title: Facile and fast preparation of low-cost silica-supported graphitic carbon nitride for solid-phase extraction of fluoroquinolone drugs from environmental waters.
abstract: The analytical application of silica-supported graphitic carbon nitride (g-C3N4@silica) for solid-phase extraction (SPE) of fluoroquinolone (FQ) pollutants from water is presented for the first time. g-C3N4@silica was easily and quickly prepared by one-pot thermal condensation of dicyandiamide and characterized by powder X-ray diffraction, thermogravimetric analysis, scanning electron microscopy, Fourier transform infrared spectroscopy and surface area measurements. The novel composite was applied as sorbent for SPE of FQs from water prior high-performance liquid chromatography with fluorescence detection. The extraction efficiency of g-C3N4was tested in tap and surface waters at actual concentrations (10-100ngL-1). Quantitative adsorption was achieved using 100mg sorbent (20wt% g-C3N4) for pre-concentration of 50-500mL sample, at the native pH (∼7.5-8). Elution was performed with 25mM H3PO4aqueous solution-acetonitrile (80:20), obtaining recoveries in the range 70-114%, enrichment factors up to 500 and inter-day RSDs≤12%. The batch-to-batch reproducibility was assessed on three independently synthesized g-C3N4@silica preparations (RSD 6-12%). g-C3N4supported on silica microparticles proved to be of easy preparation, inexpensive, reusable for at least 4 extractions of raw surface waters, and suitable for determination in real matrices.
authors.affiliation: Department of Chemistry, University of Pavia, via Taramelli 12, 27100 Pavia, Italy. Electronic address: andrea.speltini@unipv.it.
authors.forename: Andrea
authors.initials: A
authors.lastname: Speltini
authors.affiliation: Department of Chemistry, University of Pavia, via Taramelli 12, 27100 Pavia, Italy.
authors.forename: Federica
authors.initials: F
authors.lastname: Maraschi
authors.affiliation: Department of Chemistry, University of Pavia, via Taramelli 12, 27100 Pavia, Italy.
authors.forename: Roberta
authors.initials: R
authors.lastname: Govoni
authors.affiliation: Department of Chemistry, University of Pavia, via Taramelli 12, 27100 Pavia, Italy.
authors.forename: Chiara
authors.initials: C
authors.lastname: Milanese
authors.affiliation: Department of Chemistry, University of Pavia, via Taramelli 12, 27100 Pavia, Italy.
authors.forename: Antonella
authors.initials: A
authors.lastname: Profumo
authors.affiliation: Department of Chemistry and INSTM, University of Pavia, via Taramelli 12, 27100 Pavia, Italy.
authors.forename: Lorenzo
authors.initials: L
authors.lastname: Malavasi
authors.affiliation: Department of Chemistry, University of Pavia, via Taramelli 12, 27100 Pavia, Italy.
authors.forename: Michela
authors.initials: M
authors.lastname: Sturini
mesh_terms: D000900:Anti-Bacterial Agents / Q000032:analysis* / Q000302:isolation & purification; D002851:Chromatography, High Pressure Liquid; D024841:Fluoroquinolones / Q000032:analysis* / Q000302:isolation & purification; D006108:Graphite / Q000737:chemistry*; D009570:Nitriles / Q000737:chemistry*; D015203:Reproducibility of Results; D012822:Silicon Dioxide / Q000737:chemistry; D052616:Solid Phase Extraction / Q000191:economics / Q000379:methods*; D014874:Water Pollutants, Chemical / Q000032:analysis* / Q000302:isolation & purification
chemical_list: D000900:Anti-Bacterial Agents; D024841:Fluoroquinolones; D009570:Nitriles; D014874:Water Pollutants, Chemical; C011206:cyanogen; D012822:Silicon Dioxide; D006108:Graphite
keywords: Antibiotics; Determination; Graphitic carbon nitride; Pollutants; Sample enrichment; Sample preparation