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使用两种配体的温度控制离子液体基分散微萃取法测定阿尔茨海默病患者头皮毛发样本中的铝:一项多变量研究

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.

作者信息

Arain Mariam S, Arain Salma A, Kazi Tasneem G, Afridi Hassan I, Ali Jamshaid, Arain Sadaf S, Brahman Kapil Dev, Mughal Moina Akhtar

机构信息

National Centre of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080, Pakistan.

National Centre of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080, Pakistan.

出版信息

Spectrochim Acta A Mol Biomol Spectrosc. 2015 Feb 25;137:877-85. doi: 10.1016/j.saa.2014.08.068. Epub 2014 Sep 16.

Abstract

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 (Al(3+)) in scalp hair samples of Alzheimer's (AD) patients, prior to analyzing by flame atomic absorption spectrometry (FAAS). The Al(3+) 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 (3s) and enhancement factor were 0.56 μg L(-1), 0.64 μg L(-1) and 85, 73 for both ligands, respectively. The relative standard deviation (RSD) for six replicate determinations of 100 μg L(-1) Al(3+) 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 Al(3+) 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.

摘要

提出了一种基于应用离子液体1-丁基-3-甲基咪唑六氟磷酸盐([C4mim][PF6])作为萃取溶剂的绿色灵敏温度控制分散液液微萃取(TIL-DLLME)方法,用于在通过火焰原子吸收光谱法(FAAS)分析之前对阿尔茨海默病(AD)患者头皮头发样本中的痕量铝(Al(3+))进行预富集。Al(3+)分别与8-羟基喹啉(oxine)(L1)和3,5,7,2'-4'五羟基黄酮(桑色素)(L2)络合,然后在温度(50±2.0°C)下用离子液体萃取。通过多变量分析研究并优化了一些影响TIL-DLLME效率的有效因素,如pH、配体浓度、离子液体体积、离子强度和孵育时间。在最佳实验条件下,两种配体的检测限(3s)和富集因子分别为0.56 μg L(-1)、0.64 μg L(-1)以及85、73。对于与oxine和桑色素络合的100 μg L(-1) Al(3+)进行六次重复测定,相对标准偏差(RSD)分别为3.88%和4.74%。通过分析人发标准参考物质(NCSZC81002)对所建立的方法进行了验证,并令人满意地应用于AD患者和健康对照者酸消解头皮头发样本中Al(3+)的测定。所得数据表明,AD男性患者头皮头发样本中的铝含量显著高于同年龄和社会经济地位的对照者。

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