Department of Analytical Chemistry, Institute of Chemistry, Saint Petersburg State University, 7/9 Universitetskaya nab., St. Petersburg, 199034, Russia.
Department of Analytical Chemistry, Institute of Chemistry, Saint Petersburg State University, 7/9 Universitetskaya nab., St. Petersburg, 199034, Russia.
Talanta. 2020 Jul 1;214:120861. doi: 10.1016/j.talanta.2020.120861. Epub 2020 Feb 24.
A procedure for separation and preconcentration of tetracyclines from human serum samples involving magnetic dispersive micro-solid phase extraction was proposed. The extraction efficiency of different tetracyclines was improved with the use of the surfactant coated FeO magnetic nanoparticles. Sorption mechanism was presented, and the potential use of magnetic FeO nanoparticles coated with different surfactants for tetracyclines adsorption was demonstrated for the first time. The procedure involved nanoparticle floating in a liquid sample phase for analyte extraction followed by elution and determination by high performance liquid chromatography with diode array detection. Influence of the main involved parameters was studied, the system was dimensioned accordingly. The analytical curves were linear in the ranges of 0.25-10 mg L for tetracycline and 0.10-10 mg L for oxytetracycline or doxycycline. Limits of detection were estimated (IUPAC, 3 concept) as 0.08 mg L for tetracycline, and 0.03 mg L for oxytetracycline or doxycycline. The proposed procedure proved to be fast (10 min), simple (two stages), inexpensive (10 mg of nanoparticles) and was applied to human serum samples. Unlike previously synthesized nanoparticles for tetracyclines separation, the surfactant-coated FeO nanoparticles can be easily prepared with widely available and low-cost reagents. Moreover, elution of the analytes was accomplished in absence of organic solvents by an aqueous chelating agent solution.
提出了一种从人血清样品中分离和预浓缩四环素的方法,涉及磁性分散微固相萃取。使用表面活性剂包覆的 FeO 磁性纳米粒子可以提高不同四环素的萃取效率。提出了吸附机理,并首次证明了不同表面活性剂包覆的磁性 FeO 纳米粒子对四环素吸附的潜在用途。该方法包括纳米粒子在液体样品相中漂浮以萃取分析物,然后通过高效液相色谱法与二极管阵列检测进行洗脱和测定。研究了主要涉及参数的影响,并相应地对系统进行了尺寸设计。分析曲线在四环素的 0.25-10 mg L 和土霉素或强力霉素的 0.10-10 mg L 范围内呈线性。检测限(IUPAC,3 概念)估计为四环素为 0.08 mg L,土霉素或强力霉素为 0.03 mg L。该方法快速(10 min)、简单(两步)、廉价(10 mg 纳米粒子),并应用于人血清样品。与以前用于四环素分离的合成纳米粒子不同,表面活性剂包覆的 FeO 纳米粒子可以用广泛可用且低成本的试剂轻松制备。此外,通过含有螯合剂的水溶液可以在没有有机溶剂的情况下完成分析物的洗脱。