Yilmaz Erkan, Alothman Zeid A, Sumayli Hamoud M T, Ibrahim Medhat, Soylak Mustafa
Erciyes University, Faculty of Science, Department of Chemistry, 38039-Kayseri, Turkey.
J AOAC Int. 2012 Jul-Aug;95(4):1205-10. doi: 10.5740/jaoacint.10-485.
A sorbent extraction procedure for Pb(II), Cu(II), Ni(II), and Fe(III) ions on single-walled carbon nanotube disks has been established. Analyte ions were converted to 2-(5-bromo-2-pyridylazo)-5-diethylamino-phenol chelates, then adsorbed on the disk. Adsorbed chelates were easily desorbed from the disk by using 10 mL 2 M HNO3. The various analytical parameters, including pH and reagent amounts that were effective for the recoveries of the analytes on nanotube disks, were optimized. The influence of matrix ions was also studied. The LOD values based on 3sigma were in the 0.3-4.6 microg/L range. Validation of the proposed SPE procedure was carried out by the determination of analytes in certified reference materials (TMDA-54.4 fortified lake water and HR-1 Humber River sediment). Spiking and recovery experiments for the analyte ions in real samples gave good results. Application of the procedure was illustrated by the determination of analyte contents in some animal feeds and water samples from Turkey.
已建立了一种在单壁碳纳米管盘上萃取铅(II)、铜(II)、镍(II)和铁(III)离子的吸附剂萃取方法。分析物离子被转化为2-(5-溴-2-吡啶偶氮)-5-二乙氨基苯酚螯合物,然后吸附在盘上。通过使用10 mL 2 M硝酸很容易将吸附的螯合物从盘上解吸下来。对包括pH值和试剂用量等对纳米管盘上分析物回收率有效的各种分析参数进行了优化。还研究了基体离子的影响。基于3σ的检测限在0.3 - 4.6 μg/L范围内。通过测定标准参考物质(TMDA - 54.4强化湖水和HR - 1亨伯河沉积物)中的分析物对所提出的固相萃取方法进行了验证。对实际样品中分析物离子的加标和回收率实验取得了良好结果。通过测定土耳其一些动物饲料和水样中的分析物含量说明了该方法的应用。