氧化石墨烯—纳米粒子三维复合材料固相微萃取纤维的制备及在头孢抗生素残留分析中的应用研究

抗生素污染日益严重，有必要对其建立简单、高效的固相微萃取富集检测新技术。以头孢抗生素为例，因其结构中通常含有芳基、酰胺基、羧基等基团，所以具有大比表面积、丰富π电子以及极性基团的氧化石墨烯可作为萃取涂层的优选材料。然而，在常规的氧化石墨烯涂层中，强烈的分子间作用力导致氧化石墨烯层与层之间紧密叠连，使被分析物难以接触到内层氧化石墨烯，而仅与外层氧化石墨烯产生有效吸附，限制了其大比表面积优势的发挥，为此，拟在2维氧化石墨烯的基础上引入0维或1维的纳米粒子，以产生层间空隙，并通过层层自组装技术制备出具有3维结构的氧化石墨烯—纳米粒子复合涂层，使被分析物与内、外层氧化石墨烯均有充分接触，从而提高萃取效率；此外，拟在3维复合涂层的基础上键合阴、阳离子等官能团，调节萃取纤维的选择性；与液相色谱-质谱联用，以头孢抗生素为被分析物，对氧化石墨烯—纳米粒子3维复合材料固相微萃取纤维进行性能考察和应用研究。

The pollution from antibiotics becomes more and more serious. It is necessary to establish new solid phase microextraction techniques for simple and high efficient antibiotics analysis. Take cephalosporin antibiotics for example, because its structure usually has aromatic, acrylamino and carboxyl groups etc., graphene oxide with large specific surface area, abundant π electrons and polar groups is suitable for the coating material. However, in the normal graphene oxide coating, the neighboring graphene oxide sheets are overlapped closely due to the strong intermolecular forces, as a result, the analytes are hard to contact with the inner graphene oxide sheets but only are absorbed by the outer graphene oxide sheets, as a result, the superiority of large specific surface area is restricted. To solve the above problem, zero-dimensional or one-dimensional nanoparticles are to be grafted onto the two-dimensional graphene oxide to get a three-dimensional graphene oxide-nanoparticle complex coating by layer by layer self-assembly method, which is expected to make the analytes interact not only with the outer but also with the inner graphene oxide sheets adequately through the interlayer gaps and to enhance the extraction ability. Moreover, the anionic or cationic groups are to be bonded to the three-dimensional complex to improve the extraction selectivity. Combined with HPLC-MS, the extraction ability of the 3-dimensional graphene oxide-nanoparticle complex fiber and its application on residual analysis of cephalosporin antibiotics are studied.