Novel synthesized attapulgite nanoparticles-based hydrophobic monolithic column for in-tube solid-phase microextraction of thiosildenafil, pseudovardenafil, and norneosildenafil in functional foods.
作者： Chunyan Hou , Yihui Chen , Lihua Zhang , Rongrong Xuan , Tingting Wang
DOI: 10.1007/S00216-021-03155-4
关键词: Detection limit 、 Monolithic HPLC column 、 Adsorption 、 Fourier transform infrared spectroscopy 、 Monolith 、 Elution 、 Solid-phase microextraction 、 Ethylene glycol dimethacrylate 、 Chromatography 、 Materials science
摘要: In this study, a novel method which involved in-tube solid-phase microextraction (SPME) using an attapulgite (ATP) nanoparticles-based hydrophobic monolithic column was successfully developed. It coupled with high-performance liquid chromatography-ultraviolet detection for the determination of three phosphodiesterase-5 (PDE-5) inhibitors, including thiosildenafil, pseudovardenafil, and norneosildenafil, in functional foods. The prepared by one-step polymerization, 3-trimethoxysilylpropyl methacrylate-modified ATP nanoparticles 1-butyl-3-vinylimidazolium bromide (VBIMBr) as monomers, ethylene glycol dimethacrylate (EDMA) cross-linker. obtained poly(ATP-VBIMBr-EDMA) monolith characterized scanning electron microscopy equipped energy-dispersive analysis X-ray, Fourier transform infrared spectroscopy, thermogravimetric analysis, X-ray diffraction. adsorption capacity, up to 2.00 μg/cm calculated Langmuir isotherm model, about six times that poly(VBIMBr-EDMA) monolith. Crucial factors affecting extraction efficiency, sample solvent, elution flow rates sampling loading elution, volume, were investigated details. Under optimal SPME conditions, proposed showed good reproducibility run-to-run, column-to-column, batch-to-batch relative standard deviations less than 7.2%, low limits 0.5-0.9 ng/mL real samples. Thiosildenafil detected four types foods contents 1.30-4.78 μg/g. This newly based on may provide simple, efficient, promising alternative daily monitoring PDE-5 inhibitors
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