Temperature controlled ionic liquid-based dispersive micro-extraction using two ligands, for determination of aluminium in scalp hair samples of Alzheimer's patients: a multivariate study.
Temperature controlled ionic liquid-based dispersive micro-extraction using two ligands, for determination of aluminium in scalp hair samples of Alzheimer's patients: a multivariate study.
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DOI：
10.1016/j.saa.2014.08.068
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发表时间：
2015-02
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通讯作者：
M. S. Arain;S. Arain;T. Kazi;H. I. Afridi;Jamshaid Ali;Naeemulllah;S. S. Arain-S.;K. D. Brahman;M. A. Mughal
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作者：
M. S. Arain;S. Arain;T. Kazi;H. I. Afridi;Jamshaid Ali;Naeemulllah;S. S. Arain-S.;K. D. Brahman;M. A. Mughal
以离子液体1-丁基-3-甲基咪唑六氟磷酸盐[C4 mim][PF 6]为萃取剂，建立了一种绿色、灵敏的温控分散液液微萃取（TIL-DLLME）方法，用于阿尔茨海默病（AD）患者头发样品中痕量铝（Al 3+）的预富集和火焰原子吸收光谱（FAAS）分析。Al ~（3+）分别与8-羟基喹啉（oxine）（L_1）和3，5，7，2 ′-4′五羟基黄酮（morin）（L_2）络合，在50 ± 2.0 °C下用离子液体萃取。通过多变量分析对影响TIL-DLLME效率的一些因素如pH、配体浓度、IL体积、离子强度和孵育时间进行了研究和优化。在最佳实验条件下，两种配体的检测限（3s）和增强因子分别为0.56 μg L-1，0.64 μg L-1，85，73。100 μg L− 1Al 3+与8-羟基喹啉和桑色素络合物的6次重复测定的相对标准偏差（RSD）分别为3.88%和4.74%。方法经人发标准物质NCSZC 81002验证，并用于AD患者和健康人发样品中Al ~（3+）的测定，结果满意。结果显示，AD男性患者的头发样本中的水平显著高于同龄和社会经济地位的参照物。
A green and sensitive temperature controlled dispersive liquid–liquid microextraction (TIL-DLLME) methodology based on the application of ionic liquid 1-butyl-3-methylimidazolium hexafluorophosphate, [C4mim][PF6], as an extractant solvent was proposed for the preconcentration of trace levels of aluminium (Al3+) in scalp hair samples of Alzheimer’s (AD) patients, prior to analyzing by flame atomic absorption spectrometry (FAAS). The Al3+was complexed with 8-hydrooxyquinoline (oxine) (L1) and 3,5,7,2′-4′ pentahydroxy flavone (morin) (L2) separately and then extracted by IL at temperature (50 ± 2.0 °C). Some effective factors that influence the TIL-DLLME efficiency such as pH, ligands concentrations, volume of IL, ionic strength, and incubation time were investigated and optimized by multivariate analysis. In the optimum experimental conditions, the limit of detection (3 s) and enhancement factor were 0.56 μg L−1, 0.64 μg L−1and 85, 73 for both ligands, respectively. The relative standard deviation (RSD) for six replicate determinations of 100 μg L−1Al3+complexed with oxine and morin were found to be 3.88% and 4.74%, respectively. The developed method was validated by the analysis of certified reference material of human hair (NCSZC81002).and applied satisfactorily to the determination of Al3+in acid digested scalp hair samples of AD patients and healthy controls. The resulted data shows significant higher level in scalp hair samples of AD male patients with related to referents of same age and socioeconomic status.