Faculty of Chemistry and Pharmacy, University of Sofia St. Kliment Ohridski, 1 James Bourchier Blvd., Sofia 1164, Bulgaria.
J Hazard Mater. 2012 Sep 15;231-232:49-56. doi: 10.1016/j.jhazmat.2012.06.034. Epub 2012 Jun 25.
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.
在这项研究中，制备了新型汞(II)核壳印迹吸附剂(Hg(II)-IIPs)，并将其用于葡萄酒中汞的形态分析和测定。硅胶经 3-(三甲氧基硅基)丙基甲基丙烯酸酯(TSPM)化学修饰后，作为支持材料。在 Hg(II)与两种不同螯合剂形成的配合物存在下，通过甲基丙烯酸和三羟甲基丙烷三甲基丙烯酸酯的共聚反应，在硅胶上接枝 Hg(II)-印迹聚合物层：1-吡咯烷二硫代羧酸(P(PDC-Hg)/SiG)和 1-(2-噻唑基偶氮)-2-萘酚(P(TAN-Hg)/SiG)。使用 P(PDC-Hg)/SiG 时，发现对 Hg(II)的吸附和解吸过程具有高选择性和快速动力学。为选择性测定葡萄酒中的无机汞进行的回收实验表明，干扰的有机基质不会影响萃取效率。开发了柱固相萃取方案，用于葡萄酒中汞的测定和形态分析。通过 CV AAS 测定，葡萄酒样品中无机汞测定的检出限(LOD)为 0.02 μg L(-1)(3σ)。在 0.05-2 μg L(-1)Hg 水平下，相对标准偏差在 6-11%范围内变化。该吸附剂具有高机械和化学稳定性，经过 50 多次吸附/解吸循环后，萃取效率没有变化。
