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基于固体的分散液液微萃取用于邻苯二甲酸酯和己二酸二(2-乙基己基)酯的预浓缩,随后进行气相色谱-火焰离子化检测或质谱分析。

Solid-based disperser liquid-liquid microextraction for the preconcentration of phthalate esters and di-(2-ethylhexyl) adipate followed by gas chromatography with flame ionization detection or mass spectrometry.

作者信息

Farajzadeh Mir Ali, Khorram Parisa, Nabil Ali Akbar Alizadeh

机构信息

Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz, Iran.

出版信息

J Sep Sci. 2014 May;37(9-10):1177-84. doi: 10.1002/jssc.201301306. Epub 2014 Apr 13.

Abstract

A new approach for the development of a dispersive liquid-liquid microextraction followed by GC with flame ionization detection was proposed for the determination of phthalate esters and di-(2-ethylhexyl) adipate in aqueous samples. In the proposed method, solid and liquid phases were used as the disperser and extractant, respectively, providing a simple and fast mode for the extraction of the analytes into a small volume of an organic solvent. In this method, microliter levels of an extraction solvent was added onto a sugar cube and it was transferred into the aqueous phase containing the analytes. By manual shaking, the sugar was dissolved and the extractant was released into the aqueous phase as very tiny droplets to provide a cloudy solution. Under optimized conditions, the proposed method showed good precision (RSD less than 5.2%), high enrichment factors (266-556), and low LODs (0.09-0.25 μg/L). The method was successfully applied for the determination of the target analytes in different samples, and good recoveries (71-103%) were achieved for the spiked samples. No need for a disperser solvent and higher enrichment factors compared with conventional dispersive liquid-liquid microextraction and low cost and short sample preparation time are other advantages of the method.

摘要

提出了一种新的分散液液微萃取结合气相色谱-火焰离子化检测的方法,用于测定水样中的邻苯二甲酸酯和己二酸二(2-乙基己基)酯。在所提出的方法中,分别使用固相和液相作为分散剂和萃取剂,为将分析物萃取到少量有机溶剂中提供了一种简单快速的方式。在该方法中,将微升量的萃取溶剂添加到糖块上,然后将其转移到含有分析物的水相中。通过手动振荡,糖溶解,萃取剂以非常微小的液滴形式释放到水相中,形成浑浊溶液。在优化条件下,所提出的方法显示出良好的精密度(相对标准偏差小于5.2%)、高富集因子(266-556)和低检测限(0.09-0.25μg/L)。该方法成功应用于不同样品中目标分析物的测定,加标样品的回收率良好(71-103%)。与传统的分散液液微萃取相比,无需分散剂溶剂、具有更高的富集因子、低成本和短的样品制备时间是该方法的其他优点。

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