The analysis of hierarchical structure of mesoporous silica material with template of cetyltrimethylammonium bromide (CTAB) with co-surfactants of tetramethylammonium hydroxide (TMAOH) and Triton X-100 was conducted by using the technique of small angle scattering (SAS) using neutron (SANS) and X-ray (SAXS). The analysis was supported by the data of nitrogen absorption and electron microscopy. The analysis showed that the concentration of CTAB affected the characteristics and pore structures of particles. The increase of co-surfactant concentrations tended to form particles that were more uniform in size and more regular in the shape of the sphere. The results of SAS analysis showed that the morphology, shape, and size of the large particles were arranged by smaller (primary or secondary) particles that had pores. The variation of surfactant templates had influenced the formation of pore structure. For CTAB-TMAOH, it had resembled MCM-41 type which has a hexagonal structure, whereas for CTAB-Triton X-100, it would have resembled MCM-48 type which has a cubic structure. The particles that have a high surface area which resembled pore structure MCM-41 has been able to set up by using 0.25 M of CTAB with 0.040 M of TMAOH. Moreover, the particles which resembled pore structure MCM-48 were able to set up by using 0.03 M of Triton X-100 with 0.4 M of CTAB. The analysis of SANS data that was supported by electron microscopy results is entirely showing a complete information of the particles formed by each template. Whereas SAXS analysis that supported by nitrogen adsorption method is fully confirming the information of pore characteristics.
There are challenges related to cancer treatment, namely, targeting and biocompatibility associated with a drug vehicle. This research aims to prepare a theranostic cancer vehicle based on porous silica nanoparticles (PSN) with controllable nanoparticle size, supporting targeting properties, and biocompatible. The synthesis method combined the Stöber process and liquid crystal templating using a dispersant and pore expander. Triethanolamine (TEA) and Pluronic F-127 were combined as a steric stabilizer and dispersing agent, while n -hexane was used as a pore expander. The amine functionalization was carried out using the 3-aminopropyl-triethoxysilane solution. Furthermore, radiolabeling of PSN using Iodine-131 and iodogen as oxidizing agents was carried out. The results showed that the best achievable PSN size was 100–150 nm with a polydispersity index of 0.24 using TEA-Pluronic F-127. The functionalization results did not significantly affect the radioiodination result. Radiochemical purity (RCP) values up to 95% were obtained in the radioiodination, while the labeled compounds were relatively stable with 12 mCi radioactivity, indicating the absence of radiolysis. The synthesized PSN was not toxic to normal cell samples up to a concentration of 150 μg/mL for PSN and 170 μg/mL for PSN-NH 2 . The cellular uptake testing results of the PSN- 131 I in cancer cell samples showed promising uptake ability.
Ordered pores structure analysis of mesoporous silica materials using a template of poly(ethylene oxyde)-poly(propylene oxide)-poly(ethylene oxide), PEO-PPO-PEO, triblock copolymer or Pluronics in numerous synthesis conditions has been conducted. Two different length of hydrophilic chain of Pluronics, i.e., P123 (EO 20 PO 70 EO 20) and F127 (EO 106 PO 70 EO 106), produced two different fine pore structures, which were basically hexagonal and cubic. A highly ordered pore structure, confirming with many Bragg peaks, was clearly obtained with the lattice parameters in nanometer scale from analyzing the synchrotron small angle X-ray scattering (SAXS) data. Meanwhile, the surface area and pores size of mesoporous silica determined by nitrogen absorption clearly support the analysis of SAXS data, presenting a complete information of pore order characteristics. This paper shows how the synthesis parameters, such as length of hydrophilic chains, silica precursor concentration, Al:Si ratio and synthesis methods, are related to the structure and order of the pores formed. The SAXS patterns show that the pore order increases with increasing concentration of sodium silicate and decreases with longer sonication time.
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