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盐和 pH 值诱导的固态浮动有机液滴均相液相微萃取法的开发用于提取新鲜水果和果汁中的十种拟除虫菊酯类杀虫剂,随后进行气相色谱-质谱分析。

Development of salt and pH-induced solidified floating organic droplets homogeneous liquid-liquid microextraction for extraction of ten pyrethroid insecticides in fresh fruits and fruit juices followed by gas chromatography-mass spectrometry.

机构信息

Faculty of Traditional Medicine and Faculty of Nutrition, Tabriz University of Medical Sciences, Tabriz, Iran.

Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz, Iran; Engineering Faculty, Near East University, 99138 Nicosia, North Cyprus Mersin 10, Turkey.

出版信息

Talanta. 2018 Jan 1;176:565-572. doi: 10.1016/j.talanta.2017.08.074. Epub 2017 Aug 24.

Abstract

A new microextraction method named salt and pH-induced homogeneous liquid-liquid microextraction has been developed in a home-made extraction device for the extraction and preconcentration of some pyrethroid insecticides from different fruit juice samples prior to gas chromatography-mass spectrometry. In the present work, an extraction device made from two parallel glass tubes with different lengths and diameters was used in the microextraction procedure. In this method, a homogeneous solution of a sample solution and an extraction solvent (pivalic acid) was broken by performing an acid-base reaction and the extraction solvent was produced in whole of the solution. The produced droplets of the extraction solvent went up through the solution and solidified using an ice-bath. They were collected without centrifugation step. Under the optimum conditions, limits of detection and quantification were obtained in the ranges of 0.006-0.038, and 0.023-0.134ngmL, respectively. The enrichment factors and extraction recoveries of the selected analytes ranged from 365-460 to 73-92%, respectively. The relative standard deviations were lower than 9% for intra- (n = 6) and inter-day (n = 4) precisions at a concentration of 1ngmL of each analyte. Finally, some fruit juice samples were effectively analyzed by the proposed method.

摘要

一种名为盐和 pH 值诱导均相液-液微萃取的新微萃取方法已在自制萃取装置中开发,用于在气相色谱-质谱分析之前从不同果汁样品中萃取和预浓缩一些拟除虫菊酯类杀虫剂。在本工作中,在微萃取过程中使用了由两根不同长度和直径的平行玻璃管制成的萃取装置。在该方法中,通过酸碱反应使样品溶液和萃取溶剂(特戊酸)的均相溶液破裂,并在整个溶液中产生萃取溶剂。产生的萃取溶剂液滴通过溶液上升并使用冰浴凝固。无需离心步骤即可收集。在最佳条件下,检测限和定量限分别在 0.006-0.038 和 0.023-0.134ngmL 范围内获得。所选分析物的富集因子和萃取回收率范围分别为 365-460 至 73-92%。在 1ngmL 每种分析物的浓度下,日内(n=6)和日间(n=4)精密度的相对标准偏差均低于 9%。最后,通过所提出的方法有效地分析了一些果汁样品。

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