Department of Chemistry, Faculty of Science, Semnan University, Semnan, Islamic Republic of Iran.
Hum Exp Toxicol. 2013 Jun;32(6):620-31. doi: 10.1177/0960327112455672. Epub 2012 Aug 14.
A new, rapid, and simple method for the determination of cadmium in water samples was developed using ionic liquid-based dispersive liquid-liquid microextraction (IL-DLLME) coupled to flame atomic absorption spectrometry (FAAS). In the proposed approach, 2-(5-boromo-2-pyridylazo)-5-(diethyamino) phenol was used as a chelating agent and 1-hexyl-3-methylimidazolium bis(trifluoro methylsulfonyl)imide and acetone were selected as extraction and dispersive solvents, respectively. Sample pH, concentration of chelating agent, amount of ionic liquid (extraction solvent), disperser solvent volume, extraction time, salt effect, and centrifugation speed were selected as interested variables in IL-DLLME process. The significant variables affecting the extraction efficiency were determined using a Placket-Burman design. Thereafter, the significant variables were optimized using a Box-Behnken design and the quadratic model between the dependent and the independent variables was built. The optimum experimental conditions obtained from this statistical evaluation included: pH: 6.7; concentration of chelating agent: 1.1 10(-) (3) mol L(-1); and ionic liquid: 50.0 mg. Under the optimum conditions, the preconcentration factor obtained was 100. Calibration graph was linear in the range of 0.2-60 µg L(-1) with correlation coefficient of 0.9992. The limit of detection was 0.06 µg L(-) (1), which is lower than other reported approaches applied to the determination of cadmium using FAAS. The relative SD (n = 8) was 2.4%. The proposed method was successfully applied to the determination of trace amounts of cadmium in the real water samples with satisfactory results.
采用离子液体分散液液微萃取(IL-DLLME)与火焰原子吸收光谱法(FAAS)联用,建立了一种新的、快速、简单的水样中镉测定方法。在提出的方法中,2-(5-溴-2-吡啶偶氮)-5-(二乙氨基)苯酚被用作螯合剂,1-己基-3-甲基咪唑双(三氟甲基磺酰基)亚胺和丙酮分别被选为萃取和分散溶剂。样品 pH 值、螯合剂浓度、离子液体(萃取溶剂)用量、分散剂溶剂体积、萃取时间、盐效应和离心速度被选为 IL-DLLME 过程中的感兴趣变量。采用 Placket-Burman 设计确定影响萃取效率的显著变量。此后,采用 Box-Behnken 设计对显著变量进行优化,并建立了因变量与自变量之间的二次模型。从该统计评估中获得的最佳实验条件包括:pH 值:6.7;螯合剂浓度:1.1×10-3 mol·L-1;离子液体:50.0 mg。在最佳条件下,获得的预浓缩因子为 100。校准曲线在 0.2-60 µg·L-1 范围内呈线性,相关系数为 0.9992。检测限为 0.06 µg·L-1(1),低于使用 FAAS 测定镉时报道的其他方法。相对标准偏差(n=8)为 2.4%。该方法成功应用于实际水样中痕量镉的测定,结果令人满意。