In this study, six different organo-hydrogel containing Agar-Glycerol (AG) based Coconut Oil (CnO) were synthesized using different crosslinkers to ensure the controlled release of D-3 Vitamine and 5-Fluorouracil (5-Flu). Synthesized organo-hydrogels were characterized by FT-IR, Afterwards, swelling behaviors were investigated in ethanol, acetone, ethanol/ID water (1:1), acetone /ID water (1:1) and gasoline environments and different pH. As a result of hemolysis, blood clotting and antioxidant analysis, organo-hydrogels have been shown to have blood compatibility and antioxidant properties. The effects of the initial pH of the solution on the drug release process were investigated. It was observed that the most release occurred at pH 2 and glutaraldehyde crosslinker. Release kinetics models were applied to understand the mechanism of the release system of D-3 Vitamine and 5-Flu (anti-cancer) with poly(Agar-co-Glycerol-co-Coconut Oil) (p(AG-co-CnO)) organo-hydrogel. The value of the correlation coefficient (R-2) was used as the best model fit indicator of different models and it was determined that the balance data fit the Korsmeyer-Peppas with large R(2)s and the Higuchi kinetic model. The results showed that the p(AG-co-CnO) organo-hydrogel can be used as a suitable carrier for the controlled release of D-3 Vitamin and 5-Flu.