A simple room temperature solution-based method for the preparation of highly porous iron(III) benzenetricarboxylate coordination polymer films on the internal surface of a macroporous polystyrene-divinylbenzene-methacrylic acid polymer is reported. The resulting metal-organic polymer hybrid (MOPH) maintains a high specific micropore surface area of 389 m(2) g(-1) and thermal stability above 250 degrees C in air. The MOPH preparation is readily adapted to a capillary column, yielding a flow-through separation device with excellent flow permeability and modest back-pressure. The excellent separation capability of the MOPH column is demonstrated by enriching phosphopeptides from mixtures of digested proteins. This approach to MOPH synthesis is easily implemented and likely adaptable to a wide range of coordination polymers and metal-organic frameworks.