New Solid-Phase Extraction-High-Performance Liquid Chromatography Methods For Determination Of Bisphenol Estrogens

It is of great importance to develop new methods for determination of bisphenols with good selectivity and high sensitivity in environmental monitoring and food security.In this dissertation,two new approaches have been developed for determination of bisphenols in environmental waters and beverage.The detailed contents are shown as follows:Firstly,a new type of dummy molecularly imprinted magnetic nanoparticle(MI-MNP)was prepared via a hybrid imprinting technique for dispersive solid-phase extraction(d-SPE)and determination of bisphenol A(BPA).2,2-Bisphenol AF was used as the template molecule and Fe3O4 nanoparticle as the magnetic core.The MI-MNPs were characterized by FT-IR spectroscopy(FT-IR),thermo-gravimetric analysis(TGA),X-ray diffraction(XRD),transmission electron microscopy(TEM),and vibrating sample magnetometer(VSM).The adsorption tests showed that the MI-MNPs had a high binding ability for BPA and presented a fast binding kinetics.When used as a d-SPE sorbent,the MI-MNP showed high extraction efficiency,high enrichment factor and good reusability for BPA,and it can be easily recycled by a magnet.Furthermore,the dummy imprinting strategy can completely avoid the interference of the residual template in sorbent to determination of BPA.Using the MI-MNPs as sorbent,a d-SPE-HPLC method was developed and successfully applied to the analysis of BPA spiked in water samples and orange juice and that in a certified sample with recoveries of95.0-106.2%(RSD=2.5-4.5%),93.3-100.0%(RSD=1.2-5.0%)and 100.3%(RSD=3.5%),respectively.The limit of detection(S/N=3)for all samples was 0.3 ng/mL.The new MI-MNPs can be utilized as a good d-SPE sorbent for BPA in environmental water samples and beverages.Secondly,based on a new porous ?-CD polymer(P-CDP)sorbent,a SPE-HPLC-UV method was developed for the simultaneous determination of three bisphenols(BPA,BPF and BPAF).The P-CDP were characterized by FT-IR spectroscopy,BET and TGA.The adsorption tests showed that the P-CDP had a high binding ability for BPA,BPF and BPAF and presented a fast binding kinetics.When used as a SPE sorbent,the P-CDP showed high extraction efficiency,high enrichment factor and good reusability for the three bisphenols.Using the P-CDP as sorbent,a SPE-HPLC method was developed and successfully applied to the simultaneous analysis of three bisphenols spiked in water samples and orange juice and that in a certified sample.For water,the recoveries of BPF,BPA and BPAF are 91.0%-103.0%(RSD=1.4-2.9%),98.0%-101.0%(RSD=1.3-2.6%)and 96.0%-104.0%(RSD=1.3-2.9%),respectively;for orange juice,the recoveries of BPF,BPA and BPAF are 94.0%-97.0%(RSD=1.4-2.9%),103.0%-104.0%(RSD=1.7-2.1%),94.0%-101.0%(RSD=1.3-2.8%),respectively.The limit of detection(S/N=3)for all samples was 0.3 ng/mL.The new P-CDP can be utilized as a good SPE sorbent for BPF,BPA and BPAF in environmental water samples and beverages.