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合成一种磁性吸附剂,并将其应用于水样、水果和蔬菜样品中不同农药的提取,然后用气相色谱-串联质谱法对其进行测定。

Synthesis of a magnetic sorbent and its application in extraction of different pesticides from water, fruit, and vegetable samples prior to their determination by gas chromatography-tandem mass spectrometry.

机构信息

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

J Chromatogr A. 2021 Jan 4;1635:461718. doi: 10.1016/j.chroma.2020.461718. Epub 2020 Nov 13.

DOI:10.1016/j.chroma.2020.461718
PMID:33229005
Abstract

In this investigation, an efficient sorbent based on FeO@polyphenols magnetic nanoparticles has been prepared using the extract of Mentha piperita leaves for the first time. The main purposes of this study were synthesis of economically affordable and environmentally friendly sorbent using the extract of Mentha piperita leaves and evaluating its application as a sorbent in magnetic solid phase extraction. The functional groups, magnetic property, size, and shape of the synthesized sorbent were characterized. The sorbent was utilized for the extraction and preconcentration of various pesticides (chlorpyrifos, fenazaquin, penconazole, diniconazole, oxadiazon, haloxyfop-methyl, hexaconazole, clodinafop-propargyl, tebuconazole, and fenoxaprop-p-ethyl) from vegetable, fruit, and water samples. After magnetic solid phase extraction, a dispersive liquid-liquid microextraction method was done to achieve low detection limits. The enriched pesticides were monitored by gas chromatography-tandem mass spectrometry. The synthesized sorbent was characterized by Fourier transform infrared, scanning electron microscopy, energy-dispersive x-ray spectroscopy, x-ray diffraction, and vibrating sample magnetometer techniques, which confirmed the successful synthesis of the magnetic nanoparticles. The effective parameters such as the sorbent weight, ionic strength, pH, vortex time, and kind and volume of elution and extraction solvents were studied. Under optimum extraction conditions, the method showed broad linear ranges (0.05-1000 µg L) with low limits of detection (0.27-4.13 ng L) and quantification (0.91-13.8 ng L). Extraction recoveries and enrichment factors were in the ranges of 54-89 % and 491-811, respectively.

摘要

本研究首次利用胡椒薄荷叶提取物制备了一种基于 FeO@多酚的磁性纳米粒子高效吸附剂。本研究的主要目的是利用胡椒薄荷叶提取物合成经济实惠且环保的吸附剂,并评价其作为磁性固相萃取吸附剂的应用。合成的吸附剂的官能团、磁性、尺寸和形状进行了表征。该吸附剂用于从蔬菜、水果和水样中萃取和预浓缩各种农药(毒死蜱、芬扎喹、丙环唑、戊唑醇、恶草酮、精恶唑禾草灵、己唑醇、氯氟草酯丙炔基、戊唑醇和苯氧丙酚乙酯)。在进行磁性固相萃取后,采用分散液液微萃取方法以达到低检测限。用气相色谱-串联质谱法监测富集的农药。通过傅里叶变换红外光谱、扫描电子显微镜、能谱 X 射线光谱、X 射线衍射和振动样品磁强计技术对合成的吸附剂进行了表征,证实了磁性纳米粒子的成功合成。研究了吸附剂重量、离子强度、pH 值、涡旋时间以及洗脱和萃取溶剂的种类和体积等有效参数。在最佳萃取条件下,该方法具有较宽的线性范围(0.05-1000 µg L),检测限(0.27-4.13 ng L)和定量限(0.91-13.8 ng L)低。萃取回收率和富集因子分别在 54-89%和 491-811 之间。

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