Department of Chemistry, Faculty of Sciences, Azarbaijan Shahid Madani University, 35 Km Tabriz-Marageh Road, PO Box 53714-161, Tabriz, Iran.
Department of Chemistry, Faculty of Sciences, Azarbaijan Shahid Madani University, 35 Km Tabriz-Marageh Road, PO Box 53714-161, Tabriz, Iran.
Talanta. 2015 Mar;134:387-393. doi: 10.1016/j.talanta.2014.11.054. Epub 2014 Dec 2.
A magnetic solid phase extraction method based on β-cyclodextrin (β-CD) grafted graphene oxide (GO)/magnetite (Fe3O4) nano-hybrid as an innovative adsorbent was developed for the separation and pre-concentration of gemfibrozil prior to its determination by spectrofluorometry. The as-prepared β-CD/GO/Fe3O4 nano-hybrid possesses the magnetism property of Fe3O4 nano-particles that makes it easily manipulated by an external magnetic field. On the other hand, the surface modification of GO by β-CD leads to selective separation of the target analyte from sample matrices. The structure and morphology of the synthesized adsorbent were characterized using powder X-ray diffraction, Fourier transform infrared spectroscopy, and field emission scanning electron microscopy. The experimental factors affecting the extraction/pre-concentration and determination of the analyte were investigated and optimized. Under the optimized experimental conditions, the calibration graph was linear in the range between 10 and 5000 pg mL(-1) with a correlation coefficient of 0.9989. The limit of detection and enrichment factor for gemfibrozil were 3 pg mL(-1) and 100, respectively. The maximum sorption capacity of the adsorbent for gemfibrozil was 49.8 mg g(-1). The method was successfully applied to monitoring gemfibrozil in human serum and pharmaceutical wastewaters samples with recoveries in the range of 96.0-104.0% for the spiked samples.
一种基于β-环糊精(β-CD)接枝氧化石墨烯(GO)/磁铁矿(Fe3O4)纳米杂化体的磁性固相萃取方法被开发出来,用于在荧光光度法测定前分离和预浓缩吉非贝齐。所制备的β-CD/GO/Fe3O4纳米杂化物具有 Fe3O4纳米粒子的磁性,使其可以通过外部磁场轻松操作。另一方面,GO 表面由β-CD 修饰,导致目标分析物从样品基质中选择性分离。采用粉末 X 射线衍射、傅里叶变换红外光谱和场发射扫描电子显微镜对合成吸附剂的结构和形态进行了表征。考察并优化了影响萃取/预浓缩和分析物测定的实验因素。在优化的实验条件下,校准曲线在 10 至 5000 pg mL(-1) 范围内呈线性,相关系数为 0.9989。吉非贝齐的检出限和富集因子分别为 3 pg mL(-1) 和 100。该吸附剂对吉非贝齐的最大吸附容量为 49.8 mg g(-1)。该方法成功应用于人血清和制药废水中吉非贝齐的监测,加标样品的回收率在 96.0-104.0%范围内。