Department of Analytical Chemistry, Faculty of Chemistry, K.N. Toosi University of Technology, Tehran, Iran.
Department of Analytical Chemistry, Faculty of Chemistry, K.N. Toosi University of Technology, Tehran, Iran.
J Chromatogr A. 2019 Dec 6;1607:460387. doi: 10.1016/j.chroma.2019.460387. Epub 2019 Jul 19.
In this work, porphyrin-functionalized graphene oxide nanosheets (GO@meso-tetrakis(4-hydroxyphenyl)porphyrin) were synthesized and employed as the sorbent. Porphyrins owing to their unique structures and tunable terminal functional groups are expected to be promising media for extraction of the desired analytes. Also, GO with a high specific surface area has exhibited good potential for the extraction purposes. Inspired by these intriguing properties, the combination of GO and porphyrin can benefit both of these amazing features. The synthesized sorbent was utilized for micro solid phase extraction of non-steroidal anti-inflammatory drugs followed by HPLC-UV. Optimization of the experimental factors including sorbent amount, sample pH, sample and eluent flowrates, eluent volume, and the number of desorption cycles were performed with the aid of central composite design. Under the optimal conditions, the calibration curves were linear within the range of 2.0-600 ng mL and limits of detection were found between 0.5-2.0 ng mL. The preconcentration factors and absolute recoveries were obtained in the range of 4.80-9.79 and 29%-59%, respectively. The matrix effect for the urine samples varied between 81.9%-91.6% at two concentrations of 50 and 300 ng mL, respectively. Intra- and inter-day RSD% (n = 3) of the spiked urine samples at three level concentrations of 25, 100, and 300 ng mL were less than 10%. The relative recoveries of the urine samples were calculated in the range of 85.2-98.6%. Eventually, the method exhibits proper sensitivity, excellent repeatability, high reusability, and acceptable precision and accuracy.
在这项工作中,合成了卟啉功能化氧化石墨烯纳米片(GO@meso-四(4-羟基苯基)卟啉),并将其用作吸附剂。卟啉由于其独特的结构和可调节的末端官能团,有望成为提取所需分析物的有前途的介质。此外,具有高比表面积的 GO 在萃取方面也表现出了良好的潜力。受这些引人入胜的特性的启发,GO 和卟啉的组合可以同时受益于这两种特性。合成的吸附剂用于非甾体抗炎药的微固相萃取,然后进行 HPLC-UV 分析。在中心复合设计的辅助下,优化了实验因素,包括吸附剂用量、样品 pH 值、样品和洗脱液流速、洗脱液体积和洗脱循环次数。在最佳条件下,校准曲线在 2.0-600ng/mL 范围内呈线性,检出限在 0.5-2.0ng/mL 之间。浓缩因子和绝对回收率分别在 4.80-9.79 和 29%-59%的范围内。两种浓度为 50 和 300ng/mL 时,尿液样品的基质效应在 81.9%-91.6%之间变化。在三个浓度水平 25、100 和 300ng/mL 下,加标尿液样品的日内和日间 RSD%(n=3)均小于 10%。尿液样品的相对回收率在 85.2-98.6%的范围内。最终,该方法表现出适当的灵敏度、优异的重复性、高的可重复使用性以及可接受的精密度和准确性。