A　new　pressure-assisted　capillary　electrochromatography　coupled　with　electrospray　ionization-mass　spectrometry　method　using　a　silica-based　monolithic　column　as　separation　media　was　developed　for　the　analysis　of　beta(2)-agonists　in　human　urine.　Experimental　conditions　including　the　mobile　phase,　separation　voltage,　assisted　pressure,　and　sheath　liquid　were　optimized　for　the　analysis:　mobile　phase　composed　of　82%　(v/v)　ACN　and　18%　(v/v)　20　mmol/L　ammonium　acetate　(pH　6.0);　separation　voltage　25　kV;　assisted　pressure　2　bar;　and　the　sheath　liquid　consisting　of　7　5　mmol/L　acetic　acid　in　isopropanol/water　50/50%　(v/v)　that　was　delivered　at　a　flow　rate　of　3　0　mu　L/min.　Six　beta(2)-agonists　were　separated　within　12　5　min　with　LODs　(defined　as　S/N　=　3)　in　the　range　of　0.25-20　ng/mL　The　absolute　LODs　of　the　developed　method　for　analyzing　six　beta(2)-agonists　ranged　from　5　75　to　46　0　fg　Method　repeatability　of　run-to-run　and　column-to-column　was　satisfactory.　The　recovery　obtained　from　the　analysis　of　spiked　urine　samples　was　between　88.2%　and　106%　with　RSDs　lower　than　6　68%.　The　method　was　successfully　applied　to　the　analysis　of　real　urine　sample　from　volunteers　(C)　2010　Elseviei　B.V.　All　rights　reserved.