Erciyes University, Fen Faculty, Department of Chemistry, 38039 Kayseri, Turkey; Center of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080, Pakistan.
Center of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080, Pakistan.
Spectrochim Acta A Mol Biomol Spectrosc. 2014 Apr 5;123:194-9. doi: 10.1016/j.saa.2013.12.065. Epub 2013 Dec 18.
A rapid and innovative microextraction technique named as, ionic liquid-based ultrasound-assisted dual magnetic microextraction (IL-UA-DMME) was developed for the preconcentration and extraction of trace cadmium from environmental and biological samples, prior to analyzed by flame atomic absorption spectrometry (FAAS). The proposed method has many obvious advantages, including evading the use of organic solvents and achieved high extraction yields by the combination of dispersive liquid-liquid microextraction (DLLME) and magnetic mediated-solid phase extraction (MM-SPE). In this approach ionic liquid (IL) 1-butyl-3-methylimidazolium hexafluorophosphate [C4mim][PF6] play an important role to extract the cadmium-4-(2-thiazolylazo)-resorcinol (Cd-TAR) complex from acid digested sample solutions and ultrasonic irradiation was applied to assist emulsification. After then, dispersed small amount of Fe3O4 magnetic nanoparticles (MNPs) in sample solutions to salvaged the IL and complete phase separation was attained. Some analytical parameters that influencing the efficiency of proposed (IL-UA-DMME) method, such as pH, volume of IL, ligand concentration, ultra-sonication time, amount of Fe3O4 MNPs, sample volume and matrix effect were optimized. Limit of detection (LOD) and enrichment factor (EF) of the method under optimal experimental conditions were found to be 0.40μgL(-1) and 100, respectively. The relative standard deviation (RSD) of 50μgL(-1) Cd was 4.29%. The validity and accuracy of proposed method, was assessed to analyzed certified reference materials of fortified lake water TMDA-54.4, SPS-WW2 waste water, spinach leaves 1570a and also checked by standard addition method. The obtained values showed good agreement with the certified values and sufficiently high recovery were found in the range of 98.1-101% for Cd. The proposed method was facile, rapid and successfully applied for the determination of Cd in environmental and different biological samples.
一种名为离子液体-基于超声辅助双磁微萃取（IL-UA-DMME）的快速创新微萃取技术被开发出来，用于环境和生物样品中痕量镉的预浓缩和萃取，然后通过火焰原子吸收光谱法（FAAS）进行分析。该方法有许多明显的优点，包括避免使用有机溶剂，并通过分散液-液微萃取（DLLME）和磁介导固相萃取（MM-SPE）的结合实现高萃取产率。在这种方法中，离子液体（IL）1-丁基-3-甲基咪唑六氟磷酸盐[C4mim][PF6]在从酸消解的样品溶液中提取镉-4-（2-噻唑偶氮）-间苯二酚（Cd-TAR）络合物方面发挥重要作用，并应用超声波辐射辅助乳化。然后，将少量分散的 Fe3O4 磁性纳米粒子（MNPs）加入到样品溶液中以回收 IL，并实现完全的相分离。优化了影响所提出的（IL-UA-DMME）方法效率的一些分析参数，如 pH 值、IL 体积、配体浓度、超声时间、Fe3O4 MNPs 用量、样品体积和基质效应。在最佳实验条件下，方法的检出限（LOD）和富集因子（EF）分别为 0.40μgL(-1)和 100。50μgL(-1)Cd 的相对标准偏差（RSD）为 4.29%。该方法的有效性和准确性通过对加标湖水 TMDA-54.4、SPS-WW2 废水、菠菜叶片 1570a 的认证参考材料进行评估，并通过标准加入法进行检查。得到的数值与认证值吻合良好，Cd 的回收率在 98.1-101%范围内较高。该方法简便、快速，成功应用于环境和不同生物样品中 Cd 的测定。
