A liquid-liquid extraction combined with derivatization and gas chromatography-mass spectrometry (GC-MS) method was developed for the determination of C4-C9 alkylphenols (APs, included 4-tert-butylphenol, 4-n-butylphenol, 4-n-pentylphenol, 4-n-hexylphenol, 4-n-heptylphenol, 4-n-octylphenol, 4-tert-octylphenol, 4-n-nonylphenol and 4-nonylphenol) and bisphenol A (BPA) in environmental water. The extraction solvent, extraction number, extraction time, extraction solvent volume, pH value, salt content, concentration degree and derivatization time were optimized. The target compounds were quantified by internal standard method. Results showed that the optimal extraction number, time, solvent volume, pH value and salt content were 2, 5 min, 30 ml, about 2 and 5 g, respectively, and derivatization time was 1 h at room temperature. Dichloromethane was selected as the extraction solvent and was concentrated to 0.5 mL in the process of concentration. The developed method was validated and showed good linearity (R2 > 0.995), low limit of detection (LOD, 0.002 µg/L–0.006 µg/L), and excellent recovery (68.0 %–122 %) and low relative standard deviation (0.67 %–13.7 %). The developed method was finally applied to groundwater, surface water, seawater and sewage samples in Dongying City located at Yellow River Estuary and some of these target compounds were detected. The measured values of 4-nonylphenol and BPA in these water samples were below their restrictive values of relevant directives at home and abroad.