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分子印迹聚合物作为纳米吸附剂用于分散磁性微固相萃取及紫外可见分光光度法测定生物样品中缬沙坦的合成:等温线、动力学和热力学研究

Synthesis of molecularly imprinted polymer as a nanosorbent for dispersive magnetic micro solid-phase extraction and determination of valsartan in biological samples by UV-Vis Spectrophotometry: Isotherm, kinetics, and thermodynamic studies.

作者信息

Azizi-Khereshki Nasibeh, Mousavi Hassan Zavvar, Dogaheh Mahtab Ghasemi, Farsadrooh Majid, Alizadeh Nina, Mohammadi Asadollah

机构信息

Department of Chemistry, Faculty of Science, University of Guilan, Rasht, Iran; Department of Medicinal Chemistry, School of Pharmacy, Guilan University of Medical Sciences, Rasht, Iran.

Department of Chemistry, Faculty of Science, University of Guilan, Rasht, Iran.

出版信息

Spectrochim Acta A Mol Biomol Spectrosc. 2023 Aug 5;296:122656. doi: 10.1016/j.saa.2023.122656. Epub 2023 Mar 21.

Abstract

A magnetic molecularly imprinted polymer (MIP) was synthesized by precipitation polymerization utilizing FeO@SiO-MPS as a magnetic core, itaconic acid as a functional monomer, azobisisobutyronitrile as an initiator, and ethylene glycol dimethacrylate as a cross linker. It was then applied as a nanosorbent for dispersive magnetic micro solid phase extraction (DM-µ-SPE) and determination of valsartan in biological fluids. The morphology and structure of magnetic MIP were characterized by Fourier-transform infrared spectroscopy, Field Emission Scanning electron microscopy, Vibrating sample magnetometer, Energy dispersive x-ray analysis, and Thermogravimetric analysis. The influence of operation conditions on sorption, such as pH (4-10), contact time (10-25 min), initial concentration (1-30 mg L), and temperature (25-40 °C) was investigated. After the extraction step, the valsartan concentration was determined by UV-Vis spectrophotometer at 253 nm. The isotherm and kinetic of valsartan sorption were best fitted by the Langmuir model (R = 0.987) and the Pseudo second-order kinetic model (R = 0.971), respectively. The maximum monolayer sorption capacity for magnetic MIP was obtained to be 4.56 mg g. The analytical approach demonstrated favorable figures of merit, with a linear dynamic range of 10-100 µg L, a low detection limit of 0.56 µg L, and an acceptable preconcentration factor of 5 acquired in optimum conditions. The recoveries of the suggested technique at three spiked levels of analysis were in the range of 101 %-102 %. Valsartan was extracted from various real samples (urine and human blood plasma samples) utilizing the proposed magnetic nanosorbent, and the results exhibited that magnetic MIP was favorable for extraction and measurement of trace amounts of valsartan in biological samples.

摘要

以FeO@SiO-MPS为磁核、衣康酸为功能单体、偶氮二异丁腈为引发剂、乙二醇二甲基丙烯酸酯为交联剂,通过沉淀聚合法合成了磁性分子印迹聚合物(MIP)。然后将其用作纳米吸附剂,用于分散磁性微固相萃取(DM-µ-SPE)并测定生物流体中的缬沙坦。通过傅里叶变换红外光谱、场发射扫描电子显微镜、振动样品磁强计、能量色散X射线分析和热重分析对磁性MIP的形态和结构进行了表征。研究了操作条件对吸附的影响,如pH值(4 - 10)、接触时间(10 - 25分钟)、初始浓度(1 - 30 mg/L)和温度(

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