title: Non-chromatographic mercury speciation and determination in wine by new core-shell ion-imprinted sorbents.
abstract: In this study new Hg(II) core-shell imprinted sorbents (Hg(II)-IIPs) were prepared and tested for speciation and determination of Hg in wine. The silica gel, chemically modified with 3-(trimethoxysilyl)propyl methacrylate (TSPM) was used as supporting material. The Hg(II)-imprinted polymer layer was grafted by copolymerization of methacrylic acid and trimethylolpropane trimethacrylate in the presence of Hg(II) complexes with two different chelating agents: 1-pyrrolidinedithiocarboxylic acid (P(PDC-Hg)/SiG) and 1-(2-thiazolylazo)-2-naphthol (P(TAN-Hg)/SiG). High selectivity and fast kinetics of processes of sorption and desorption for Hg(II) were found by using P(PDC-Hg)/SiG. Recovery experiments performed for selective determination of inorganic mercury in wines showed that the interfering organic matrix did not influence the extraction efficiency. Column solid phase extraction scheme was developed for the determination and speciation of Hg in wines. The limit of detection (LOD) achieved for inorganic mercury determination in wine samples is 0.02 μg L(-1) (3σ), measured by CV AAS. The relative standard deviation varied in the range 6-11% at 0.05-2 μg L(-1) Hg levels. The sorbents showed high mechanical and chemical stability and extraction efficiency has not changed after more than 50 sorption/desorption cycles.
authors: Faculty of Chemistry and Pharmacy, University of Sofia St. Kliment Ohridski, 1 James Bourchier Blvd., Sofia 1164, Bulgaria. i.dakova@chem.uni-sofia.bg
authors: Ivanka
authors: I
authors: Dakova
authors: Tanya
authors: T
authors: Yordanova
authors: Irina
authors: I
authors: Karadjova
mesh_terms: D001391:Azo Compounds; D006863:Hydrogen-Ion Concentration; D008024:Ligands; D008628:Mercury / Q000032:analysis*; D008689:Methacrylates; D008767:Methylmercury Compounds / Q000032:analysis*; D017646:Organosilicon Compounds; D058428:Silica Gel; D013054:Spectrophotometry, Atomic; D013816:Thermodynamics; D014920:Wine / Q000032:analysis*
chemical_list: D001391:Azo Compounds; D008024:Ligands; D008689:Methacrylates; D008767:Methylmercury Compounds; D017646:Organosilicon Compounds; C054556:1-(2-thiazolylazo)-2-naphthol; C008384:methacrylic acid; D058428:Silica Gel; D008628:Mercury; C505504:3-(trimethoxysilyl)propyl methacrylate; C028643:trimethylolpropane trimethacrylate