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PROBLEM TO BE SOLVED : To improve the yield and space-time yield of an unsaturated nitrile and control the ratio of oxidative decomposition of ammonia into nitrogen by using an oxide catalyst obtained by a process in which an oxide containing molybdenum, vanadium, and antimony, after being brought into contact with a basic aqueous solution, is burned. SOLUTION : In the production an unsaturated nitrile by the gas-phase catalytic ammoxidation of propane and isobutane, an oxide having a composition expressed by the formula : MolVaSbbZcOn (wherein Z is at least one element selected from Nb, W, Cr, rare earth elements, alkaline earth metals, and others; a to c represent an atomic ratio per one Mo atom and 0.1<=a<=1, 0.01<=b<=0.6, 0<=c<=1, and n is an atomic ratio determined by the oxidation state of the metals) is brought into contact with a basic aqueous solution, which is separated/removed. In this way, an unsaturated nitrile is produced at a low temperature in a high yield with the use of a catalyst which contains antimony and is low in volatility.