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Graphical abstract Figure. No Caption available. HighlightsChitosan/PEO nanofibrous mats were crosslinked by tripolyphosphate solution.Prepared mat was used as a floating gastro‐retentive delivery system for ranitidine.Structural characteristics of nanofibers were evaluated using different techniques.Swelling profile of the prepared nanofibers were investigated at different media.Release profile of the nanofibrous mats were studied at different physiological pH. Abstract The present study describes the fabrication of Tripolyphosphate (TPP)‐crosslinked nanofibrous mats based on chitosan for use as a floating gastro‐retentive delivery system. TPP‐crosslinked chitosan (CH)/poly (ethylene oxide) (PEO)‐ ranitidine hydrochloride (RH) electrospun nanofibers (75.27 ± 2.10 nm) were prepared by electrospinning 70% v/v acetic acid solutions, and followed by crosslinking by TPP anions. The mechanical, structural and morphological properties of the prepared nanofibers were evaluated via tensile testing, XRD, FT‐IR, TGA, NMR, AFM and SEM experimental techniques. The prepared nanofibrous mats showed a pH sensitive swelling profile with maximum water absorbing at pH 1.2. Results obtained from above experimental techniques indicated that crosslinking process did not significantly altered morphological property of nanofibers but rather decreased their diameter and swelling degree, and increased their mechanical properties, thermal stability and bioadhesive strength. Viscosity measurements showed that the addition of PEO and RH to the chitosan solution, depending to its concentration lead to decrease in the viscosity of its solution. Also, floating test showed that the prepared nanofibrous mats remain floated onto surface of the dissolution medium for more than 48 h. Based on in‐ vitro drug release data analysis, TPP‐crosslinked CH/PEO nanofibrous mats decreased initial burst release and it was exhibited a sustained release profile for the RH from the TPP‐crosslinked CH/PEO‐RH electrospun nanofibrous mats.