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基于全因子和中心组合设计的离子液体预富集-微萃取-火焰原子吸收光谱法测定食品中的镍

Determination of nickel in food samples by flame atomic absorption spectroscopy after preconcentration and microextraction based ionic liquids using full factorial and central composite design.

机构信息

Dept. of Analytical Chemistry, Faculty of Chemistry, Univ. College of Science, Univ. of Tehran, Tehran, Iran.

出版信息

J Food Sci. 2012 Dec;77(12):C1242-8. doi: 10.1111/j.1750-3841.2012.02820.x. Epub 2012 Jul 31.

Abstract

In this research, a microextraction technique based on ionic liquids (ILs) termed in situ solvent formation microextraction (ISFME) was used for determination of nickel in solutions. 1-(2-pyridylazo)-2-naphtol (PAN) was chosen as a complexing agent. After preconcentration, the settled IL-phase was dissolved in 50 μL of ethanol and aspirated into the flame atomic absorption spectrometer (FAAS) using a home-made microsample introduction system. Injection of 50 μL volumes of analyte into an air-acetylene flame provided very sensitive spike-like and reproducible signals. ISFME is based on phase separation phenomenon of ionic liquids in aqueous solutions. This method is simple and rapid for extraction and preconcentration of metal ions from food samples and can be applied for the sample solutions containing very high concentrations of salt. Furthermore, this technique is much safer in comparison with the organic solvent extraction because of using ionic liquid. The effective parameters such as amount of IL, salt effect, concentration of the chelating agent and ion pairing agent were inspected by a full factorial design to identify important parameters and their interactions. Next, a central composite design was applied to obtain optimum point of the important parameters. Under the optimum conditions, the calibration graph was linear over the range of 2 to 80 ng/mL. The limit of detection and relative standard deviation (n= 6) were 0.6 ng/mL and 2%, respectively.

摘要

在这项研究中,使用了一种基于离子液体(ILs)的微萃取技术,称为原位溶剂形成微萃取(ISFME),用于测定溶液中的镍。1-(2-吡啶偶氮)-2-萘酚(PAN)被选为络合剂。在预浓缩后,沉淀的 IL 相溶解在 50μL 的乙醇中,并使用自制的微样品进样系统吸入火焰原子吸收光谱仪(FAAS)中。将 50μL 体积的分析物注入空气-乙炔火焰中,可提供非常灵敏的尖峰状和可重现的信号。ISFME 基于离子液体在水溶液中的相分离现象。该方法简单快速,可用于从食品样品中萃取和预浓缩金属离子,并可用于含有高浓度盐的样品溶液。此外,由于使用了离子液体,与有机溶剂萃取相比,该技术更安全。通过完全析因设计检查了 IL 量、盐效应、络合剂和离子对试剂的浓度等有效参数,以确定重要参数及其相互作用。接下来,应用中心组合设计获得重要参数的最佳点。在最佳条件下,校准曲线在 2 至 80ng/mL 范围内呈线性。检测限和相对标准偏差(n=6)分别为 0.6ng/mL 和 2%。

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