Preparation and characterization of magnetic chitosan microsphere sorbent for separation and determination of environmental estrogens through SPE coupled with HPLC

摘要

In this paper, a new separation sorbent of magnetic chitosan microsphere was prepared by means of suspension process using magnetic-Fe3O 4 nanoparticles as magnetic material and glutaraldehyde as the cross-linker. The morphology and properties of magnetic chitosan microspheres were characterized by FT-IR, SEM and adsorption test, and the results showed that they had good recognition, high selective ability and fast adsorption-desorption dynamics for estriol (E3), 17β-estradiol (E2) and diethylstilbestrol (DES). Applying this material as SPE sorbent, a method for separation, enrichment and analysis of estrogens in samples coupled with HPLC was developed. Under the optimized condition, the detection limit (S/N=3) for three estrogens was 3.2-20.1 ng/L, and the RSD for five replicate extractions of 50 μg/L E3, E2 and DES was 4.6-8.3%. The blank river water spiked with E3, E2 and DES at 0.05 and 0.2 mg/L levels were extracted and determined by the developed method with good recoveries ranging from 85.5 to 103.7%.