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采用基于深共晶溶剂冷冻分散液液微萃取结合石墨炉原子吸收光谱法对血液样品中的有机/无机汞和总汞进行形态分析。

Speciation of organic/inorganic mercury and total mercury in blood samples using vortex assisted dispersive liquid-liquid microextraction based on the freezing of deep eutectic solvent followed by GFAAS.

机构信息

School of Medical, Kermanshah University of Medical Sciences, Kermanshah, Iran; Clinical Research Development Center, Mohammad Kermanshahi Hospital, Kermanshah University of Medical Sciences, Kermanshah, Iran.

Research Center for Environmental Determinants of Health (RCEDH), Kermanshah University of Medical Sciences, Kermanshah, Iran.

出版信息

Talanta. 2018 Aug 15;186:17-23. doi: 10.1016/j.talanta.2018.04.042. Epub 2018 Apr 12.

Abstract

In this research, a new vortex assisted dispersive liquid-liquid microextraction based on the freezing of deep eutectic solvent (VADLLME-FDES) has been developed for the determination of organic mercury (R-Hg) and inorganic mercury (Hg) in blood samples prior to their analysis by graphite furnace atomic absorption spectrometry (GFAAS). In this method, a green solvent consisting of 1-octyl-3-methylimidazolium chloride and 1-undecanol was used as an extraction solvent, yielding the advantages of material stability, low density, and a suitable freezing point near room temperature. Under the optimum conditions, enrichment factor is 112. The calibration graph is linear in the range of 0.30-60 µg L and limit of detection (LOD) is 0.10 µg L. Repeatability and reproducibility of the method based on seven replicate measurements of 5.0 µg L of Hg in analyzed samples were 3.7% and 6.2%, respectively. The relative recoveries of blood samples which have been spiked with different levels of Hg are 90-109%. A new deep eutectic solvent consists of two parts: [DMIM]Cl and 1-undecanol in the molar ratio of 1-2. The accuracy of the proposed procedure was also assessed by determining the concentration of the mercury in a standard reference material. All organic mercury (R-Hg) species were converted to Hg and finally, the concentration of R-Hg is simply calculated by mathematically subtracting the concentrations of Hg from the concentration of total mercury (t-Hg). The extraction methodology is simple, rapid, cheap and green since small amounts of non-toxic solvents are necessary.

摘要

在这项研究中,开发了一种基于深共晶溶剂冷冻的新型涡旋辅助分散液液微萃取(VADLLME-FDES),用于石墨炉原子吸收光谱法(GFAAS)分析前测定血样中的有机汞(R-Hg)和无机汞(Hg)。在该方法中,使用由 1-辛基-3-甲基咪唑氯和 1-十一醇组成的绿色溶剂作为萃取溶剂,具有材料稳定性、低密度和接近室温的合适冰点的优点。在最佳条件下,富集因子为 112。校准曲线在 0.30-60μg/L 范围内呈线性,检测限(LOD)为 0.10μg/L。在分析样品中 5.0μg/L 的 Hg 进行 7 次重复测量的方法重复性和重现性分别为 3.7%和 6.2%。用不同水平的 Hg 对血液样品进行加标回收的相对回收率为 90-109%。深共晶溶剂由两部分组成:[DMIM]Cl 和 1-十一醇,摩尔比为 1-2。通过测定标准参考物质中汞的浓度来评估所提出程序的准确性。所有有机汞(R-Hg)物种均转化为 Hg,最后通过从总汞(t-Hg)浓度中减去 Hg 的浓度,即可简单计算出 R-Hg 的浓度。萃取方法简单、快速、廉价且环保,因为只需要少量的无毒溶剂。

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