Layer Double Hydroxides (LDH) and Metal-Organic Frameworks (MOF) are excellent adsorbents due to their physicochemical properties. The new LDH-MOF hybrid materials created by combining these materials will be used for pesticide determination in this project. The use of new nanocomposites, which will be obtained by the synthesis of these two materials, which allow different modifications, in the determination of pesticides, will increase their application potential in the determination of pollutants such as nanopesticides, organic-based drugs, dyes and polyaromatic hydrocarbons, inorganic-based heavy metals and radioactive substances. In this context, this hybrid material has a larger surface area and higher adsorption capacity compared to adsorbents such as carbon-based (MWCNT, activated carbon, carbon dots, graphene derivatives) materials, silica gels, spinel metal oxides, molecularly imprinted polymers, polymer resins in the literature. It is aimed to contribute to the literature within the framework of food safety by enabling sensitive determinations of pesticides by making use of their superior properties such as being selectively optimized against the relevant analyte/analytes depending on their chemical structures that allow their modification. Since studies on the determination of pesticides with LDH-MOF structures are very limited, their applications in food and water matrices are quite lacking. Since synthesizing new adsorbents for more precise determination of pesticides remains important, primarily modified new LDH and MOF structures will be synthesized during this project, and then new LDH-MOF nanocomposites will be synthesized with different combinations. The characterization of the synthesized materials will be done with SEM-EDS, XPS, FTIR, TGA, XRD, VSM, BET and TGA devices. Liquid chromatography systems will be used in the validation of the methods, optimization studies and sample applications. The properties of new adsorbents for pesticide analysis in food and water samples will be revealed by synthesizing modified and original structures of LDH-MOF nanocomposites, for which sample application studies are very few. With the use of these hybrid structures as adsorbent in the determination of pesticides, the specificity of the project will be increased, and the determination of pesticides and other organic and inorganic pollutants that have even trace toxic effects on the entire ecosystem with LDH-MOF hybrid materials and their use in pesticide transport systems will be opened.