Halloysite is an alumosilicate tubular clay with a diameter of 50 nm, an inner lumen of 15 nm and a length of 600-900 nm. It is a natural biocompatible nanomaterial available in thousands of tons at low price, which makes it a good candidate for nanoarchitectural composites. The inner lumen of halloysite may be adjusted by etching to 20-30% of the tube volume and loading with functional agents (antioxidants, anticorrosion agents, flame-retardant agents, drugs, or proteins) allowing for formulations with sustained release tuned by the tube end-stoppers for hours and days. Clogging the tube ends in polymeric composites allows further extension of the release time. Thus, antioxidant-loaded halloysite doped into rubber enhances anti-aging properties for at least 12 months. The addition of 3-5 wt% of halloysite increases the strength of polymeric materials, and the possibility of the tube's orientation promises a gradient of properties. Halloysite nanotubes are a promising mesoporous media for catalytic nanoparticles that may be seeded on the tube surface or synthesized exclusively in the lumens, providing enhanced catalytic properties, especially at high temperatures. In vitro and in vivo studies on biological cells and worms indicate the safety of halloysite, and tests for efficient adsorption of mycotoxins in animals' stomachs are also carried out.

Halloysite Clay Nanotubes for Loading and Sustained Release of Functional Compounds.

Halloysite nanotubes (HNTs) are clay minerals with a hollow nanotubular structure. There is growing interest in these nanomaterials, due to their biocompatibility, potential applications and availability. The surface chemistry of HNTs is versatile for the targeted chemical modification of the inner lumen and outer surface. Functionalized halloysite constitutes a valuable support for metal nanoparticles, promoting catalytic applications with tunable properties. The peculiar tubular shape of HNTs favors the dispersion and surface availability of the supported metal nanoparticles that are active in the catalytic path. Moreover, the presence of an empty lumen opens new perspectives for the production of nanoarchitectures with synergistic catalytic effects, due to the increase in local concentrations and confinement. The main focus of this review is the research on modified halloysite nanotubes for the preparation of valuable supports for metal nanoparticles and their applications in catalytic processes.

Halloysite Nanotubes as Support for Metal-Based Catalysts

Halloysite nanotubes (HNTs) have a unique tubular structure in nanoscale, and have shown potential as novel carriers for various drugs. Coating the nanotubes with a hydrophilic polymer shell can significantly decrease the toxicity and provide colloidal stability during blood circulation. Here, we synthesized chitosan grafted HNTs (HNTs-g-CS) and investigated their potential as a nano-formulation for the anticancer drug curcumin. The structure and properties of HNTs-g-CS were characterized using water contact angle, zeta-potential, Fourier transform infrared (FTIR) spectroscopy, thermogravimetric analysis (TGA), and transmission electron microscopy (TEM) techniques. HNTs-g-CS exhibit a maximum 90.8% entrapment efficiency and 3.4% loading capacity of curcumin, which are higher than those of raw HNTs. HNTs-g-CS also show no obvious hemolytic phenomenon and good stability in serum. The cumulative release ratio of curcumin from HNTs-g-CS/curcumin at cell lysate after 48 hours is 84.2%. The curcumin loaded HNTs-g-CS show specific toxicity to various cancer cell lines, including HepG2, MCF-7, SV-HUC-1, EJ, Caski and HeLa, and demonstrate an inhibition concentration of IC50 at 5.3–192 μM as assessed by cytotoxicity studies. The anticancer activity of this nanoformulation is extremely high in EJ cells compared with the other cancer cell lines. The cell uptake of HNTs-g-CS is confirmed by fluorescence microscopy. Flow cytometric analysis of curcumin loaded HNTs-g-CS shows that curcumin loaded HNTs-g-CS increase apoptosis on EJ cells. The content of ROS created by HNTs-g-CS/curcumin is more than that of free curcumin. All these results suggest that HNTs-g-CS are potential nanovehicles for anticancer drug delivery in cancer therapy.

Functionalized halloysite nanotube by chitosan grafting for drug delivery of curcumin to achieve enhanced anticancer efficacy

Halloysite nanotubes (HNTs) are natural aluminosilicates with unique hollow lumen structure, also having high specific area, good biocompatibility, nontoxicity, and low price. Here, we designed a chitosan oligosaccharide-grafted HNTs (HNTs-g-COS) as a doxorubicin (DOX) carrier for treating breast cancer both in vitro and in vivo. The structure of HNTs-g-COS was first characterized by various methods. HNTs-g-COS showed positively charged surface and improved hemocompatibility. DOX-loaded HNTs-g-COS (DOX@HNTs-g-COS) released in cell lysate in a controlled manner. The IC50 value of DOX@HNTs-g-COS toward MCF-7 cells was 1.17 μg mL–1, while it was 2.43 μg mL–1 for free DOX. DOX@HNTs-g-COS increased the apoptosis effects of MCF-7 cells as shown in flow cytometry results. Also, reactive oxygen species of cells induced by DOX@HNTs-g-COS were drug-dose-dependent. DOX@HNTs-g-COS could enter the MCF-7 cells and induce mitochondrial damage as well as attack the nuclei. The in vivo antitumor effect of DOX@HNTs-g-COS w...

Enhanced Therapeutic Efficacy of Doxorubicin for Breast Cancer Using Chitosan Oligosaccharide-Modified Halloysite Nanotubes

Halloysite nanotubes as support for metal-based catalysts

A novel aging-resistant styrene–butadiene rubber (SBR) composite is prepared using the antioxidant N-isopropyl-N′-phenyl-p-phenylenediamine (4010NA) loaded inside of halloysite clay nanotubes and used as filler. Loading the antioxidant inside of halloysite allows for its sustained release for nine months in the rubber matrix. By utilizing modified halloysite, the antioxidant concentration in this rubber nanoformulation is tripled without causing “blooming” defects. Furthermore, the halloysite is silanized to enhance its miscibility with rubber. The aging resistance of SBR–halloysite composites is studied by comparing the mechanical properties before and after thermal-oxidative aging. A seven-day test at 90 °C shows preservation of mechanical properties, and no 4010NA blooming is observed, even after one month. Styrene–butadiene rubber with 27 wt % halloysite loaded with 4010NA shows marked increase in aging resistance and promising future of halloysite as a functional rubber filler.

Highly aging-resistant elastomers doped with antioxidant-loaded clay nanotubes.

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Highly aging-resistant elastomers doped with antioxidant-loaded clay nanotubes.