Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University, 54124 Thessaloniki, Greece.
International Forensic Research Institute, Department of Chemistry and Biochemistry, Florida International University, Miami, FL 33131, USA.
Molecules. 2020 Dec 22;26(1):9. doi: 10.3390/molecules26010009.
A novel simple and sensitive, time-based flow injection solid phase extraction system was developed for the automated determination of metals at low concentration. The potential of the proposed scheme, coupled with flame atomic absorption spectrometry (FAAS), was demonstrated for trace lead and chromium(VI) determination in environmental water samples. The method, which was based on a new sorptive extraction system, consisted of a microcolumn packed with glass fiber coated with sol-gel poly (diphenylsiloxane) (sol-gel PDPS), which is presented here for the first time. The analytical procedure involves the on-line chelate complex formation of target species with ammonium pyrrolidine dithiocarbamate (APDC), retention onto the hydrophobic sol-gel sorbent coated surface of glass fibers, and finally elution with methyl isobutyl ketone prior to atomization. All main chemical and hydrodynamic factors, which affect the complex formation, retention, and elution of the metal, were optimized thoroughly. Furthermore, the tolerance to potential interfering ions appearing in environmental samples was also explored. Enhancement factors of 215 and 70, detection limits (3 s) of 1.1 μg·L and 1.2 μg·L, and relative standard deviations (RSD) of 3.0% (at 20.0 μg·L) and 3.2% (at 20.0 μg·L) were obtained for lead and chromium(VI), respec tively, for 120 s preconcentration time. The trueness of the developed method was estimated by analyzing certified reference materials and spiked environmental water samples.
一种新颖的简单而灵敏的基于时间的流动注射固相萃取系统被开发出来,用于自动测定低浓度金属。该方案与火焰原子吸收光谱法(FAAS)相结合,用于环境水样中痕量铅和铬(VI)的测定。该方法基于一种新的吸附萃取体系,由微柱填充玻璃纤维涂层的溶胶-凝胶聚二苯基硅氧烷(sol-gel PDPS)组成,这是首次提出。分析程序包括目标物种与氨基金刚烷二硫代氨基甲酸盐(APDC)的在线螯合络合形成、保留在玻璃纤维涂覆的疏水性溶胶-凝胶吸附剂表面上,最后用甲基异丁基酮洗脱,然后进行原子化。所有主要的化学和流体力学因素,影响配合物的形成、保留和洗脱的因素,都进行了彻底优化。此外,还探讨了环境样品中潜在干扰离子的容忍度。对于铅和铬(VI),分别获得了 215 和 70 的增强因子、3 s 的检测限(1.1 μg·L 和 1.2 μg·L)以及 3.0%(20.0 μg·L)和 3.2%(20.0 μg·L)的相对标准偏差(RSD),用于 120 s 的预浓缩时间。通过分析认证参考材料和加标环境水样来评估所开发方法的准确性。