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基于核壳型金属有机骨架的分子印迹聚合物用于尿液样品中敌百虫的灵敏选择性磁分散微萃取。

Sensitive and selective magnetic dispersive microextraction of diazinon from urine samples by molecularly imprinted polymer based on core-shell metal-organic frameworks.

机构信息

Department of Occupational Health Engineering, Faculty of Health, , Research Center for Health Sciences Infectious Diseases Research Center, Gonabad University of Medical Sciences, Gonabad, Iran.

Department of Occupational Health Engineering, Research Center for Health Sciences, School of Health, Larestan University of Medical Sciences, Larestan, Iran.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2022 Sep 1;1207:123364. doi: 10.1016/j.jchromb.2022.123364. Epub 2022 Jul 16.

Abstract

A core-shell magnetic metal-organic framework (FeO SiO/ PAEDTC@ MIL- 101 (Fe)) was synthesized as the substrate and then covered with a surface molecularly imprinted polymer (MIP) layer. Next, FeO SiO/ 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, respectively. Excellent extraction recovery (98.5 %), wide linearity range (0.02-200000 ng mL, R > 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.

摘要

一种核壳型磁性金属有机骨架(FeO@SiO/PAEDTC@MIL-101(Fe))被合成作为基底,然后覆盖一层表面分子印迹聚合物(MIP)层。接下来,通过 XRD、FT-IR、BET、VSM、TEM 和 FE-SEM 技术对 FeO@SiO/PAEDTC@MIL-101(Fe)@MIP 进行了表征,并应用于通过 GC-FID 检测方法从尿液样品中选择性、快速和灵敏地磁性分散固相微萃取(M-DµSPE)敌敌畏。通过中心复合设计(CCD)研究并优化了影响 M-DµSPE 的关键实验变量。在最佳条件下(5 mL;样品 pH 值为 7.0,固相吸附剂质量为 6 mg,萃取时间为 4 min,乙腈作为洗脱溶剂 1.5 mL,解吸时间为 3 min,然后用 100 µL 甲醇重新配制),该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。具有良好的萃取回收率(98.5%)、宽线性范围(0.02-200000 ng mL,R > 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 方法可用于高精度和宽线性范围,从真实尿液样品中提取和分析痕量敌敌畏。

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