Natural polymers are superior compared with synthetic polymers when used in medical applications, especially if they are already present in the human body.The current work involves the production of microspheres from bio-natural polymer (Dextrin maize starch) as primary material and Poly (vinyl alcohol) PVA or PEG by using aqueous two phase system (ATPS) technique. PEG and PVA of 2, 2.5, 3 wt% was mixed with 18% Dextrin using sonication process and then stirred for 20 hr at 5°C. Different samples taken after 4, 8, 12, 16, and 20 hr during stirring process for each concentration.The effect of changing the rheological properties on the specification conditions similar to human body conditions (PBS, pH = 7.4, T = 37 ºC) and stability studied. Microspheres were also, loaded by insulin and study the effect of changing pH to simulate body conditions and release control.Optical Microscope (OM), Atomic Force Microscope (AFM), Cone-plate, Zeta Potential (ZP), Fourier Transform Infrared (FTIR), Dynamic light Scattering (DLS), pH Matter, Scanning Electron Microscope (SEM) and Ultra Violet (UV) characterizations techniques have been used to characterize the microspheres.