Summary: 5‐Fluorouracil‐poly(L ‐lactide) (5‐Fu‐PLLA) microparticles have been prepared by an SEDS process. First, the 5‐Fu is successfully micronized and is then used to produce the 5‐Fu‐PLLA microparticles. The 5‐Fu‐PLLA microparticles synthesized by the SEDS process exhibit a rather spherical shape and a narrow particle size distribution, where it ranges from 615 to 1 990 nm, with a mean particle size of 980 nm. The dichloromethane residue in the 5‐Fu‐PLLA microparticles without any further treatment is 46 ppm. The average drug load and encapsulation efficiency of the 5‐Fu‐PLLA microparticles are 3.05 and 17.8%, respectively. The rate of drug release from the 5‐Fu‐PLLA microparticles shows mainly first‐order kinetics.