Endocrine disrupting chemicals (EDCs), including bisphenol A (BPA), tert-nonylphenol (t-NP) in aqueous solutions, were extracted by cubic mesoporous silica material (MCM-48) and determined by high performance liquid chromatography--fluorometric detection simultaneously. The effect of eluent solvent and its volume, the pH of sample solution and the sample volume on the extraction recovery of MCM-48 composite for EDCs was investigated by the batch techniques. Comparative studies showed that MCM-48 was superior to C18 for the extraction of the more polar analyte bisphenol A and and at least as effective as C18 for the extraction of tert-nonylphenol. The results showed that the excellent recovery towards BPA (87.4%-95.6%) and t-NP (83.6%-96.3%) was achieved by using this method. The good linearity was obtained for BPA and t-NP (R2 > 0.993) at a range from 5 to 1000 μg L(-1). Under the optimum conditions, the detection limits of this method were 96 and 150 ng L(-1) for BPA and t-NP in water sample, based on a signal-to-noise ratio (S/N) of 3, respectively. This method has been also successfully applied for the determination of other EDCs in natural environmental water samples.