The application of zeolite based molecular sieves as catalysts and sorbents in thin layer chromatography (TLC) has been investigated for a single step evaluation of porphyrins and calix (4) pyrroles by in situ synthesis from pyrrole with aromatic aldehydes and ketones under microwave irradiation. The molecular sieves used were microporous zeolites such as HZSM-5, HY, H beta and mesoporous MCM-41 material and the results are compared. Among the various sorbents studied, MCM-41 proves to be the potential candidate and offered quantitative conversions. This glass-backed zeolite coated TLC plate presumably acted as a reactor and facilitated simultaneous chromatographic separation of the macrocycles as well. The process is simple, economically viable, rapid, selective, solvent free and finds a novel application in high through put parallel synthesis and chromatographic screening in a single step. (c) 2007 Elsevier B.V. All rights reserved.