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一种由多酸和氧化石墨烯组成的纳米杂化材料,用于高效液相色谱法测定非甾体抗炎药之前的分散微固相萃取。

A nanohybrid composed of polyoxotungstate and graphene oxide for dispersive micro solid-phase extraction of non-steroidal anti-inflammatory drugs prior to their quantitation by HPLC.

机构信息

Department of Chemistry, Faculty of Sciences, Hakim Sabzevari University, Sabzevar, 96179-76487, Iran.

Department of Chemistry, Faculty of Science, Ferdowsi University of Mashhad, Mashhad, 91775-1436, Iran.

出版信息

Mikrochim Acta. 2019 Jul 16;186(8):534. doi: 10.1007/s00604-019-3694-0.

DOI:10.1007/s00604-019-3694-0
PMID:31312945
Abstract

A nanohybrid was prepared from polyoxotungstate anion and graphene oxide (POT/GO) and characterized in terms of porosity by applying Fourier transform infrared and transmission electron microscopy. The nanohybrid was applied as a sorbent for the dispersive micro solid-phase extraction of the non-steroidal anti-inflammatory drugs (NSAIDs) ibuprofen, diclofenac, and naproxen. Different types of sorbents were compared, and the POT/GO nanohybrid was found to have the best adsorption affinity. The NSAIDs were quantified via HPLC with UV detection. Under the optimum conditions, the limits of detection (at an S/N ratio of 3) range between 0.02-0.03 ng.mL, and the linear response ranges extend from 0.08-200 ng.mL, respectively. The relative standard deviations (RSDs) for five replicates at three concentration levels (0.1, 5 and 100 ng.mL) of NSAIDs ranged from 4.1 to 6.1%. The applicability of the method was confirmed by analyzing spiked real water samples, and satisfactory results were obtained, with recoveries between 95.6 and 99.6%. Graphical abstract Schematic representation of the polyoxotungstate/graphene oxide nanohybrid preparation.

摘要

一种纳米杂化材料由多酸阴离子和氧化石墨烯(POT/GO)制备,并通过傅里叶变换红外和透射电子显微镜对其多孔性进行了表征。该纳米杂化材料被用作非甾体抗炎药(NSAIDs)布洛芬、双氯芬酸和萘普生的分散微固相萃取的吸附剂。比较了不同类型的吸附剂,发现 POT/GO 纳米杂化材料具有最佳的吸附亲和力。通过 HPLC 与紫外检测对 NSAIDs 进行定量分析。在最佳条件下,检测限(信噪比为 3)范围在 0.02-0.03ng.mL 之间,线性响应范围分别扩展到 0.08-200ng.mL。在 NSAIDs 三个浓度水平(0.1、5 和 100ng.mL)的五个重复实验的相对标准偏差(RSD)在 4.1-6.1%之间。通过分析加标实际水样验证了该方法的适用性,获得了令人满意的结果,回收率在 95.6-99.6%之间。

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