Warsaw University of Technology, Faculty of Chemistry, Chair of Analytical Chemistry, Noakowskiego 3, 00-664, Warsaw, Poland.
Warsaw University of Technology, Faculty of Chemistry, Chair of Analytical Chemistry, Noakowskiego 3, 00-664, Warsaw, Poland.
Talanta. 2020 Nov 1;219:121162. doi: 10.1016/j.talanta.2020.121162. Epub 2020 May 22.
The photochemical generation technique of mercury vapor (PCVG) coupled with headspace solid phase microextraction (SPME) and microwave induced plasma optical emission spectrometry (MIP-OES) has been developed and successfully applied for fast and sensitive determination of mercury in complex matrix samples. Mercury vapor was generated by UV photo-reduction of inorganic mercury and methylmercury to mercury vapor in 5% (v/v) formic acid with subsequent gas-liquid separation and preconcentration by solid phase microextraction. A stopped-flow mode of the PCVG-SPME unit was employed with the aim of increasing analyte preconcentration factor, thus improving both sensitivity of determination and detection limits for mercury. The calibration curves were linear up to 20 ng mL with the limit of detection for inorganic mercury and methylmercury of 0.030 and 0.045 ng mL, respectively. This manifold allowed a repeatability, expressed as relative standard deviation, of below 5%. Due to differences in efficiency of Hg vapor generation for Hg and CHHg, the quantification was performed against external Hg and CHHg aqueous standards, respectively. The method was validated by the analysis of two CRM materials of different matrix composition, i.e. estuarine sediment ERM CC580 for total mercury content and tuna fish ERM CE464 for methylmercury content, respectively. The results proved good accuracy of the method with recovery of 101% total mercury and 87.3% methylmercury and precision of 3.8% and 12.5%, respectively. Effect of concomitants in the stopped-flow generation of mercury vapor with the new manifold was also investigated. Next, the proposed method was successfully applied for monitoring of bioaccessible fraction of mercury during their incubation in simulated body fluid in the presence of selenium nanoparticles examined as a potential mercury detoxifying agent.
汞蒸气的光化学发生技术（PCVG）与顶空固相微萃取（SPME）和微波诱导等离子体光学发射光谱法（MIP-OES）相结合，已经被开发出来，并成功应用于快速灵敏地测定复杂基质样品中的汞。汞蒸气是通过在 5%（v/v）甲酸中紫外线光还原无机汞和甲基汞生成的，随后通过固相微萃取进行气-液分离和预浓缩。采用 PCVG-SPME 单元的停流模式，目的是增加分析物的预浓缩因子，从而提高汞的测定灵敏度和检测限。校准曲线在 20ng/mL 以内呈线性，无机汞和甲基汞的检测限分别为 0.030 和 0.045ng/mL。该多通道允许重复性，以相对标准偏差表示，低于 5%。由于 Hg 蒸气生成效率的差异，Hg 和 CHHg 的定量分别针对外部 Hg 和 CHHg 水溶液标准品进行。该方法通过分析两种不同基质组成的 CRM 材料进行了验证，即河口沉积物 ERM CC580 用于总汞含量，金枪鱼 ERM CE464 用于甲基汞含量。结果表明，该方法具有良好的准确性，总汞的回收率为 101%，甲基汞的回收率为 87.3%，精密度分别为 3.8%和 12.5%。还研究了在新多通道中用停流法生成汞蒸气时共存物质的影响。然后，该方法成功应用于监测在模拟体液中孵育时生物可利用的汞的含量，硒纳米粒子被作为一种潜在的汞解毒剂进行了考察。
