This paper describes a method for preparing silica-coated silver iodide (AgI/SiO2) particles and immobilizing proteins on the AgI/SiO2 particles. Colloid solution of AgI particles was prepared by mixing AgClO4 aqueous solution and KI aqueous solution. Silica-coating of the AgI particles was performed by adding 3-mercaptopropyltrimethoxysilane, tetraethylorthosilicate/ethanol solution and NaOH aqueous solution successively to the AgI colloid solution. TEM observation revealed that the AgI nanoparticles were coated with uniform silica shell. The AgI/SiO2 particles were surface-modified with 3-aminopropyltrimethoxysilane and succinic anhydride. It was confirmed by XPS measurement that amino group or carboxyl group was introduced onto the AgI/SiO2 particles. Protein-immobilization was performed in aqueous solution with bovine serum albumin (BSA) in the presence of the surface-modified AgI/SiO2 particles. UV-VIS absorption spectroscopy revealed that the BSA was adsorbed on the surface-modified particles.
Methods for high concentration silica-coated silver iodide (AgI/SiO2) particles, which could be practically used as X-ray contrast agent, were examined. The first was a single-step method, which was to prepare AgI nanoparticles at an AgI concentration of 5 x 10(-3) M and coat the AgI nanoparticles with silica shell by a Stöber method. The second was a multiple-step method, which was to repeat a step for preparing a AgI/SiO2 particle colloid solution with 10(-3) M AgI 5 times for adjusting a final AgI concentration to 5 x 10(-3) M. In the two methods, dominant particle aggregation took place, though core-shell particles were also produced. The third was a salting-out method, which was to salt out AgI/SiO2 particles in their colloid solution prepared at an AgI concentration of 10(-3) M, remove supernatant by decantation, and redisperse the particles in a fresh solvent. Consequently, AgI/SiO2 particles with an AgI concentration as high as 0.05 M were successfully prepared with the salting-out method, and their core-shell structure was not damaged during the salting-out.
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