A selective and sensitive method was developed based on dispersive micro-solidphase extraction for the extraction of hydroquinone, resorcinol, pyrocatechol and phenol from water samples prior to high-performance liquid chromatography with UV detection. SiO2, SiO2@MPTES, and SiO2@MPTES@Au nanoparticles (MPTES = 3-mercaptopropyltriethoxysilane) were synthesized and characterized by scanning electronic microscopy, thermogravimetric analysis, differential thermogravimetric analysis, and infrared spectroscopy. Variables such as the amount of sorbent (mg), pH and ionic strength of sample the solution, the volume of eluent solvent (L), vortex and ultrasonic times (min) were investigated by Plackett–Burman design. The significant variables optimized by a Box– Behnken design were combined by a desirability function. Under optimized conditions, the calibration graphs of phenol and dihydroxybenzenes were linear in a concentration range of 1–500 g/L, and with correlation coefficientsmore than 0.995. The limits of detection for hydroquinone, resorcinol, pyrocatechol, and phenol were 0.54, 0.58, 0.46, and 1.24 g/L, and the limits of quantification were 1.81, 1.93, 1.54, and 4.23 g/L, respectively. This procedure was successfully employed to determine target analytes in spiked water samples; the relative mean recoveries ranged from 93.5 to 98.9%.
