Abstract: Layered super-hydrophilic Ti—Cu-MOFs and a preparation method and use thereof provided, which relates to the technical field of composite materials. According to the present application, copper ions and titanium ions are used as bimetallic centers to have a coordination reaction with rigid aromatic amine ligands, and layered super-hydrophilic Ti—Cu-MOFs with a lamellar structure is efficiently synthesized. Compared with the prior technology, the preparation method of the present application is simple, and the morphology and structure are controllable; the surface of the prepared layered super-hydrophilic Ti—Cu-MOFs are rich in hydroxyl groups, and have high adsorption capacity for phospholipid co-extracts in clinical biological samples, and thus can be used for the analysis of phenothiazine drugs and metabolites thereof in biological samples and realize one-step separation and purification, thus greatly improving the pretreatment efficiency of clinical biological samples and shortening the analysis time.