In order to increase the recoveries of steroid estrogens (SEs) for quantitative determination in sewage, response surface methodology (RSM) was adopted to optimize the solid-phase extraction (SPE) procedure. Quadratic models were established for predicting SE recoveries, and the effectiveness of models and the interaction of factors were analyzed. SE concentrations of typical sewage treatment plants (STPs) in Jiangsu province were detected under the optimized conditions. The optimal operating conditions of SPE were obtained with elution volume of 10.68 mL, a sample rate of 10.47 mL·min^-1 and elution rate of 4.07 mL·min^-1. The predicted recoveries were 81.63% for E1, 88.86% for E2, and 84.55% for EE2. SEs were detected in all the three STPs, and concentrations in the influents and effluents ranged from 13.4 to 78.0 ng·L^-1 and from 5.3 to 20.5 ng·L^-1, respectively.