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二氧化硅包覆氧化石墨烯表面的分子印迹聚合物用于从生物样品中快速、选择性地分散固相萃取卡马西平。

Molecularly imprinted polymer on a SiO2 -coated graphene oxide surface for the fast and selective dispersive solid-phase extraction of Carbamazepine from biological samples.

作者信息

Khalilian Faezeh, Ahmadian Setareh

机构信息

Department of Chemistry, College of Basic Science, Yadegar-e-Imam Khomeini (RAH) Shahre Rey Branch, Islamic Azad University, Tehran, Iran.

出版信息

J Sep Sci. 2016 Apr;39(8):1500-8. doi: 10.1002/jssc.201501392. Epub 2016 Mar 23.

Abstract

A surface carbamazepine-imprinted polymer was grafted and synthesized on the SiO2 /graphene oxide surface. Firstly SiO2 was coated on synthesized graphene oxide sheet using the sol-gel technique. Prior to polymerization, the vinyl group was incorporated on to the surface of SiO2 /graphene oxide to direct selective polymerization on the surface. Methacrylic acid, ethylene glycol dimethacrylate and ethanol were used as monomer, cross-linker and porogen, respectively. Nonimprinted polymer was also prepared for comparison. The properties of the molecularly imprinted polymer were characterized using field-emission scanning electron microscopy and Fourier-transform infrared spectroscopy. The surface molecularly imprinted polymer was utilized as an adsorbent of dispersive solid-phase extraction for separation and preconcentration of carbamazepine. The effects of the different parameters influencing the extraction efficiency, such as sample pH were investigated and optimized. The specificity of the molecular imprinted polymer over the nonimprinted polymer was examined in absence and presence of competitive drugs. The carbamazepine calibration curve showed linearity in the ranges 0.5-500 μg/L. The limits of detection and quantification under the optimized conditions were 0.1 and 0.3 μg/L, respectively. The within-day and between-day relative standard deviations (n = 3) were 3.6 and 4.3%, respectively. Furthermore, the relative recoveries for spiked biological samples were above 85%.

摘要

一种表面印有卡马西平的聚合物接枝并合成于二氧化硅/氧化石墨烯表面。首先,采用溶胶-凝胶技术将二氧化硅包覆在合成的氧化石墨烯片上。在聚合反应之前,将乙烯基引入到二氧化硅/氧化石墨烯表面,以引导在该表面进行选择性聚合。分别使用甲基丙烯酸、乙二醇二甲基丙烯酸酯和乙醇作为单体、交联剂和致孔剂。还制备了非印迹聚合物用于比较。利用场发射扫描电子显微镜和傅里叶变换红外光谱对分子印迹聚合物的性能进行了表征。表面分子印迹聚合物用作分散固相萃取的吸附剂,用于卡马西平的分离和预富集。研究并优化了不同参数(如样品pH值)对萃取效率的影响。在有无竞争药物存在的情况下,考察了分子印迹聚合物相对于非印迹聚合物的特异性。卡马西平校准曲线在0.5 - 500 μg/L范围内呈线性。优化条件下的检测限和定量限分别为0.1和0.3 μg/L。日内和日间相对标准偏差(n = 3)分别为3.6%和4.3%。此外,加标生物样品的相对回收率高于85%。

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