Based on the inhibition by hydroquinone, catechol and resorcinol of chemiluminescence from luminol potassium hexacyanoferrate(Ⅲ) system, a high performance liquid chromatographic procedure with chemiluminescent detection was developed for simultaneous determination of hydroquinone, catechol and resorcinol. The separation was carried out on RP C 18 column at 37 ℃ by using a step gradient elution made by the mobile phases of methanol(A) and 0 05% H 3PO 4(B). The gradient elution condition was 95% B, 5 min; 95%B 50%B, 1 min; 50% B, 6 min. This method has the merits of high senstivity and good selectivity. The detection limits for hydroquinone, catechol and resorcinol are 2 0×10 -9 , 3 2×10 -9 and 6 8×10 -7 g/mL, respectively. The relative standard deviation( n =5) is 1 9% for 2 5×10 -7 g/mL hydroquinone, 1 0% for 7 5×10 -7 g/mL catechol, 4 0% for 5 0×10 -5 g/mL resorcinol, respectively. The recovery is in the range of 94%—104%. [WT5HZ]