positively charged layers with hydrated anions intercalated in the interlamellar domain. LDHs are a class of materials represented by the general formula: [{\\rm M}_{1-{\\rm x}}^{2+} {\\rm M}_{\\rm x}^{3+} ({\\rm OH}){}_2] {\\rm A}_{{\\rm x/m}}^{{\\rm m}-} \\cdot {\\rm nH}_2 {\\rm O} where: M 2+ is a bivalent cation; M 3+ is a trivalent cation; A is an anion with m m charge. We have studied the intercalation and "in vitro" liberation of aspartic and glutamic amino acids in Mg-Al-LDHs. LDHs intercalated with this type of anions could combine both the compound and the LDH properties. The materials were prepared by the coprecipitation method under constant pH, followed by a hydrothermal treatment for 18 hours, and subsequent characterisation of intercalated materials using PXRD, ATG/DTA and FT-IR. Studies of "in vitro" liberation were made by determination of amino acid concentrations in solution through UV-VIS (nynhydrin methods). Moreover, simultaneous pH monitoring was conducted during the experiment.