A novel， simple and rapid method was established for the determination of estradiol（E2）， estradiol（E3） and estrone（E1） in water， based on solid-phase micro-extraction（SPME） using porous metal－organic framework MIL－101（Cr） filled syringe nylon filter combined with high performance liquid chromatography－fluorescence detector. Firstly， the MIL－101（Cr） powder material was prepared by the hydrothermal synthesis method， whose structure， crystal forms and surface properties were proved by characterization of X－ray diffraction（XRD）， scanning electron microscopy（SEM）， nitrogen adsorption－desorption isotherms and pore size distribution. Secondly， the integrity of the nylon membrane in the proposed SPME device was verified by simulating the solid-phase extraction process. Next， the dominant parameters affecting enrichment efficiency， including extraction speed， sample pH value， salt concentration， washing and desorption conditions were investigated. It was found that when the sample was set at pH 6.0， the salt concentration was 0， the syringe speed was 2.5 mL/min， the elution solvent was methanol， and the washing solvent was 2 mL of 10% methanol/H,2,O， the extraction effect for the three targets was the best. Under the optimized conditions， three target estrogens in 10 mL water sample could be adsorbed within 4 min and eluted within 1 min. This method showed good linear relationships in the range of 0.2－500 μg/L for E2 and E3， and 5－500 μg/L for E1， with their correlation coefficients（,r,2,） of 0.998 2－0.999 3. The limits of detection for three analytes were 0.05， 0.06 and 1.50 μg/L， respectively. The relative standard deviations（RSD） for intra-day（,n ,= 6） and inter-day（,n ,= 3） were in the ranges of 0.20%－3.2% and 5.9%－6.1%， respectively．The recoveries for all targets in water samples at three spiked levels ranged from 84.1% to 108%， with RSDs not more than 5.5%. The developed method is simple and sensitive， and could be used for the rapid determination and accurate quantification of estrogens in water samples. In this method， MIL－101（Cr） and nylon membrane showed a synergistic adsorption effect on estrogen， providing a new strategy for multi-objective purification and extraction from complex environmental samples.