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Water-dispersible TiO2 nanoparticles via a biphasic solvothermal reaction method.

ABSTRACT: A biphasic solvothermal reaction method has been used for the synthesis of TiO2 nanoparticles (NPs). In this method, hydrolysis and nucleation occur at the interface of organic phase (titanium (IV) n-propoxide and stearic acid dissolved in toluene) and water phase (tert-butylamine dissolved in water) resulting in the nucleation of the stearic acid-capped TiO2 NPs. These NPs are hydrophilic due to hydrophobic stearic acid ligands and could be dispersed in toluene, but not in water. These stearic acid-capped TiO2 NPs were surface-modified with 2,3-dimercaptosuccinic acid (DMSA) in order to make them water soluble. The resultant TiO2 NPs were easily redispersed in water without any noticeable aggregation. The Rietveld profile fitting of X-ray diffraction (XRD) pattern of the TiO2 NPs revealed highly crystalline anatase structure. The average crystallite size of TiO2 NPs was calculated to be 6.89 nm, which agrees with TEM results. These results have important implications for the use of TiO2 in biomedical, environmental, and industrial applications.

SUBMITTER: Mohan R

PROVIDER: S-EPMC4219175 | biostudies-literature | 2013 Dec

REPOSITORIES: biostudies-literature

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Water-dispersible TiO2 nanoparticles via a biphasic solvothermal reaction method.

Mohan Rajneesh R Drbohlavova Jana J Hubalek Jaromir J

Nanoscale research letters 20131201 1

A biphasic solvothermal reaction method has been used for the synthesis of TiO2 nanoparticles (NPs). In this method, hydrolysis and nucleation occur at the interface of organic phase (titanium (IV) n-propoxide and stearic acid dissolved in toluene) and water phase (tert-butylamine dissolved in water) resulting in the nucleation of the stearic acid-capped TiO2 NPs. These NPs are hydrophilic due to hydrophobic stearic acid ligands and could be dispersed in toluene, but not in water. These stearic ...[more]

PMID: 24289214

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Project description:BACKGROUND:OZ439 is a new chemical entity which is active against drug-resistant malaria and shows potential as a single-dose cure. However, development of an oral formulation with desired exposure has proved problematic, as OZ439 is poorly soluble (BCS Class II drug). In order to be feasible for low and middle income countries (LMICs), any process to create or formulate such a therapeutic must be inexpensive at scale, and the resulting formulation must survive without refrigeration even in hot, humid climates. We here demonstrate the scalability and stability of a nanoparticle (NP) formulation of OZ439. Previously, we applied a combination of hydrophobic ion pairing and Flash NanoPrecipitation (FNP) to formulate OZ439 NPs 150 nm in diameter using the inexpensive stabilizer hydroxypropyl methylcellulose acetate succinate (HPMCAS). Lyophilization was used to process the NPs into a dry form, and the powder's in vitro solubilization was over tenfold higher than unprocessed OZ439. METHODS:In this study, we optimize our previous formulation using a large-scale multi-inlet vortex mixer (MIVM). Spray drying is a more scalable and less expensive operation than lyophilization and is, therefore, optimized to produce dry powders. The spray dried powders are then subjected to a series of accelerated aging stability trials at high temperature and humidity conditions. RESULTS:The spray dried OZ439 powder's dissolution kinetics are superior to those of lyophilized NPs. The powder's OZ439 solubilization profile remains constant after 1 month in uncapped vials in an oven at 50 °C and 75% RH, and for 6 months in capped vials at 40 °C and 75% RH. In fasted-state intestinal fluid, spray dried NPs achieved 80-85% OZ439 dissolution, to a concentration of 430 µg/mL, within 3 h. In fed-state intestinal fluid, 95-100% OZ439 dissolution is achieved within 1 h, to a concentration of 535 µg/mL. X-ray powder diffraction and differential scanning calorimetry profiles similarly remain constant over these periods. CONCLUSIONS:The combined nanofabrication and drying process described herein, which utilizes two continuous unit operations that can be operated at scale, is an important step toward an industrially-relevant method of formulating the antimalarial OZ439 into a single-dose oral form with good stability against humidity and temperature.

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Water-dispersible TiO2 nanoparticles via a biphasic solvothermal reaction method.

Publications

Water-dispersible TiO2 nanoparticles via a biphasic solvothermal reaction method.

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