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A delicate method was developed for simultaneous analysis of 16 illegal residual beta-agonists in pork tissues including liver, kidney and meat. The samples were subjected to enzymatic hydrolysis, extracted with perchloric acid. and then dual Oasis HLB and MCX solid phase extraction (SPE) cartridges were used for cleanup. The analytes were quantified by ultra performance liquid chromatography coupled with electrospray ionisation tandem mass spectrometry (UPLC-ESI-MS/MS) operating in positive multiple-reaction mode (MRM). Matrix-fortified calibration curves were performed to compensate for the matrix effect and loss in sample preparation. CC alpha and CC beta of the analytes upon the method ranged from 0.02 to 0.79 mu g/kg and from 0.04 to 1.62 mu g/kg. respectively. (C) 2008 Elsevier Ltd. All rights reserved.