A new method for the determination of four endocrine disrupting compounds (EDCs) (bisphenol A, 17-β-estradiol, estrone and diethylstilbestrol) in water samples has been developed using polypropylene hollow-fiber-supported ionic liquid (IL, 1-Octyl-3-methylimidazolium hexafluorophosphate, [C8MIM][PF6]) microextraction [HF-liquid-phase microextraction (LPME)] combined with high-performance liquid chromatography (HPLC)/UV. This method was used to investigate pollutants in surface water, on the Neijiang River, located at Zhenjiang, Jiangsu Province. Several parameters (sample pH, volume of accepter phase, ionic strength) were investigated. Under the optimum extraction conditions (sample pH, 2.0; volume of extraction solvent, 2.5 μL; ionic strength, 2.57) the proposed method offered: good linearity range, 0.15–100 μg L−1, with the correlation coefficients (r2) of 0.9996, 0.9994, 0.9990 and 0.9984, respectively; low limits of detection, 0.03, 0.05, 0.10, 0.05 μg L−1 (S/N = 3) for bisphenol A, 17-β-estradiol, estrone and diethylstilbestrol, respectively; good reproducibility (relative standard deviation (RSD), 8.41, 7.61, 9.00, 7.22%, respectively, n = 5); satisfactory recoveries (80.2–107.1%, n = 5); and high enrichment factors, 5,240, 3,693, 2,425 and 2,086, were achieved, for the four chemicals, respectively. Using the proposed HF-LPME, among 15 sampling sites along Neijiang River, bisphenol A, diethylstilbestrol and 17-β-estradiol were detected in some sites, all of which were the near suburban sampling sites. The results indicate that the role of municipal sewage is an important source of EDC contamination.

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