Formation of biodegradable polymeric fine particles by supercritical antisolvent precipitation process

Abstract

The supercritical antisolvent (SAS) precipitation process as a "green" alternative to specialty particles recrystallization was successfully used to generate poly(L-lactide) acid (L-PLA) from dichloromethane (DCM) solution using CO2 as antisolvent. The influence of main operating parameters on the synthesis of L-PLA particles in the SAS process was methodically examined. In particular, antisolvent addition rate (30, 40, 50, and 60 g/min), temperature (35, 40°C, 45°C, and 50°C), solute concentration (50, 75, 100, and 150 mg/10 ml), and solution addition rate (1, 2.5, 5, and 7.5 ml/min). These parameters could be tuned to give a mean particle diameter of 0.62 μm. It was found using scanning electron microscopy and laser diffraction that increasing the antisolvent addition rate and the solution addition rate, while decreasing the temperature and solute concentration, led to a decrease in the L-PLA mean particle diameter. Furthermore, a unimodal particle size distribution was obtained at the higher solution and antisolvent addition rates. Spherical-like primary particles have been obtained in all the experimental runs; thus, no change of particle morphology with the process parameters has been noticed. These results manifested that SAS recrystallization process is a valuable technique to generate reproducibly polymer particles with controlled size and size distribution. © 2012 Society of Plastics Engineers.