目的 探索合成聚乙二醇改性的磁性共价有机框架(MCOF-COOH),并将其用于萃取检测水样中的拟除虫菊酯类农药。方法 以均苯三甲酰氯和对苯二胺为原料在室温下一锅法合成共价有机框架(COF-COOH),在其表面通过共沉淀法负载聚乙二醇改性的Fe3O4纳米颗粒,合成聚乙二醇改性磁性共价有机框架(MCOF-COOH),将其作为萃取水样中拟除虫菊酯类农药的磁性吸附剂,用高效液相色谱法进行检测。结果 MCOF-COOH具有吸附效率高、萃取速度快等特点,对两种生活水的中、低加标浓度下具有较好的加标回收率(78.98%~118.04%),相对标准偏差为2.52%~9.05%。结论 合成MCOF-COOH以及建立的磁固相萃取-高效液相色谱法可以快速高效的萃取检测水样中拟除虫菊酯类农药残留。
Abstract
Objective To explore the synthetic magnetic covalent organic framework modified by polyethylene glycol (MCOF-COOH)and apply it to the extraction and detection of pyrethroid pesticides in water samples. Methods The covalent organic framework (COF-COOH) was synthesized by one-pot method with trimesoyl chloride and p-phenylenediamine as raw materials at room temperature.The magnetic covalent organic framework (MCOF-COOH) modified by polyethylene glycol was synthesized by co-precipitation loading of PEG-modified Fe3O4 nanoparticles on its surface.MCOF-COOH was used as magnetic adsorbent for pyrethroid pesticide in extracted water and detected by high performance liquid chromatography (HPLC). Results MCOF-COOH extraction technology had the characteristics of high adsorption efficiency and fast extraction speed,and had good spiked recovery (78.98%~118.04%) for the two kinds of domestic water at the low and medium spiked concentration,with the relative standard deviation (RSD) of 2.52%~9.05%. Conclusion MCOF-COOH and establishing a magnetic solid-phase extraction-high performance liquid chromatography method,pyrethroid pesticide residues in water samples can be extracted and detected rapidly and efficiently.
关键词
磁性共价有机框架 /
磁性固相萃取 /
拟除虫菊酯类农药残留 /
聚乙二醇
Key words
Magnetic covalent organic frameworks /
Magnetic solid-phase extraction /
Pyrethroid pesticide residues /
Polyethylene glycol
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基金
中国农业大学创新训练项目(X2021100190830)
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