A novel reverse microemulsion approach for the synthesis of LDH nanoplatelets has been developed. The method employs oleylamine which performs multiple functions, acting as the oil phase, base and the surfactant. MgAl-LDH nanoplatelets have been prepared with mean diameters (μ) of 49.2, 64.0 and 75.4 nm with standard deviations (σ) of 15.0, 17.2, and 16.0 nm respectively. AFM studies show that on average the nanoplatelets comprise of 14, 20 and 35 layers respectively. The observed mean diameter and thickness of the isolated LDH nanoparticles is linearly dependent on the oleylamine–water ratio.