A highly efficient microwave-assisted synthesis of an LED-curable methacrylated gelatin for bio applications.

This study deals with the development of an LED-curable methacrylated gelatin (GelMA) synthesis via microwave (MW) irradiation with a reaction and purification time-, energy-, and methacrylation reagent-saving approach. To investigate the efficiency of MW irradiation in GelMA synthesis, characteristics of the GelMAs prepared by using glycidyl methacrylate (GMA) or methacrylic anhydride (MA) via the MW-assisted (MWA) method were compared comprehensively with those synthesized via the conventional heating method. Moreover, MWA reaction conditions were optimized in terms of methacrylation reagent concentrations ( C ), reaction time ( t ), and MW power ( P ). Characterization and assessment of the GelMAs were conducted with 1 H NMR, FT-IR, and Raman spectroscopy along with physical-mechanical, thermal, and hydrophilicity analysis. The results demonstrated that the MWA synthesized GMA-GelMA hydrogels were possessed of increased methacrylation degree (MD), gel fraction (GF), tensile strength (TS), elongation at break (EB), glass transition temperature ( T g ), and water contact angle (WCA) as well as decreased swelling degree (SD) values in comparison to those of MA-GelMA and GMA-GelMA hydrogels prepared via the MWA and conventional method, respectively. Enhanced properties of the MWA synthesized GMA-hydrogels suggested an effective methacryloyl conjugation leading to a greater amount of covalent crosslinking density justified by the dipolar moment calculations. Optimal GMA C , t , P , and purification time for a highly crosslinked GelMA hydrogel (MD: 96.1%, GF: 98.3%, SD: 10.11%, TS: 6.7 MPa, EB: 175.2%, T g : 75.34 °C, and WCA: 72.22°) were found to be a 5 times molar excess over the primary amine groups of gelatin, 5 min, 500 W, and 24 h, respectively. Thus, the optimized MW conditions offer a promising green method to prepare GelMAs for bio applications.