Yu Zhendong, Xu Tiantian, Lin Shumin, Liang Shuxuan
Key Laboratory of Analytical Science and Technology of Hebei Province, College of Chemistry and Materials Science, Hebei University, Baoding 071002, China.
College of Public Health, Hebei University, Baoding 071002, China.
Foods. 2024 Aug 12;13(16):2511. doi: 10.3390/foods13162511.
In this study, a magnetic porous polymer composite with both hydrophilic and hydrophobic groups was synthesized for magnetic solid phase extraction (MSPE) of milk substrates. Optimization was conducted on various parameters, including adsorption dose, solution pH, adsorption time, and some elution conditions. Coupled with a high-performance liquid chromatography fluorescence detector, a novel MSPE method for determination of norfloxacin (NFX), ciprofloxacin (CIP), and enrofloxacin (ENR) in milk was developed based on magnetic metal organic framework polystyrene polymer (FeO@MOF@PLS) as adsorbent. The FeO@MOF@PLS exhibited significantly improved adsorption performance compared to MOF and PLS. Under optimized experimental conditions, the method exhibited good linearity for the three fluoroquinolones (FQs) in the range of 0.5-1000 μg/kg, with limit of detections (LODs) ranging from 0.21 to 1.33 μg/kg, and limit of quantitations (LOQs) from 0.71 to 4.42 μg/kg. The relative standard deviation (RSD) for the three FQs were 3.4-8.8%. The recoveries of three FQs in milk samples ranged from 84.2% to 106.2%. This method was successfully applied to the detection of three FQs in 20 types of milk, demonstrating its simplicity, speed, and effectiveness in analyte enrichment and separation. The method presented advantages in adsorbent dosage, adsorption time, LODs, and LOQs, making it valuable for the analysis and detection of FQs in milk.
在本研究中，合成了一种具有亲水和疏水基团的磁性多孔聚合物复合材料，用于牛奶基质的磁性固相萃取（MSPE）。对各种参数进行了优化，包括吸附剂量、溶液pH值、吸附时间和一些洗脱条件。结合高效液相色谱荧光检测器，基于磁性金属有机骨架聚苯乙烯聚合物（FeO@MOF@PLS）作为吸附剂，开发了一种测定牛奶中诺氟沙星（NFX）、环丙沙星（CIP）和恩诺沙星（ENR）的新型MSPE方法。与MOF和PLS相比，FeO@MOF@PLS表现出显著提高的吸附性能。在优化的实验条件下，该方法对三种氟喹诺酮类药物（FQs）在0.5 - 1000 μg/kg范围内具有良好的线性，检测限（LODs）为0.21至1.33 μg/kg，定量限（LOQs）为0.71至4.42 μg/kg。三种FQs的相对标准偏差（RSD）为3.4 - 8.8%。牛奶样品中三种FQs的回收率为84.2%至106.2%。该方法成功应用于20种牛奶中三种FQs的检测，证明了其在分析物富集和分离方面的简便性、快速性和有效性。该方法在吸附剂用量、吸附时间、LODs和LOQs方面具有优势，对牛奶中FQs的分析检测具有重要价值。
