Institute of Chemistry, Saint-Petersburg University St.Petersburg State University, SPbSU, SPbU, 7/9 Universitetskayanab., St. Petersburg 199034, Russia.
Institute of Chemistry, Saint-Petersburg University St.Petersburg State University, SPbSU, SPbU, 7/9 Universitetskayanab., St. Petersburg 199034, Russia.
Anal Chim Acta. 2018 Feb 25;1001:59-69. doi: 10.1016/j.aca.2017.11.065. Epub 2017 Dec 8.
An automated magnetic dispersive micro-solid phase extraction procedure in a fluidized reactor was developed for the determination of fluoroquinolone antimicrobial drugs (fleroxacin, norfloxacin and ofloxacin) in meat-based baby food samples. A stepwise injection system was successfully combined with afluidized reactorand applied for the magnetic dispersive micro-solid phase extraction procedure automation. The developed automated procedure involved injection of the sample solution into the fluidized reactor followed by the on-line separation of the analytes from the sample matrix based on fluidized beds strategy using magnetic nanoparticles, elution and determination of the analytes using a high performance liquid chromatography system with fluorescence detection. The floating of the magnetic nanoparticles in a liquid sample phase was accomplished by air-bubbling. In the developed method Zr-Fe-C magnetic nanoparticles were used as an efficient sorbent for the determination of fleroxacin, norfloxacin and ofloxacin. Under the optimal conditions, the calibration graphs were linear over the concentration ranges of 10-1000 μg L for fleroxacin (R = 0.996), 5-1000 μg Lfor norfloxacin (R = 0.998) and ofloxacin (R = 0.998). The limits of detection, calculated from the blank tests based on 3σ, were 3.0 μg Lforfleroxacin, 1.5 μg Lfor norfloxacin and ofloxacin. The limits of quantification, calculated from the blank tests based on 10σ, were 10 μg L forfleroxacin, 5 μg Lfor norfloxacin and ofloxacin. The method was applied for the determination of fluoroquinolonesin meat-based baby food samples and the results were compared with those obtained by the reference method. The recovery values for all analytes were within of 86-122% range.
一种在流化床反应器中自动磁分散微固相萃取程序被开发用于测定肉类婴儿食品样品中的氟喹诺酮类抗菌药物（氟沙星、诺氟沙星和氧氟沙星）。逐步注射系统与流化床反应器成功结合，用于自动化磁分散微固相萃取程序。所开发的自动程序包括将样品溶液注入流化床反应器，然后根据流化床策略在线分离样品基质中的分析物，使用磁性纳米粒子进行洗脱，并用荧光检测的高效液相色谱系统测定分析物。通过气泡将磁性纳米粒子浮在液体样品相中。在开发的方法中，Zr-Fe-C 磁性纳米粒子被用作测定氟沙星、诺氟沙星和氧氟沙星的有效吸附剂。在最佳条件下，氟沙星的校准曲线在 10-1000μg L 的浓度范围内呈线性（R=0.996），诺氟沙星（R=0.998）和氧氟沙星（R=0.998）的浓度范围为 5-1000μg L。基于 3σ 从空白试验计算得出的检测限，氟沙星为 3.0μg L，诺氟沙星和氧氟沙星为 1.5μg L。基于 10σ 从空白试验计算得出的定量限，氟沙星为 10μg L，诺氟沙星和氧氟沙星为 5μg L。该方法用于测定肉类婴儿食品样品中的氟喹诺酮类，将结果与参考方法进行比较。所有分析物的回收率均在 86-122%范围内。
