CAS Key Laboratory of Chemistry of Northwestern Plant Resources and Key Laboratory for Natural Medicine of Gansu Province, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000, China.
Department of Chemistry and Chemical Engineering, Education and Research Center for Smart Energy and Materials, Inha University, Incheon 402-701, Republic of Korea.
J Chromatogr A. 2022 Dec 6;1685:463600. doi: 10.1016/j.chroma.2022.463600. Epub 2022 Nov 2.
In this work, magnetic nitrogen-doped porous carbon (FeO@N-PC) was prepared via incomplete combustion coupled with solvothermal synthesis for extraction of four benzoylureas (BUs) insecticides. Among them, nitrogen-doped porous carbon was produced through incomplete combustion of filter paper loaded with mixture formed by Zn(NO)·6HO and polyethyleneimine solution, and magnetic nanoparticles were further introduced by solvothermal method. Compared with magnetic porous carbon (FeO@PC), the surface hydrophilicity of FeO@N-PC was improved by virtue of the doping of nitrogen atoms, and the dispersion of FeO was more uniform, which greatly exposed the adsorption site. The characterization of FeO@N-PC were carried out by TEM, XRD, elemental analysis, XPS, BET and magnetic hysteresis curve. Besides, FeO@N-PC was successfully used as magnetic solid-phase extraction (MSPE) adsorbent, which showed excellent enrichment factors and extraction recoveries toward polar BUs insecticides due to the polar surface and introduction of Lewis-basic nitrogen. The optimum amount of FeO@N-PC adsorbent, extraction time, pH value, desorption solvent, desorption time and PEI concentration for BUs insecticides extraction were determined to be 3 mg, 10 min, 8, acetone/acetic acid (19:1, V/V), 6 min and 60 g L, respectively. Under this experimental condition, the enrichment factors ranged from 182 to 192 with good intra- and inter-day relative standard deviations (RSDs). The calibration lines were linear over the concentration in the range of 1-800 μg L, the limit of detection (LOD) and limit of quantification (LOQ) were 0.3 μg L as well as 1 μg L, respectively. The recoveries for spiked sample ranged from 90.7 to 107.3% in spiked Yellow River water with the RSDs less than 7.0%. The results showed that the established MSPE strategy based on FeO@N-PC could be used for the detection of trace BUs in complex samples.
在这项工作中，通过不完全燃烧结合溶剂热合成制备了磁性氮掺杂多孔碳（FeO@N-PC），用于提取四种苯甲酰脲（BU）类杀虫剂。其中，氮掺杂多孔碳是通过滤纸负载由 Zn(NO)·6HO 和聚乙烯亚胺溶液形成的混合物不完全燃烧产生的，然后通过溶剂热法进一步引入磁性纳米颗粒。与磁性多孔碳（FeO@PC）相比，由于氮原子的掺杂，FeO@N-PC 的表面亲水性得到提高，FeO 的分散更加均匀，从而大大暴露了吸附位点。通过 TEM、XRD、元素分析、XPS、BET 和磁滞回线对 FeO@N-PC 进行了表征。此外，FeO@N-PC 成功用作磁性固相萃取（MSPE）吸附剂，由于极性表面和路易斯碱性氮的引入，它对极性 BU 类杀虫剂表现出优异的富集因子和萃取回收率。确定了 BU 类杀虫剂萃取的最佳 FeO@N-PC 吸附剂用量、萃取时间、pH 值、解吸溶剂、解吸时间和 PEI 浓度分别为 3mg、10min、8、丙酮/乙酸（19:1，V/V）、6min 和 60gL。在该实验条件下，富集因子范围为 182 至 192，具有良好的日内和日间相对标准偏差（RSD）。校准曲线在 1-800μg L 的浓度范围内呈线性，检测限（LOD）和定量限（LOQ）分别为 0.3μg L 和 1μg L。在黄河水样中加标回收率为 90.7%至 107.3%，RSD 小于 7.0%。结果表明，基于 FeO@N-PC 的建立的 MSPE 策略可用于复杂样品中痕量 BU 的检测。
