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基于深共晶溶剂的超声辅助分散液液微萃取法用于水样和食品样中硒(IV)和(VI)形态分析、预浓缩和测定。

Ultrasonic assisted dispersive liquid-liquid microextraction method based on deep eutectic solvent for speciation, preconcentration and determination of selenium species (IV) and (VI) in water and food samples.

机构信息

National Centre of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080, Pakistan; Gaziosmanpasa University, Faculty of Science and Arts, Chemistry Department, 60250 Tokat, Turkey.

Gaziosmanpasa University, Faculty of Science and Arts, Chemistry Department, 60250 Tokat, Turkey.

出版信息

Talanta. 2017 Dec 1;175:352-358. doi: 10.1016/j.talanta.2017.07.063. Epub 2017 Jul 22.

Abstract

A novel ultrasound-assisted liquid phase microextraction (UALPME) based on environmental friendly extractants, deep eutectic solvent (DES) was first time presented for speciation of selenium. In present study, five DES solvents of different composition was prepared and used as efficient extractive medium for hydrophobic chelate of Se(IV) with 3,3'-Diaminobenzidine (DAB). The total inorganic Se species were determined after pre-reduction of Se(VI) to Se(IV), prior to applying developed method. The concentration of Se(VI) was calculated by the difference of Se(IV) values and total selenium contents. The concentration of Se in DES rich phase was measured with electrothermal atomic absorption spectrometer (ETAAS). The effects of different parameters on extraction efficiency of study analyte, including pH, ligand concentration, type and volume of DES, sonication time, volumes tetrahydrofuran and aqueous samples were examined. At the optimum conditions, limit of detection and quantification, preconcentration factor, and relative standard deviation (RSD %) were determined as 4.61ngL, 15.4ngL, 50% and 4.1%, respectively. The accuracy of the presented method was confirmed by analysis of certified reference material and standard addition method for different water and ice tea samples. The developed method was effectively applied to real water and food samples.

摘要

首次提出了一种基于环境友好型萃取剂——深共晶溶剂(DES)的新型超声辅助液相微萃取(UALPME)方法,用于硒的形态分析。在本研究中,制备了五种不同组成的 DES 溶剂,并将其用作 3,3'-二氨基联苯胺(DAB)与 Se(IV) 的疏水性螯合物的有效萃取介质。在应用所开发的方法之前,先用预还原将 Se(VI)还原为 Se(IV),以测定总无机硒物种。通过 Se(IV)值与总硒含量的差值计算 Se(VI)的浓度。DES 富相中 Se 的浓度用电热原子吸收光谱仪(ETAAS)测定。考察了不同参数对研究分析物萃取效率的影响,包括 pH 值、配体浓度、DES 的类型和体积、超声时间、四氢呋喃和水样的体积。在最佳条件下,测定了检出限和定量限、预浓缩因子和相对标准偏差(RSD%)分别为 4.61ng/L、15.4ng/L、50%和 4.1%。通过对不同水样和冰茶样品的标准物质分析和标准加入法验证了所提出方法的准确性。该方法已成功应用于实际水样和食品样品的分析。

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