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A high performance liquid chromatography-ion trap mass spectrometric method combined with the technique of solid phase extraction had been developed for the determination of 12 beta(2)-agonists and 4 beta-blockers in urine samples. Urine samples were enzyme hydrolyzed by beta-glucuronidase/arylsulfatase, then extracted and deproteinized by perchloric acid, and then cleaned up by Waters Oasis HLB and MCX solid phase extraction cartridges. The separation was performed on an Atlantis T3 chromatographic column with gradient elution using methanol and water containing 0.1% formic acid. EST source performed under positive mode was used for the monitoring of the granddaughter ions. The linear ranges for 12 beta(2)-agonists and 4 beta-blockers were 0.005-0.160 mg/L and the correlation coefficients were not less than 0.995. The detection limits of 12 beta(2)-agonists and 4 beta-blockers were less than 0.2 mu g/kg. The pooled standard solution was added into blank urine samples at levels of 0.005, 0.01 and 0.02 mg/L, and the recovery rates were ranged from 41.2% to 88.2% with the relative standard deviations of 12.7%-19.2%. The method is easy, fast, sensitive, and suitable for confirmation and quantification of 12 beta(2)-agonists and 4 beta-blockers in urine samples.