Determination of Estrogens in Milk Samples by Magnetic-Solid-Phase Extraction Technique Coupled With High-Performance Liquid Chromatography.
A magnetic-solid-phase extraction method coupled with high-performance liquid chromatography and diode array detection has been developed for simultaneous determination of 3 estrogens in milk samples. In this work, Fe3O4 NPs were synthesized by a simple chemical co-precipitation reaction, and the surface of Fe3O4 was modified with cetyltrimethyl ammonium bromide (CTAB; designed as Fe3O4@CTAB). The synthesized Fe3O4@CTAB NPs were characterized by Fourier transformed infrared spectroscopy, scanning electron microscopy, and transmission electron microscope. Fe3O4@CTAB NPs have high binding affinity toward estrone (E1), 17β-estradiol (17β-E2), and diethylstilbestrol (DES). Fe3O4@CTAB NPs can be easily separated from sample solutions using an external magnet due to the high super-paramagnetic property. The separation, preconcentration procedure is fast and will be completed in 2 min. Estrogens linear dynamic ranges were achieved in the range of 10 to 1000 ng/mL with regression coefficients (R(2)) higher than 0.9992. The limits of detection were between 0.26 and 0.61 ng/mL. Parameters influencing the recoveries were investigated and optimized. The proposed method was used for the determination of E1, 17β-E2, and DES in milk samples, and recoveries were ranged from 91.3% to 105.0%, with the relative standard deviations in the range of 2.7% to 4.0%.
the Faculty of Life Science and Technology, Kunming Univ. of Science and Technology, Yunnan Province, 650500, China.
Juan
J
Wang
Yunnan Province Food Safety Research Inst, Yunnan Province, 650500, China.
Chunsheng
C
Cheng
the Faculty of Life Science and Technology, Kunming Univ. of Science and Technology, Yunnan Province, 650500, China.
Yaling
Y
Yang
D000818:Animals; D000077286:Cetrimonium; D002593:Cetrimonium Compounds; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004054:Diethylstilbestrol / Q000032:analysis*; D004958:Estradiol / Q000032:analysis*; D004967:Estrogens / Q000032:analysis*; D004970:Estrone / Q000032:analysis*; D008892:Milk / Q000737:chemistry*; D052616:Solid Phase Extraction / Q000379:methods*
D002593:Cetrimonium Compounds; D004967:Estrogens; D004970:Estrone; D004958:Estradiol; D004054:Diethylstilbestrol; D000077286:Cetrimonium
Fe3O4@CTAB NPs; estrogens; high-performance liquid chromatography; magnetic-solid-phase extraction