石墨烯-氧化物/金属杂化材料对动物源食品中抗生素残留高选择性富集分离的机理及应用研究

In this study, new functional graphene-oxide/metal (e.g. ZnO, CuO,Al2O3, Ag,Au) hydrid materials are designed and constructed based on their characteristics of high surface area and active sites. The performance of these products on selective enrichment of antibiotics (abbreviated as target molecular)is explored. Their good performance combined chromatography technique can be expected to enrich and detect trace antibiotics remaining in complex samples(such as aquatic organisms, milk and eggs). Their shapes, sizes and relative properties are characterized by many approaches such as TEM, SEM, , XRD, FT-IR. The mechanism of adsorption/desorption of antibiotics on the as-prepared products are in situ investigated in some detail, through Raman, FT-IR. In addition, stability, dispersity, repeatability, and regeneration are also explored for these products. The products will provide a facile, low-cost and high efficient method for the analysis of antiobitic residues in foodstuffs of animal origins.The aims of this study are to develop new solid phase extraction adsorbent based on the modern nano-materials technology, and to realize the efficient enrichment and sensitive detection of trace components in complex samples.

本项目拟将石墨烯、氧化物（如ZnO、CuO、Al2O3等）和金属纳米粒子（如Au、Ag等）高比表面积、高活性位点等特点相结合，设计、合成新型功能石墨烯-氧化物/金属杂化材料，探索其对抗生素（靶向分子）的选择性吸附、萃取性能，结合色谱分析技术，实现动物源食品（如水生生物、牛奶、鸡蛋等）中痕量靶向分子的高效富集和灵敏检测。利用TEM、SEM、XRD、FT-IR、UV-Vis等技术对所制备材料的形貌、尺度及性能等进行表征。采用激光拉曼、FT-IR等原位表征技术研究靶向分子在功能石墨烯-氧化物/金属杂化材料表面的吸附/解吸，探讨靶向分子在其表面的吸附保留机理。考察所制备材料的稳定性、分散性、重复性及再生性，建立便捷、经济及高效的分析方法，用于动物源食品中抗生素的残留分析。本项目利用现代纳米材料技术发展新型固相萃取吸附剂，实现复杂样品中痕量组分的高效富集和灵敏检测。

本课题主要针对牛奶、蜂蜜等食品中的磺胺类抗生素残留，成功制备了几种石墨烯复合材料（CoFe2O4 –石墨烯，石墨烯-Fe3O4，石墨烯-壳聚糖），并利用TEM、SEM、XRD、FT-IR、UV-Vis 等技术对所制备材料的形貌、尺度及性能等进行了表征；将所制备的功能材料用于磁性固相萃取或新型固相萃取的吸附剂，对影响萃取效率的因素如样品溶液pH、吸附剂用量、洗脱剂类型、萃取时间等进行了详细优化；将所建立的样品前处理方法对牛奶、蜂蜜等复杂样品中的痕量磺胺类抗生素残留进行预富集，结合液相色谱、毛细管电泳等技术建立了复杂样品中痕量靶向分子残留分析的新方法和新技术；初步探讨了新型吸附剂对靶向分子的吸附/解吸机理。此外，利用实验室常见的移液器枪头，设计组装出一种微型化固相萃取装置（m-SASPE），用于样品的前处理操作。此装置大大减少了萃取过程中吸附剂和有机试剂的使用量，而且操作简便快速，绿色环保、成本低，避免了传统SPE装置中商业化萃取小柱的浪费和过柱耗时、过程繁冗的问题。此外，相关的研究成果发表SCI论文9篇，培养研究生5名，参加学术交流6人次。