The study based on the chemiluminescence (CL) reaction of potassium ferricyanide and luminol in sodium hydroxide medium, enrofloxacin (ENRO) could dramatically enhance CL intensities and incorporated with matrix solid-phase dispersion (MSPD) technique (Florisil used as dispersant, dichloromethane eluted the target compounds). A simple flow injection chemiluminescence (FL-CL) method with MSPD technique for determination of ENRO in eggs was described. Under optimal conditions, the CL intensities were linearly related to ENRO concentration ranging from4.0×10-8 g.L−1to5.0×10-5 g.L−1, with a correlation coefficient of 0.9989 and detection limit of5.0×10-9 g.L−1. The relative standard deviation was 3.6% at an ENRO concentration of2.0×10-6 g.L−1. Our testing technique can help ensure food safety, and thus, protect public health.