title: 1-Butyl-3-aminopropyl imidazolium-functionalized graphene oxide as a nanoadsorbent for the simultaneous extraction of steroids and β-blockers via dispersive solid-phase microextraction.
abstract: In this study, we describe the synthesis of graphene oxide functionalized with the ionic liquid 1-butyl-3-aminopropyl imidazolium chloride and its use as an adsorbent for the dispersive solid-phase microextraction (micro SPE) of four anabolic steroids and six β-blockers from aqueous samples of environmental importance, prior to their HPLC-diode array detector analysis. As the ionic liquid is covalently attached to graphene oxide sheets, it is made possible for it to participate in the dispersive micro SPE procedure. The limits of detection and limits of quantification of the proposed method were found to be in the range of 7-23ng/L and between 20 and 70ng/L, respectively. The linearity was satisfactory, with the determination coefficients to range from 0.9940 to 0.9998 while the within- and between-day relative standard deviation of the method ranged between 3.1 and 7.6% and from 4.0 to 8.5%, respectively. In order to test the applicability of the proposed method in real-life samples, the effluent from a municipal wastewater treatment plant as well as natural water samples from two rivers and a lake were collected and analyzed. After the analysis of samples, the effluent from municipal wastewater treatment plant was fortified with the analytes, at concentrations equal to 2 and 10 times the LOQs. Recoveries were calculated after subtracting the native (no-spike) concentrations of analytes, when needed. All the recoveries were in the range of 87-98%. A comparison study attests to the superiority of the developed nanomaterial over graphene oxide and graphene for the dispersive micro SPE of steroids and β-blockers.
authors: Department of Analytical Chemistry, University of Cordoba, 14071 Cordoba, Spain.
authors: Maria
authors: M
authors: Serrano
authors: Laboratory of Analytical Chemistry, Department of Chemistry, University of Ioannina, 45110 Ioannina, Greece.
authors: Theodoros
authors: T
authors: Chatzimitakos
authors: Department of Analytical Chemistry, University of Cordoba, 14071 Cordoba, Spain.
authors: Mercedes
authors: M
authors: Gallego
authors: Laboratory of Analytical Chemistry, Department of Chemistry, University of Ioannina, 45110 Ioannina, Greece. Electronic address: cstalika@cc.uoi.gr.
authors: Constantine D
authors: CD
authors: Stalikas
mesh_terms: D000319:Adrenergic beta-Antagonists / Q000302:isolation & purification*; D000327:Adsorption; D045930:Anabolic Agents / Q000302:isolation & purification*; D002851:Chromatography, High Pressure Liquid; D006108:Graphite / Q000737:chemistry*; D007093:Imidazoles / Q000737:chemistry*; D052578:Ionic Liquids / Q000737:chemistry; D060106:Lakes / Q000737:chemistry; D045483:Rivers / Q000737:chemistry; D052617:Solid Phase Microextraction / Q000379:methods; D013256:Steroids / Q000302:isolation & purification*; D062065:Wastewater / Q000032:analysis; D014874:Water Pollutants, Chemical / Q000302:isolation & purification*
chemical_list: D000319:Adrenergic beta-Antagonists; D045930:Anabolic Agents; D006108:Graphite; D007093:Imidazoles; D052578:Ionic Liquids; D013256:Steroids; D062065:Wastewater; D014874:Water Pollutants, Chemical; C583483:1-(3-aminopropyl)-3-butylimidazolium
keywords: Dispersive solid–phase microextraction; Graphene oxide-1-butyl-3-aminopropyl imidazolium chloride; HPLC; Room–temperature ionic liquid; Steroids; β-Blockers