Zein is a promising natural biodegradable polymer and regarded as a hydrophobic protein. However, electrospun structures prepared from Zein have poor mechanical and wetting properties. Cellulose Acetate (CA) is an economical biodegradable polymer having good mechanical and water retention properties. The aim of present study was to fabricate a novel material by electrospinning Zein/CA polymer blends. A series of Zein/CA hybrid nanofibers was electrospun and characterized. The ATR-FTIR spectrum showed the characteristic peaks of both Zein and CA, and was composition dependent. TGA studies confirmed that the Zein/CA hybrid nanofibers have a higher degradation temperature and better thermal stability than pristine Zein nanofibers. Zein/CA hybrid nanofibers have hydrophilic surface character as revealed by water contact angle (WCA) analysis. SEM imaging showed bead free morphology of the electrospun nanofibers. The electrospun Zein/CA hybrid nanofibers may be used for tissue engineering scaffolds and for other biomedical materials. Keywords: Zein; cellulose acetate; hybrid nanofibers; electrospinning; scaffold.