RESUMEN
Molecularly imprinted polymers (MIPs) synthesized by conventional functional monomers have poor specific recognition ability in strong polar solvent, which is not favorable to their applications in separation and analysis. In this work, an ionic liquid functional monomer, 1-allyl-3-vinylimidazolium chloridize, is introduced to prepare sulfamonomethoxine imprinted polymer on the surface of silica carriers in methanol. 1H NMR and 35Cl NMR spectroscopy is performed to discuss the interactions between template and the functional monomer. The rebinding experiments show that the MIP has excellent selectivity towards sulfonamide antibiotic (sulfamonomethoxine, sulfamethoxazole and sulfadiazine) in methanol. From 1H NMR and 35Cl NMR analysis and selective adsorption results, it was inferred that hydrogen bond, electrostatic and π-π interactions are the driving force for the selective recognition of MIP in methanol. Combined solid phase extraction (SPE) with HPLC detection, 98.0-108.0% of sulfamonomethoxine have been extracted by MIP-SPE cartridge from the mixture of sulfamonomethoxine, diphenylamine and N-butylpyridinium chloride. Under optimal condition, the proposed MIP-SPE column can response sulfamonomethoxine linearly in the concentration range from 3.0-1.0×104 µg L-1, and the established MIP-SPE-HPLC system has been successfully applied for extraction and analysis of sulfamonomethoxine in soil and sediment with recoveries ranging from 95.0% to 105.0%.
Asunto(s)
Técnicas de Química Analítica/métodos , Líquidos Iónicos/química , Polímeros/química , Sulfamonometoxina/química , Sulfamonometoxina/aislamiento & purificación , Adsorción , Cromatografía Líquida de Alta Presión , Enlace de Hidrógeno , Impresión Molecular , Dióxido de Silicio , Extracción en Fase Sólida , Solventes/químicaRESUMEN
Ionic liquid-modified magnetic polymeric microspheres (ILMPM) were prepared based on Fe3O4 magnetic nanoparticles (MNPs) and ionic liquids (ILs) incorporated into a polymer. The composites were characterized using scanning electron microscopy, Fourier transform infrared analysis, thermogravimetric analysis, X-ray diffraction, and vibrating magnetometer, which indicated that ILMPM had a regularly spherical shape and strong magnetic property. The obtained ILMPM were successfully applied as a special adsorbent of magnetic dispersive solid phase extraction (MDSPE) for the rapid extraction and isolation of sulfamonomethoxine sodium and sulfachloropyrazine sodium in urine. The factors that affected extraction efficiency, such as adsorption conditions, desorption conditions, washing and elution solvents, and pH of the sample solution, were optimized. Under the optimum condition, good linearity in the range of 0.005-2.0 µg g(-1) (r ≥ 0.9996) was obtained for the two sulfonamides (SAs); the average recoveries at three spiked levels ranged from 86.9 to 102.1 %, with relative standard deviations of ≤4.3 %. The presented ILMPM-MDSPE method combined the advantages of ILs, MNPs, and MDSPE and therefore could be potentially applied for rapid screening of SAs in urine.
Asunto(s)
Polímeros/química , Extracción en Fase Sólida/instrumentación , Sulfamonometoxina/aislamiento & purificación , Sulfanilamidas/aislamiento & purificación , Adsorción , Humanos , Líquidos Iónicos/química , Fenómenos Magnéticos , Microesferas , Extracción en Fase Sólida/métodos , Sulfamonometoxina/orina , Sulfanilamidas/orinaRESUMEN
A simple, convenient, and economic self-assembly miniaturized syringe assisted extraction (mini-SAE) using poly (hydroxyethyl methacrylate) polymer (PHEMA) as sorbent coupled with liquid chromatography was proposed for rapid screening of sulfadiazine (SD) and sulfamonomethoxine (SMM) in milk. The water-compatible PHEMA was synthesized by reversible addition-fragmentation chain transfer precipitation polymerization using trithiocarbonate as chain transfer agent and methanol-water system as reaction medium. The obtained PHEMA sorbent showed good affinity to sulfonamides and was successfully applied as a special sorbent for a mini-SAE device for simultaneous extraction and isolation of SD and SMM in milk samples. Under the optimum condition, good linearity was obtained in a range of 7.0-700 ng g(-1) (r≥0.9995) and the average recoveries of SD and SMM at three spiked levels were ranged from 85.6 to 100.3% with the relative standard deviations (RSD) ≤6.5%. The presented PHEMA-mini-SAE protocol could be potentially applied as an alternative tool for analyzing the residues of SAs in complicated biological samples.