In this study, resin adsorption as a means to enrich rare stilbenes cajaninstilbene acid (CSA) and longistyline C (LLC), and coumarin cajanuslactone (CL) from pigeon pea leaves was investigated. Among widely used twenty macroporous adsorption resins, NKA-9 resin presented higher adsorption capacity and desorption ratio in static tests. The adsorption kinetic model fitted better depended on types of compounds and pH values. The experimental adsorption data were better fitted to Langmuir isotherm (R-2 0.921-0.991) than Freundlich isotherm (R-2 0.753-0.988). In order to optimize the operating parameters for separating CSA, LLC and CL, dynamic adsorption and desorption tests were carried out. After one run treatment with NKA-9 resin, the contents of GSA, LLC and CL in the product were 10.82-, 9.07- and 108.90-fold increased with recovery yields of 81.31%, 89.76% and 96.77%, respectively. Moreover, NKA-9 resin exhibited excellent reusability within at least five cycles of adsorption/desorption. The developed methodology is a promising basis for large-scale preparation of CSA, LLC and CL from pigeon pea leaves. (C) 2011 Elsevier B.V. All rights reserved.