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磁性 FeO@nSiO@mSiO-NH 核壳介孔纳米复合材料的制备及其在尿液和血浆样品中高效超声辅助分散 µSPE-荧光光谱法检测氧氟沙星中的应用。

Fabrication of magnetic FeO@nSiO@mSiO-NH core-shell mesoporous nanocomposite and its application for highly efficient ultrasound assisted dispersive µSPE-spectrofluorimetric detection of ofloxacin in urine and plasma samples.

机构信息

Chemistry Department, College of Science, Shahid Chamran University of Ahvaz, Ahvaz, Iran.

Chemistry Department, College of Science, Shahid Chamran University of Ahvaz, Ahvaz, Iran.

出版信息

Ultrason Sonochem. 2018 Jan;40(Pt A):101-112. doi: 10.1016/j.ultsonch.2017.06.027. Epub 2017 Jun 29.

DOI:10.1016/j.ultsonch.2017.06.027
PMID:28946397
Abstract

In this research, a sensitive, simple and rapid ultrasound assisted dispersive micro solid-phase extraction (USAD-µSPE) was developed using a synthesized core-shell magnetic mesoporous nanocomposite (FeO@nSiO@mSiO-NH) as an efficient adsorbent for the preconcentration and spectrofluorometric determination of ofloxacin (OFL) in biological samples. The synthesized adsorbent was characterized using FT-IR spectroscopy, transmission electron microscopy (TEM), vibrating sample magnetometer (VSM), energy dispersive X-ray (EDX) spectroscopy, thermogravimetric analysis (TGA) and Brunauer-Emmett-Teller (BET) analysis. The application of this magnetic nanocomposite as a sensitive solid phase for removal, preconcentration and spectrofluorometric quantification of trace amount of OFL was developed. Influence of various variables including pH, sorbent dosage, desorption solvent properties and sonication time on present method response was studied and optimized. The results showed that using the proposed method OFL can be determined in the linear concentration range of 1.0-500.0µgL with a limit of detection as low as 0.21µgL and relative standard deviation less than 2.5 (%). The results of human urine and blood plasma analysis showed that the method is a good candidate for biological sample analysis purposes.

摘要

在这项研究中,开发了一种灵敏、简单和快速的超声辅助分散微固相萃取(USAD-µSPE),使用合成的核壳型磁性介孔纳米复合材料(FeO@nSiO@mSiO-NH)作为高效吸附剂,用于生物样品中氧氟沙星(OFL)的预浓缩和荧光分光光度法测定。通过傅里叶变换红外光谱(FT-IR)、透射电子显微镜(TEM)、振动样品磁强计(VSM)、能量色散 X 射线(EDX)光谱、热重分析(TGA)和 Brunauer-Emmett-Teller(BET)分析对合成的吸附剂进行了表征。将这种磁性纳米复合材料作为一种灵敏的固相,用于痕量氧氟沙星的去除、预浓缩和荧光分光光度定量分析。研究并优化了各种变量(包括 pH 值、吸附剂用量、解吸溶剂性质和超声时间)对本方法响应的影响。结果表明,采用所提出的方法,OFL 的线性浓度范围为 1.0-500.0µgL,检测限低至 0.21µgL,相对标准偏差小于 2.5(%)。人尿和血浆分析的结果表明,该方法是生物样品分析的良好候选方法。

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