A process for efficiently separating and recovering a ruthenium compound used as the catalyst in the production of adamantanols. The adamantanols are produced by hydroxylating an adamantane compound in the presence of a ruthenium compound and a salt of hypochlorous acid in a water/organic solvent two-phase system. The hydroxylation product liquid is added with an oxidizing agent to allow the ruthenium compound to be extracted into the organic phase. The ruthenium compound is separated and recovered from the organic phase. Alternatively, the ruthenium compound is back-extracted into the aqueous phase by adding an aqueous alkali solution to the organic phase. Then, the ruthenium compound is separated and recovered from the aqueous phase.