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Graphical abstract Figure. No Caption available. HighlightsNovel methodology for the development of magnetic core mesoporous silica.Radiolabeling process of monoclonal antibodies with 99mTc.Efficient methodology to calculate the Incorporation of monoclonal antibodies into nanoparticles by radiolabeling process. Abstract The use of monoclonal antibodies (Mab) in the current medicine is increasing. Antibody‐drug conjugates (ADCs) represents an increasingly and important modality for treating several types of cancer. In this area, the use of Mab associated with nanoparticles is a valuable strategy. However, the methodology used to calculate the Mab entrapment, efficiency and content is extremely expensive. In this study we developed and tested a novel very simple one‐step methodology to calculate monoclonal antibody entrapment in mesoporous silica (with magnetic core) nanoparticles using the radiolabeling process as primary methodology. The magnetic core mesoporous silica were successfully developed and characterised. The PXRD analysis at high angles confirmed the presence of magnetic cores in the structures and transmission electron microscopy allowed to determine structures size (58.9 ± 8.1 nm). From the isotherm curve, a specific surface area of 872 m2/g was estimated along with a pore volume of 0.85 cm3/g and an average pore diameter of 3.15 nm. The radiolabeling process to proceed the indirect determination were well‐done. Trastuzumab were successfully labeled (>97%) with Tc‐99m generating a clear suspension. Besides, almost all the Tc‐99m used (labeling the trastuzumab) remained trapped in the surface of the mesoporous silica for a period as long as 8 h. The indirect methodology demonstrated a high entrapment in magnetic core mesoporous silica surface of Tc‐99m‐traztuzumab. The results confirmed the potential use from the indirect entrapment efficiency methodology using the radiolabeling process, as a one‐step, easy and cheap methodology.