In this work, an octahedral magnetic metal organic frameworks composed of Fe₃O₄@NH₂-MIL-101 was synthesized through simple solvothermal reaction for magnetic solid phase extraction (MSPE) of six pesticides with benzene ring in environmental water samples. The Fe₃O₄@NH₂-MIL-101 was characterized by various techniques. The results showed Fe₃O₄@NH₂-MIL-101 exhibits ultra-high surface area (1012.7 m² g⁻¹), large pore volume (0.64 cm³ g⁻¹) and high magnetic responsivity (30.0 emu g⁻¹), which can be used as an ideal adsorbent for rapid isolation and enrichment of target analytes. A sensitive method was developed by using Fe₃O₄@NH₂-MIL-101-based MSPE coupled with HPLC (High performance liquid chromatography) with UV (Ultraviolate) detector. The linear range extended to 1000 µg L⁻¹ was achieved, low limits of detection (S/N = 3) of 0.13–0.86 µg L⁻¹ and good reproducibility (1.8–3.1%). The applicability of Fe₃O₄@NH₂-MIL-101 was demonstrated for determining six pesticides in water samples with satisfactory recoveries at two spiking levels of 20.0, 80.0 µg L⁻¹ were in the range of 70.5 to 119.8% with the RSDs less than 8.1%. These accurate experimental results by this method indicated that the novel Fe₃O₄@NH₂-MIL-101 as a MSPE adsorbent was an attractive option for efficient extraction and enrichment trace pesticides in future.

本文通过简单的溶剂热反应合成了Fe ₃ O ₄ @NH ₂ -MIL-101组成的八面体磁性金属有机骨架，用于环境水样中六种农药与苯环的磁性固相萃取（MSPE）。通过各种技术表征了Fe ₃ O ₄ @NH ₂ -MIL-101。结果表明，Fe ₃ O ₄ @NH ₂ -MIL-101具有超高的表面积（1012.7 m ² g ^-1），大的孔体积（0.64 cm ³ g ^-1）和高的磁响应率（30.0 emu g ^-1）），可以用作快速分离和富集目标分析物的理想吸附剂。通过使用基于Fe ₃ O ₄ @NH ₂ -MIL-101的MSPE结合带有UV（紫外线）检测器的HPLC（高效液相色谱）开发了一种灵敏的方法。线性范围扩展至1000 µg L ^-1，检测限（S / N = 3）低至0.13–0.86 µg L ^-1，重现性好（1.8–3.1％）。证明了Fe ₃ O ₄ @NH ₂ -MIL-101的适用性用于测定水样中的六种农药，两种加标水平分别为20.0，80.0 µg L ^-1时，回收率令人满意范围在70.5至119.8％之间，相对标准偏差小于8.1％。通过这种方法得到的准确实验结果表明，新型的Fe ₃ O ₄ @NH ₂ -MIL-101作为MSPE吸附剂是将来有效萃取和富集微量农药的有吸引力的选择。