Shokrollahi Ardeshir, Ebrahimi Foroogh
Yasouj University, Department of Chemistry, Yasouj, Iran.
J AOAC Int. 2017 Nov 1;100(6):1861-1868. doi: 10.5740/jaoacint.17-0042. Epub 2017 Aug 15.
In the present work, a simple, efficient, and environmentally friendly method was proposed for the simultaneous preconcentration and determination of minute quantities of copper and cobalt in water samples and serum by a supramolecular-based ultrasonic-assisted dispersion solidification liquid-liquid microextraction (DSLLME) procedure coupled with flame atomic absorption spectrometry. The procedure is based on the DSLLME of copper and cobalt with decanoic acid-tetrahydrofuran supramolecular solvent (SUPRAS) in the presence of sodium diethyldithiocarbamate, as the complexing agent. SUPRAS is a nanostructured liquid generated from amphiphiles through a sequential self-assembly process occurring on two scales, molecular and nano. Several variables that affect the extraction efficiency-including pH, concentration of complexing agent, volume of the extraction and dispersive solvents (volume of SUPRAS), sonication time, and ionic strength-were investigated and optimized. The method provided enrichment factors of 23.31 and 22.38 for copper and cobalt, respectively. The preconcentration factor for the two analytes was 20.00. Calibration plots were linear in the range of 5.00-700.00 ng/mL for copper and 5.00-500.00 ng/mL for cobalt, with correlations of determination of 0.9973 and 0.9981. The precision of the method were expressed as RSDs for six replicate measurements and LODs and found to be ±4.10 and ±2.30% for copper and 2.90 and 3.50 ng/mL for cobalt. The proposed method was successfully applied to the simultaneous determination of trace copper and cobalt in real water samples and serum with satisfactory results.
在本研究中,提出了一种简单、高效且环保的方法,通过基于超分子的超声辅助分散固化液液微萃取(DSLLME)程序结合火焰原子吸收光谱法,同时预富集和测定水样及血清中的痕量铜和钴。该程序基于在二乙基二硫代氨基甲酸钠作为络合剂存在下,铜和钴与癸酸 - 四氢呋喃超分子溶剂(SUPRAS)的DSLLME。SUPRAS是一种由两亲分子通过分子和纳米两个尺度上的顺序自组装过程产生的纳米结构液体。研究并优化了几个影响萃取效率的变量,包括pH值、络合剂浓度、萃取和分散溶剂的体积(SUPRAS的体积)、超声处理时间和离子强度。该方法对铜和钴的富集因子分别为23.31和22.38。两种分析物的预富集因子为20.00。铜的校准曲线在5.00 - 700.00 ng/mL范围内呈线性,钴的校准曲线在5.00 - 500.00 ng/mL范围内呈线性,测定相关系数分别为0.9973和0.9981。该方法的精密度以六次重复测量的相对标准偏差(RSD)表示,铜和钴的检测限(LOD)分别为±4.10%和±2.30%,以及2.90和3.50 ng/mL。所提出的方法成功应用于实际水样和血清中痕量铜和钴的同时测定,结果令人满意。