This paper presents two techniques for microencapsulation of bovine serum albumin (BSA), namely, solvent evaporation and in situ polymerization. Both these processes have been designed to give improved loading and release rates. We achieved high encapsulation efficiency with high microcapsule yield using high power ultrasonication for formation of microemulsion and an efficient microsprayer for the formation of double emulsion. In situ polymerization in the organic (methyl methacrylate, MMA) liquid membrane of the microemulsion was conducted in inert atmosphere. Both the methods are cost-effective and may be designed for predetermined release of the biomaterials.