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无有机溶剂模式下基于漂浮有机液滴的分散液液微萃取用于从蜂蜜样品中萃取多环芳烃,然后用气相色谱-质谱法测定。

Development of organic solvents-free mode of solidification of floating organic droplet-based dispersive liquid-liquid microextraction for the extraction of polycyclic aromatic hydrocarbons from honey samples before their determination by gas chromatography-mass spectrometry.

机构信息

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

Food and Drug Safety Research Center, Tabriz University of Medical Sciences, Tabriz, Iran.

出版信息

J Sep Sci. 2020 Jun;43(12):2393-2400. doi: 10.1002/jssc.202000136. Epub 2020 Apr 2.

DOI:10.1002/jssc.202000136
PMID:32145048
Abstract

In this study, a green mode of solidification of floating organic droplet-based dispersive liquid-liquid microextraction has been developed for the extraction of 16 polycyclic aromatic hydrocarbons from honey samples before their determination by gas chromatography-mass spectrometry. In this method, an appropriate volume of menthol:decanoic acid deep eutectic solvent (as an extraction solvent) is added on a sugar cube (as a disperser agent). In the following, the cube is released into the diluted honey sample placed in a tube. After manual shaking a cloudy state is obtained as a result of dispersing the extraction solvent droplets throughout the sample solution and the analytes are extracted into them. After placing the tube in an ice bath, the droplet of the extractant is solidified on the top of the solution. This drop is taken and after dissolving in acetonitrile, an aliquot of the solution is injected into the separation system. Under optimum conditions, the suggested approach had high extraction recoveries (76-93%) and enrichment factors (380-465), low limits of detection (14-52 ng/kg) and quantification (47-173 ng/kg), and satisfactory repeatability (relative standard deviation ≤ 9%).

摘要

在这项研究中,开发了一种基于浮有机液滴的分散液液微萃取的绿色固化模式,用于从蜂蜜样品中提取 16 种多环芳烃,然后通过气相色谱-质谱法进行测定。在该方法中,加入适量的薄荷醇:癸酸深共晶溶剂(作为萃取溶剂)在方糖(作为分散剂)上。接下来,将方糖释放到放置在试管中的稀释蜂蜜样品中。手动摇晃后,由于萃取溶剂液滴分散在整个样品溶液中,使溶液呈现混浊状态,分析物被萃取到其中。将试管置于冰浴中后,萃取剂液滴在溶液顶部凝固。取出该液滴,溶解在乙腈中,然后取一部分溶液注入分离系统。在最佳条件下,该方法具有较高的萃取回收率(76-93%)和富集因子(380-465),较低的检测限(14-52 ng/kg)和定量限(47-173 ng/kg),并且重复性良好(相对标准偏差≤9%)。

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