Mixed valence manganite materials have been studied due to their interesting physical properties such as their magnetoresistance (MR) effect. The change of Mn3+ /Mn4+ ratio affects the possible bonds between anion and cation and their spin structure that may occur in the samples. The aim of this research is to study the change of magnetoresistance effect and magnetic properties of La0.67Sr0.33MnO3 (LSMO) by doping the Mn site with Ni ion. La0.67Sr0.33Mn1-xNixO3 samples were synthesized by using sol-gel method and characterized by using X-ray diffractometer (XRD) and Energy Dispersive X-ray spectroscopy (EDX) to confirm whether Ni has been doped successfully to the parental compound or not. XRD results showed that the samples have a single phase and Ni peak has been detected in the EDX result of Ni-doped LSMO. Resistivity and magnetic measurement showed that LSMO material has ferromagnetic metallic behavior, while x = 0.20 Ni-doped LSMO sample showed paramagnetic insulator behavior. The absolute value of the MR for un-doped sample is higher than the doped sample when the low field is applied, while under the influence of the high magnetic field, it become smaller than the doped sample.