A new technique was proposed for the determination of alkylphenols, chlorophenols and bisphenol A in tap water samples. The sample preparation consists of a solid phase extraction (SPE) of alkylphenols, chlorophenols and bisphenol A from a water sample with XAD-4 and subsequent conversion to isobutyloxycarbonyl(isoBOC) derivatives or tert-butyldimethylsilyl(TBDMS) derivatives for sensitive analysis with the GC/MS-SIM mode. The recoveries were 86.6~105.2% (isoBOC derivatization) and 97.6~484.5%(TBDMS derivatization), respectively. The limit of quantitation of alkylphenols, chlorophenols and bisphenol A for SIM were 0.001~0.050㎍/l(isoBOC derivatization) and 0.003~0.050㎍/l(TBDMS derivatization). The SIM responses were linear with the correlation coefficient varying 0.9755~0.9981(isoBOC derivatization), and 0.9908~0.9996(TBDMS derivatization). When these methods were applied to tap water samples, the range of concentrations were 22.8~31.3 ng/l in 2,4-dichlorophenol, 28.6~70.3 ng/l in pentachlorophenol, 15.2~17.4 ng/l in t-butylphenol, 10.8~13.2 ng/l in t-octylphenol and 17.6~36.3 ng/l in bisphenol A, respectively.