A　boronate　ACE　coupled　with　chemiluminescence　(CL)　detection　was　developed　for　sensitive　determination　of　three　isomeric　benzenediols,　which　was　based　on　the　principle　of　an　inhibited　effect　of　borate　complexation　on　the　CL　reaction　between　luminol　and　potassium　hexacyanoferrate　(K3Fe(CN)(6))　in　alkaline　solution.　The　effects　of　some　important　factors　on　CE　separation　and　CL　intensity　were　systemically　investigated.　Baseline　separation　of　isomeric　benzenediols　including　o-benzenediol,　m-benzenediol,　and　p-benzenediol　was　achieved　by　using　a　mobile　phase　of　40　mmol/L　glycine-NaOH　buffer　at　pH　9.4　containing　0.8　mmol/L　luminol　and　0.4mol/L　4-iodophenylboronic　acid.　The　calibration　curves　of　the　analytes　by　plotting　the　peak　height　against　corresponding　concentration　were　linear　over　the　range　of　4.5　x　10(-8)　approximate　to　4.5　x　10(-5)mol/L　for　p-benzenediol,　6.8x10(-8)approximate　to　2.7x10(-5)mol/L　for　m-benzenediol,　and　9.0x10(-8)　approximate　to　4.5x10(-5)mol/L　for　o-benzenediol.　The　corresponding　detection　limits　for　p-,　m-,　and　o-benzenediols　were　2.8x10(-8)mol/L　(68　amol),　3.2　x　10(-8)mol/L　(108.4amol),　and　3.7　x　10(-8)mol/L　(125.8　amol;　S/N=　3),　respectively.　The　proposed　method　has　been　successfully　applied　to　the　analysis　of　trace　benzenediols　in　spiked　human　urine　sample　and　the　recoveries　were　＞97.2%.　Our　primary　result　demonstrated　the　proposed　CE-CL　method　has　great　potential　for　biomarker　determination　in　clinical　diagnosis.