A novel radiochemical separation for 48 V radiotracer in no-carrier-added (NCA) form, via proton irradiation on Ti targets of natural isotopic composition has been developed. Metallic Ti targets irradiated with 21 MeV proton beam energy was submitted to a selective radiochemical separation consisting of an alkaline fusion-precipitation step, followed by column Chelex-100 chromatographic purification. Very high specific activity 48 V, at levels of hundreds MBq . µg -1 was prepared. Chemical analysis of radiotracer was carried out by ET-AAS and INAA. The decontamination factor from Ti target was 5 . 10 5 , with an overall radiochemical yield for 48 V larger than 90p. The NCA 48 V has used for labeling a range of chemical forms of V(III, IV, V) and applied in the study of metabolic behavior of different chemical forms in in-vivo and in-vitro experiments on rats and cell cultures.