Chromatographic micro-preparative separation of a racemic mixture of naproxen enantiomers using a chiral stationary phase of Chiralcel OJ-H has been studied. Optimum conditions for the separation have been found. It is shown that a special fraction collection scheme involving an intermediate region between the minimum between peaks and the maximum of the second peak should be used for the simultaneous recovery of both enantiomers. In this case, S-(0.12 mg) and R-naproxen (0.12 mg) with a purity of up to 99.4 and 94.5%, respectively, can be isolated in one run using a standard analytical column.