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Sensitive and selective magnetic dispersive microextraction of diazinon from urine samples by molecularly imprinted polymer based on core–shell metal–organic frameworks
Journal of Chromatography B ( IF 3 ) Pub Date : 2022-07-16 , DOI: 10.1016/j.jchromb.2022.123364
Ali Firoozichahak 1 , Abdolrasoul Rahmani 2 , Faeze Mehregan 3 , Razzagh Rahimpoor 2
Affiliation  

A core–shell magnetic metal–organic framework (Fe3O4 SiO2/ PAEDTC@ MIL- 101 (Fe)) was synthesized as the substrate and then covered with a surface molecularly imprinted polymer (MIP) layer. Next, Fe3O4 SiO2/ PAEDTC@ MIL- 101 (Fe) @ MIP was characterized by XRD, FT-IR, BET, VSM, TEM, and FE-SEM techniques and applied for selective, fast, and sensitive magnetic dispersive solid-phase microextraction (M-DµSPE) of diazinon from urine samples by the GC- FID detection method. The key experimental variables affecting M-DµSPE were studied and optimized by central composite design (CCD). Under optimum conditions (5 mL; sample at pH: 7.0, the mass of solid sorbent; 6 mg, extraction time; 4 min, acetonitrile as an eluent solvent; 1.5 mL, and desorption time; 3 min, and then reconstituted with 100 µL of methanol), the proposed method exhibits high sensitivity with limits of detection and quantification of 0.005 and 0.017 ng mL−1, respectively. Excellent extraction recovery (98.5 %), wide linearity range (0.02–200000 ng mL−1, R2 > 0.992), high enrichment factors (47–53), and satisfactory precision (<6.3 % RSD) were achieved. The MIP- MOF@ M-DµSPE -GC-FID method can be used with high precision and wide linearity to extract and analyze trace levels of diazinon in real urine samples.



中文翻译:

基于核-壳金属-有机骨架的分子印迹聚合物对尿样中二嗪农的灵敏选择性磁色散微萃取

合成了核壳磁性金属有机骨架(Fe 3 O 4 SiO 2 / PAEDTC@MIL-101 (Fe))作为基底,然后覆盖有表面分子印迹聚合物(MIP)层。接下来,Fe 3 O 4 SiO 2/ PAEDTC@MIL-101 (Fe)@MIP 通过 XRD、FT-IR、BET、VSM、TEM 和 FE-SEM 技术进行表征,并应用于选择性、快速、灵敏的磁分散固相微萃取 (M-DµSPE) ) 通过 GC-FID 检测方法从尿样中检测二嗪农。通过中心复合设计 (CCD) 研究和优化了影响 M-DµSPE 的关键实验变量。在最佳条件下(5 mL;样品 pH:7.0,固体吸附剂的质量;6 mg,萃取时间;4 分钟,乙腈作为洗脱溶剂;1.5 mL,解吸时间;3 分钟,然后用 100 µL 复溶甲醇),所提出的方法表现出高灵敏度,检测限和定量限分别为 0.005 和 0.017 ng mL -1。出色的萃取回收率 (98.5 %),宽线性范围 (0.02–200000 ng mL)-1 , R 2  > 0.992)、高富集因子 (47–53) 和令人满意的精密度 (<6.3 % RSD)。MIP-MOF@ M-DµSPE -GC-FID 方法可用于提取和分析真实尿样中痕量二嗪农,具有高精度和宽线性。

更新日期:2022-07-16
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