D-γ-tocotrienol (G-T3) chiefly present in palm oil has stolen the spotlight as a promising radiation protective agent for the treatment of acute radiation syndrome (ARS). Although G-T3 is a promising counteracting agent discovered, the separation and purification from its matrix are painstaking. These have limited its characterization, derivatization, and biomedical application. In this study, we developed chromatographic and distillation methods to enhance the purity and synthesis of G-T3 derivatives. Exactly 8% ethyl acetate (EA) in hexanes used in TLC resulted in right spots separation. Two gradient column chromatographic methods were examined using solvent mixtures of EA/hexanes and EA/petroleum ether (PE), respectively. We verified that a gradient elution with EA in PE led to the maximum purity (≥95%) based on the NMR and GC-MS outcomes. Also, G-T3 was stable in an emulsion to some extent, and some soluble G-T3 derivatives were synthesized, and their structure was confirmed