Based on the Polyethylene glycol (PEG)-salt aqueous two phase system (ATPS), a novel, green and economical approach was proposed for the chiral separation and determination of alpha-cyclohexyl-mandelic-acid (CHMA). The result showed that this new technique has good chiral recognition ability for CHMA. The separation factor, alpha, was affected by various factors, including the molecular weight of PEG, pH, temperature, the amount of Cu-2-beta-cyclodextrin, which influenced on either the formation of the host-guest complex or the distribution of the complex. In this work, Cu-2-beta-cyclodextrin was inclined to recognize R-CHMA. Under the optimum conditions, alpha could reached 1.36 after just one step extraction. This method has explored a new path for preparative separation of racemic compounds. (C) 2012 Elsevier B.V. All rights reserved.