Key Laboratory of the Ministry of Education for Coastal and Wetland Ecosystems, Fujian Provincial Key Laboratory for Coastal Ecology and Environmental Studies, College of the Environment and Ecology, Xiamen University, Xiamen, 361005, China.
Department of Materials Science and Engineering, College of Materials, Xiamen University, Xiamen, Fujian, 361005, China.
J Chromatogr A. 2019 Sep 13;1601:86-94. doi: 10.1016/j.chroma.2019.06.020. Epub 2019 Jun 10.
Effective extraction is an indispensable procedure for the sensitive analysis of fluoroquinolones (FQs) in complex samples. According to the molecular properties of FQs, a new highly fluorinated and boron-rich adsorbent (FBA) was synthesized and employed as the extraction phase of magnetic solid-phase extraction (MSPE). Results revealed that the prepared FBA displayed satisfactory extraction capability for FQs through fluorophilic and B-N coordination interactions. Besides, the synthesized FBA also exhibited strong magnetic responsiveness and good life-span. Under the most favorable conditions, the FBA/MSPE was combined with high-performance liquid chromatography with diode array detection (HPLC-DAD) to sensitively quantify trace levels of FQs in environmental water and milk samples. The developed approach showed good linearity within the studied concentration range, satisfactory precision and low limits of detection (0.0049-0.016 μg/L for water sample and 0.010-0.046 μg/kg for milk sample). In the analysis of target FQs in real samples, the recoveries of different fortified concentrations were in the ranges of 80.1-120% and 78.9-119% for water and milk samples, respectively. The relative standard deviations for reproducibility were all below 11%. The results well evidence that the introduced FBA/MSPE is a promising extraction technology for FQs, and the established FBA/MSPE-HPLC/DAD approach is suitable to measure low concentrations of FQs in water and milk samples.
有效提取是对复杂样品中的氟喹诺酮类（FQs）进行灵敏分析的不可或缺的程序。根据 FQs 的分子特性，合成了一种新型高度氟化和富硼吸附剂（FBA），并将其用作磁性固相萃取（MSPE）的萃取相。结果表明，所制备的 FBA 通过亲氟和 B-N 配位相互作用对 FQs 表现出令人满意的萃取能力。此外，合成的 FBA 还表现出强的磁响应性和良好的寿命。在最有利的条件下，将 FBA/MSPE 与高效液相色谱-二极管阵列检测（HPLC-DAD）相结合，用于灵敏地定量环境水样和牛奶样品中的痕量 FQs。所开发的方法在研究的浓度范围内表现出良好的线性关系、令人满意的精密度和低检测限（水样为 0.0049-0.016μg/L，牛奶样为 0.010-0.046μg/kg）。在实际样品中目标 FQs 的分析中，不同加标浓度的回收率在水和牛奶样品中分别为 80.1-120%和 78.9-119%。重现性的相对标准偏差均低于 11%。结果充分证明，所引入的 FBA/MSPE 是一种很有前途的 FQs 萃取技术，建立的 FBA/MSPE-HPLC/DAD 方法适用于测量水样和牛奶样品中低浓度的 FQs。
