Abstract

A simple and efficient pH-mediated dispersive solid phase extraction (dSPE) based on terbium doped titanium dioxide nanoparticles (TiO₂-Tb NPs) combined with high performance liquid chromatography (HPLC) has been firstly developed for the determination of quinolones (QNs) in various biological samples. The adsorption kinetics and isotherms were investigated to indicate that the kinetic and equilibrium adsorption were well-described by pseudo-second order kinetic and Henry, Langmuir isotherm model, respectively. The parameters influencing the extraction performance were systematically investigated. The QNs are transferred into TiO₂-Tb NPs in the first step at pH = 6.0 and eluted into acidic aqueous phase at pH = 2.5 in the second step. Under the optimum extraction and determination conditions, a linearity range with the coefficient of determination (R²) from 0.9977 to 0.9991 were obtained in a range of 10–10,000 ng mL⁻¹. The limits of detection (LODs) based on a signal-to-noise ratio of 3 were 3.3 ng mL⁻¹. The recoveries of the three QNs in human urine, rabbit plasma and serum samples ranged from 69.3% to 117.6%, with standard deviations ranging from 2.4% to 9.9%. Therefore, this pH-mediated dSPE-HPLC method exhibited the advantages of remarkable sensitivity, ease of operation, rapidity, low cost and environmental friendliness.

摘要

首次开发了一种基于铽掺杂二氧化钛纳米粒子（TiO ₂ -Tb NPs）的简单高效的pH介导分散固相萃取（dSPE）结合高效液相色谱（HPLC），用于测定喹诺酮类药物（QNs）。各种生物样品。研究了吸附动力学和等温线，表明动力学和平衡吸附分别由准二级动力学和亨利，朗缪尔等温线模型很好地描述。系统地研究了影响萃取性能的参数。QN 被转移到 TiO _2中-Tb NPs 在 pH = 6.0 的第一步中，并在第二步中在 pH = 2.5 时洗脱到酸性水相中。在最佳提取和测定条件下，在10-10,000 ng mL ^-1范围内，线性范围为0.9977～0.9991 ，决定系数( R ² ) 。基于信噪比为 3 的检测限 (LOD) 为 3.3 ng mL ^-1。人尿、兔血浆和血清样品中三种 QNs 的回收率范围为 69.3% 至 117.6%，标准偏差范围为 2.4% 至 9.9%。因此，该pH介导的dSPE-HPLC方法具有灵敏度高、操作简便、快速、成本低、环境友好等优点。