Doxorubicin is a chemotherapeutic drug which can cause severe nausea during treatment to relieve the patient from nausea and vomiting effects we selected palonosetron drug. So we prepared and evaluated Bilayered tablets containing Doxorubicin SR and palonosetron IR layered tablets by wet granulation method. A new analytical method has been developed to estimate the doxorubicin and palonosetron and validated for the use in this study. The prepared formulations evaluated for physiochemical properties and found to be within limits. The optimized formulation F6 (palonosetron IR) contains the average thickness of 2.52±0.54 average hardness of 4.3±0.21, average weight of 151±0.06, friability of 0.41% and disintegration time 2min 30sec.The prepared dry mixer for the sustained release maintained the physiochemical properties of tablets such as thickness, hardness, weight variation, friability. The optimized formulation F5 (doxorubicin SR) contains the average thickness of 3.44±0.21average hardness of 7.1±0.55, friability of 0.31%. The F5 formulation which releases the doxorubicin in sustained manner in up to 12 hours and Palonosetron immediate release F6 formulation showed 98% drug release with in 60min. both optimised formulations are compressed together to prepare bilayer tablets and dissolution data of bilayer tablet proved there is no change in drug release profile, and FTIR studies proved no interaction between polymers and drug hence successful in developing bilayer tablet of doxorubicin and palonosetron.