A novel method was developed for the simultaneous determination of 2,4-dichlorophenol, 2,4, 6-trichlorophenol and pentachlorophenol in surface water by HPLC-MS/MS with solid phase extraction. The sample was concentrated by HLB extraction cartridge, and then eluted with dichloromethane and acetone eluants. The solvent was changed into methanol after drying by nitrogen blow. Quality and quantity analysis was carried out by HPLC-MS/MS with SRM mode. Under the experimental condition, the linear regress equations were Y = 2524 X = 6029, Y = 1809X - 11341 and Y = 2296X - 2894, the correlation coefficients were 0.9993, 0.9996 and 0.9989, the detection limits were 2.0, 3.0 and 0.1 mu g/L, the limits of quantification were 6.7, 10.1 and 0.32 ng/L respectively, and a recovery ranged of 70.5% 102.3% with a RSD between 2.2% and 14.7% (n = 7) were obtained. The method has good innovative, advanced and practical value.