Preparation of magnetic mesoporous epoxy resin by initiator-free ring-opening polymerization for extraction of bile acids from human serum.
In this work, we reported a simple two-step method for the synthesis of magnetic mesoporous epoxy resin (MMER), including one-pot template-free hydrothermal synthesis of nanoscale amine-functionalized magnetic nanoparticles (MN-NH2) and initiator-free ring-opening polymerization of epoxy resin. The resultant MMER was characterized in detail by transmission electron microscope (TEM), Fourier transform-infrared (FT-IR) spectra, X-ray photoelectron spectroscopy (XPS), thermogravimetic analysis (TGA) and magnetization curves. These results demonstrated successful synthesis of MMER with sufficient magnetic property and excellent thermal stability. The epoxy resin was covalent bonding MN-NH2 on and synthesized by hydrophobic monomers, so the MMER exhibited excellent adsorption quantity for hydrophobic bile acids. The MMER was used as magnetic solid-phase extraction (MSPE) sorbent, and combined with liquid chromatography-tandem mass spectrometry to extract and monitor 11 kinds of bile acids from serum sample. The proposed MSPE combined with LC-MS/MS method exhibited low limit of detection between 0.1 and 5 ng mL-1. In blank serum sample, 9 kinds of bile acids were detected, and ranged from -2.29 ng mL-1 to 6.86 ng mL-1. In standard addition recovery test, the recovery values of detectable bile acids ranged 102.4% to 108.5%, 96.0% to 104.0% and 82.3% to 103.3% when spiked with 0.2, 2.0 and 20 ng mL-1, respectively. The intra- and inter-day precision (n = 6) ranged 3.7% to 5.9% and 7.0% to 9.5%, respectively. The above results demonstrated that the MSPE combined with LC-MS/MS method was accurate and effective for quantitative determination of bile acids from complex biological samples.
['Sun|Lu|L|', 'Duan|Rui|R|', 'Fan|Yu|Y|', 'Chen|Xin-Zhu|XZ|', 'Peng|Chao|C|', 'Zheng|Chao|C|', 'Dong|Lin-Yi|LY|', 'Wang|Xian-Hua|XH|']
D000327:Adsorption D001647:Bile Acids and Salts D002853:Chromatography, Liquid D004853:Epoxy Resins D006801:Humans D057230:Limit of Detection D060328:Magnetic Phenomena D053758:Nanoparticles D058105:Polymerization D016062:Porosity D052616:Solid Phase Extraction D012996:Solutions D017550:Spectroscopy, Fourier Transform Infrared D053719:Tandem Mass Spectrometry
Magnetic mesoporous epoxy resin Ring-opening polymerization Bile acids Magnetic solid-phase extraction