title: Grafting of norfloxacin imprinted polymeric membranes on silica surface for the selective solid-phase extraction of fluoroquinolones in fish samples.
abstract: A high-density imprinted polymeric membrane was immobilized on a porous silica-gel support by polymerization of methacrylic acid with vinyl-silanized silica gel for the selective solid-phase extraction (SPE) of norfloxacin (NOR) in fish samples. The imprinted membranes showed high adsorption capacity (423.2 μmol g(-1)), significant selectivity (k=14.64, k'=9.61) and good site accessibility (2h) for NOR. The conditions of SPE were investigated, and water (pH=6), methanol:water (1:1, v/v) and methanol-acetic acid-trifluoroacetic acid (90:9:1, v/v) were selected as the sample solvent, the washing solution and the eluting solution, respectively. Under the optimal SPE condition, three fluoroquinolone residues in fish were separated and detected by an off-line MIP-SPE-HPLC with better clean up and enrichment. The recoveries of norfloxacin, ofloxacin and ciprofloxacin were 89.3-94.8%, 69.3-102.8% and 85-90.5%, respectively, with relative standard deviations lower than 6.5%. The limits of detection (LOD) of the proposed method (S/N=3) were in a range of 2.65-3.65 μg kg(-1), and the limits of quantification (LOQ, S/N=10) were in a range of 8.82-12.16 μg kg(-1).
authors.affiliation: College of Chemistry and Environmental Science, Hebei University, Key Laboratory of Analytical Science and Technology of Hebei Province, Baoding 071002, China. lvyunkai@hbu.edu.cn
authors.forename: Yun-Kai
authors.initials: YK
authors.lastname: Lv
authors.forename: Yong
authors.initials: Y
authors.lastname: Ma
authors.forename: Xiao-Bo
authors.initials: XB
authors.lastname: Zhao
authors.forename: Cui-Ling
authors.initials: CL
authors.lastname: Jia
authors.forename: Han-Wen
authors.initials: HW
authors.lastname: Sun
mesh_terms: D000327:Adsorption; D000818:Animals; D002851:Chromatography, High Pressure Liquid; D002939:Ciprofloxacin / Q000032:analysis*; D005399:Fishes / Q000378:metabolism*; D057230:Limit of Detection; D008567:Membranes, Artificial; D008689:Methacrylates / Q000737:chemistry; D054802:Molecular Imprinting; D009643:Norfloxacin / Q000032:analysis*; D015242:Ofloxacin / Q000032:analysis*; D011108:Polymers / Q000737:chemistry; D016062:Porosity; D012821:Silanes / Q000737:chemistry; D058428:Silica Gel; D052616:Solid Phase Extraction; D012997:Solvents; D014753:Vinyl Compounds / Q000737:chemistry
chemical_list: D008567:Membranes, Artificial; D008689:Methacrylates; D011108:Polymers; D012821:Silanes; D012997:Solvents; D014753:Vinyl Compounds; C008384:methacrylic acid; D002939:Ciprofloxacin; D058428:Silica Gel; D015242:Ofloxacin; D009643:Norfloxacin