In this study, poly(D,L-lactic acid)–polyethylene glycol–poly(D,L-lactic acid), hereafter referred to as PDLLA–PEG–PDLLA, triblock copolymer membranes were prepared by electrospinning. Scanning electron microscopy images revealed the morphology of the microfibers, which had a diameter ranging from 300 to 900 nm. Fourier transform infrared spectroscopy was employed for structural analysis of the PDLLA–PEG–PDLLA/florfenicol (FF) membranes, which exhibited three absorption peaks at 3455, 1684, and 1533 cm−1, respectively, indicating that the triblock copolymer and FF are very well blended in the composite membranes. Differential scanning calorimetry revealed that weak interaction possibly decreased the activity of the segment and elevated the T g from 43 °C to 46 °C. From the in vitro dissolution tests, PDLLA as a biodegradable and biocompatible polymer can improve the solubility of FF. The rate of drug release increased with increasing PEG proportion. Furthermore, tensile and nanoindentation tests demonstrated that nanofibers exhibit mechanical properties such as tensile stress (700–2800 KPa), strain (40–120%), and good toughness (0.28–0.98 GPa). In conclusion, PDLLA–PEG–PDLLA nanofibers as a carrier improve the solubility of FF and control drug release.
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