College of Chemistry and Molecular Sciences, Wuhan University, Wuhan 430072, Hubei Province, P. R. China.
Analyst. 2023 Aug 21;148(17):4203-4212. doi: 10.1039/d3an01060k.
Extraction and determination of trace hazardous components from complex matrices continue to attract public attention. In this work, magnetic porous carbon (MPC) was prepared for efficient magnetic solid phase extraction (MSPE) of fluoroquinolone (FQ) antibiotics in food and water samples. To prepare the MPC, an Fe-based metal-organic framework (MIL-101(Fe)) was grown on a network of graphene oxide and multi-walled carbon nanotubes through a hydrothermal method, and then a carbonization process under a nitrogen atmosphere was carried out to obtain the MPC with high specific surface area and good magnetism. Four target FQs including ciprofloxacin (CIP), enrofloxacin (ENO), lomefloxacin (LOM) and ofloxacin (OFX) were enriched using the as-prepared MPC and determined by coupled high-performance liquid chromatography. Under the optimal conditions, the established MSPE-HPLC-UV detection method exhibited a linear range of 0.5-800 μg L and detection limits of 0.11-0.18 μg L with relative standard deviations (RSDs) of 0.5-4.8%. When applied in the determination of the above four FQs in real samples such as lake water, milk and pork, good recoveries between 85.2 and 103.7% were obtained, and the RSDs were less than 4.8%. This work indicates that the MPC material can be a good adsorption material and has good application prospects in antibiotics enrichment and/or removal from complex samples.
从复杂基质中提取和测定痕量有害成分仍然引起公众关注。在这项工作中,制备了磁性多孔碳(MPC),用于食品和水样中氟喹诺酮(FQ)抗生素的高效磁固相萃取(MSPE)。为了制备 MPC,通过水热法在氧化石墨烯和多壁碳纳米管的网络上生长了基于 Fe 的金属有机骨架(MIL-101(Fe)),然后在氮气气氛下进行碳化过程,得到具有高比表面积和良好磁性的 MPC。使用所制备的 MPC 对四种目标 FQ(环丙沙星(CIP)、恩诺沙星(ENO)、洛美沙星(LOM)和氧氟沙星(OFX))进行了富集,并通过高效液相色谱法进行了测定。在最佳条件下,建立的 MSPE-HPLC-UV 检测方法在 0.5-800 μg L 的线性范围内具有良好的线性关系,检测限为 0.11-0.18 μg L,相对标准偏差(RSD)为 0.5-4.8%。当将该方法应用于湖水、牛奶和猪肉等实际样品中四种 FQ 的测定时,可获得 85.2-103.7%的良好回收率,且 RSD 小于 4.8%。这项工作表明,MPC 材料可以作为一种良好的吸附材料,在从复杂样品中富集和/或去除抗生素方面具有良好的应用前景。