Rapid magnetic-mediated solid-phase extraction and pre-concentration of selected endocrine disrupting chemicals in natural waters by poly(divinylbenzene-co-methacrylic acid) coated Fe3O4 core-shell magnetite microspheres for their liquid chromatography-tandem mass spectrometry determination

摘要

A new Fe3O4/poly(divinylbenzene-co-methacrylicacid)core-shell magnetite microspheric material have been successfully developed as magnetic-mediated solid-phase extraction micro-particle sorbent ill dispersion mode (MM-SPE-MP) for the determination of selected estrogenic endocrine disrupting chemicals (EDCs).namely estrone(E1),17 beta-estradiol(E2),estriol(E3).17 alpha-ethynylestradiol(EE2)and bisphenol-A (BPA), in natural water, via quantification by HPLC tandem mass spectrometry The magnetite Fe3O4 core of this MM-SPE-MP sorbent was fabricated by a solvothermal approach and the thin layer of amphipolar poly((divinylbenzene-co-methacrylic acid))(pDVB-MAA)coating was established via suspension polymerization The resultant core-shell MM-SPE-MP sorbent material was characterized by electron microscopy.. X-ray diffraction and Fourier-transformed infiared spectroscopy. Particle size distribution of the core-shell microspheres was within the range 300-700 nm in diameter and the thickness of the pDVB-MAA coating was ca 10 nm This magnetite microspheric material can be easily dispersed In aqueous Samples and retrieved by the application of external magnetic field via a small piece of permanent magnet The MM-SPE-MP process for the selected estrogenic EDCs involved the dispersion of the core-shell macrospheric sorbent in water samples with sonication. followed by magnetic aided retrieval of the sorbent and solvent (methanol) desorption of extracted EDCs for LC-MS/MS analysis Partition equilibrium for all the selected EDCs onto this MM-SPE-MP sot bent was achieved within 15 mitt Recoveries of the EDCs were in ranges of 56-111% Analytes with smaller K-ow value showed relatively lower recovery (and relatively longer equilibration time for partitioning) Method detection limits achieved were found to be 1-36 pg ml(-1) (n=3). while the repeatability was 6-34%(p<005, n=3) This work demonstrates the usefulness of MM-SPE-MP in the rapid and highly sensitive monitoring of trace organic contaminants in natural waters.