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中空纤维支撑的ZIF-8@GO增强溶胶-凝胶用于在紫外可见分光光度法测定百草枯之前的预富集。

Hollow Fiber-Supported ZIF-8@GO Reinforced Sol-Gel for Preconcentration of Paraquat Before Determination by UV-Vis Spectrophotometry.

作者信息

Vaezi Narges, Dalali Naser

机构信息

Phase Separation & FIA Lab., Department of Chemistry, Faculty of Science, University of Zanjan, Zanjan, Iran.

出版信息

J Anal Methods Chem. 2025 Jun 21;2025:6883692. doi: 10.1155/jamc/6883692. eCollection 2025.

Abstract

A novel, sensitive, and efficient method was developed for the determination of paraquat in soil samples, centered on solid-phase microextraction using hollow fiber-supported ZIF-8@GO reinforced sol-gel combined with UV-Vis spectrophotometry at 257 nm. Silica-based ZIF-8@GO was synthesized through sol-gel technology by reacting tetraethyl orthosilicate (TEOS) with hydrochloric acid (HCl) as a catalyst. The resulting solution was injected into hollow polypropylene fiber segments for in situ gelation. Key microextraction parameters, such as the donor phase pH and volume, stirring rate, extraction time, and desorption conditions (solvent type and volume), were systematically studied and optimized. Under optimal conditions, the method demonstrated linearity within the range of 0.5-2000 μg L, with a correlation coefficient of 0.999. The relative standard deviation for seven replicate measurements at a concentration of 600 μg L paraquat was 0.4%. A preconcentration factor of 631 and a detection limit of 0.15 μg L were achieved. Validation of the method was conducted by analyzing soil samples from various sites, yielding recoveries between 96% and 105% with low relative standard deviations, indicating its high accuracy and reliability in detecting trace levels of paraquat.

摘要

开发了一种新颖、灵敏且高效的测定土壤样品中百草枯的方法,该方法以中空纤维支撑的ZIF-8@GO增强溶胶-凝胶结合257nm紫外可见分光光度法的固相微萃取为核心。通过溶胶-凝胶技术,以正硅酸乙酯(TEOS)与盐酸(HCl)作为催化剂反应合成了二氧化硅基ZIF-8@GO。将所得溶液注入中空聚丙烯纤维段进行原位凝胶化。系统研究并优化了关键微萃取参数,如供体相pH值和体积、搅拌速率、萃取时间以及解吸条件(溶剂类型和体积)。在最佳条件下,该方法在0.5-2000μg L范围内呈线性,相关系数为0.999。百草枯浓度为600μg L时七次重复测量的相对标准偏差为0.4%。实现了631的预富集因子和0.15μg L的检测限。通过分析不同地点的土壤样品对该方法进行验证,回收率在96%至105%之间,相对标准偏差较低,表明其在检测痕量百草枯方面具有高准确性和可靠性。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/3160/12226166/c55893cd4a94/JAMC2025-6883692.001.jpg

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