Laboratory of Pathogenic Biology and Immunology, School of Basic Medicine and Life Science, Hainan Medical University, Haikou, China.
Department of Environmental Science, School of Tropical Medicine, Hainan Medical University, Haikou, China.
J Environ Sci Health A Tox Hazard Subst Environ Eng. 2022;57(8):656-666. doi: 10.1080/10934529.2022.2101340. Epub 2022 Jul 26.
A simple and efficient pH-mediated dispersive solid phase extraction (dSPE) based on terbium doped titanium dioxide nanoparticles (TiO-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 TiO-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 () from 0.9977 to 0.9991 were obtained in a range of 10-10,000 ng mL. The limits of detection (LODs) based on a signal-to-noise ratio of 3 were 3.3 ng mL. 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.
基于掺铽二氧化钛纳米粒子（TiO-Tb NPs）的 pH 介导分散固相萃取（dSPE）与高效液相色谱（HPLC）相结合，首次建立了一种简单高效的测定各种生物样品中喹诺酮类（QNs）的方法。研究了吸附动力学和吸附等温线，结果表明，准二级动力学和亨利、朗缪尔等温模型能够很好地描述动力学和平衡吸附。系统研究了影响萃取性能的参数。在第一步中，将 QNs 在 pH = 6.0 下转移到 TiO-Tb NPs 上，在第二步中在 pH = 2.5 下将其洗脱到酸性水相中。在最佳萃取和测定条件下，在 10-10,000ng mL 的范围内，得到了线性范围，相关系数（r）为 0.9977-0.9991。基于信噪比为 3 的检出限（LOD）为 3.3ng mL。在人尿、兔血浆和血清样品中，三种 QNs 的回收率为 69.3%-117.6%，标准偏差为 2.4%-9.9%。因此，这种 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。
