基于PDA修饰磁性纳米材料富集尿液氯霉素、甲砜霉素和氟甲砜霉素的研究

Study on Enrichment of Chloramphenicol, Thiamphenicol and Thiamphenicol in Urine Based on PDA-Modified Magnetic Nanomaterials

摘要: 针对人体抗生素暴露问题，开发了基于Fe₃O₄@PDA磁性纳米材料实现对尿液中3种氯霉素类抗生素(氯霉素、甲砜霉素和氟甲砜霉素)的富集及其生物监测。采取SEM和TF-IR技术表征Fe₃O₄@PDA磁性纳米材料的形貌和结构功能，结果表明制备的PDA通过Fe-O-C化学键连接到磁性Fe₃O₄纳米颗粒表面，修饰于Fe₃O₄外层。磁性强度实验表明制备的Fe₃O₄@PDA材料在磁场中具有高的磁反应性。通过对影响因素的优化，在Fe₃O₄@PDA用量为20 mg，溶液pH为7，吸附时间为15 min，10 mL 5% (v/v)氨水甲醇溶液作为洗脱剂，超声洗脱时间10 min时，3种目标物的平均回收率在90%以上，且检出限和定量限分别为0.10~0.16 μg/L和0.30~0.47 μg/L。利用该方法对实际儿童尿液样本进行检测，3种物质的加标回收率为95.95%~117.64%。该方法可有效地检测出尿液中3种氯霉素类抗生素，其在实际尿液样本检测中具有较高的应用前景。

Abstract: Considering the antibiotic exposure in humans, a magnetic solid-phase extraction technology based on Fe₃O₄@PDA magnetic nanomaterials was developed to enrich three kinds of chloramphenicol antibiotics (chloramphenicol, thiamphenicol, and florfenicol) in urine samples for biomonitoring. Firstly, the morphology and structural properties of Fe₃O₄@PDA magnetic nanomaterials were characterized by SEM and TF-IR techniques, and the results showed that the prepared PDA nanoparticles was connected to the surface of magnetic Fe₃O₄ nanoparticles through Fe-O-C chemical bonds, and modified on the outer layer of Fe₃O₄. In addition, magnetic strength experiments showed that the prepared Fe₃O₄@PDA material has high magnetic reactivity in a magnetic field. Under the optimal conditions as follows: 20 mg of Fe₃O₄@PDA were added, pH of the solution was 7, the adsorption time was 15 min, 10 mL of 5% (v/v) ammonia methanol solution used as the eluent, and the ultrasonic elution time of 10 min, the average recovery rate of the target compound was above 90%. The limit of detection and quantification was in the range of 0.10~0.16 μg/L and 0.30~0.47 μg/L, respectively. When applied to detect actual urine samples, the recovery rates of the method ranged from 95.95% to 117.64% for three targeted chloramphenicols. It suggested the proposed method can effectively enrich chloramphenicol antibiotics in urine, thereby having a great potential for application in the biomonitoring of actual urine samples.