Disclosed is a process for preparing an oxycodone salt having an amount of 14-hydroxycodeinone of less than 25 ppm, which process comprises the steps of: (a) preparing a mixture of oxycodone free base, solvent and an acid, wherein the oxycodone free base has an 8a,14-dihydroxy-7,8-dihydrocodeinone component (b) incubating the mixture under conditions suitable to convert the oxycodone free base to an oxycodone salt, wherein said conditions promote an acid catalysed dehydration consisting of conversion of the 8a,14-dihydroxy-7,8-dihydrocodeinone component to 14-hydroxycodeinone and (c) preferentially removing the 14-hydroxycodeinone from the oxycodone salt, wherein the resultant oxycodone salt contains 14-hydroxycodeinone in an amount less than about 25 ppm and wherein the mixture of step (a) has a pH of about 1 or less. Also disclosed is an oxycodone salt composition having an amount of 14-hydroxycodeinone of less than 25 ppm, wherein at least a portion of the 14-hydroxycodeinone is derived from 8a,14-dihydroxy-7,8-dihydrocodeinone.
