KR20160025262A - Gold nanorod-grafted titania nanotubes and preparation method thereof - Google Patents

Gold nanorod-grafted titania nanotubes and preparation method thereof Download PDF

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KR20160025262A
KR20160025262A KR1020140112269A KR20140112269A KR20160025262A KR 20160025262 A KR20160025262 A KR 20160025262A KR 1020140112269 A KR1020140112269 A KR 1020140112269A KR 20140112269 A KR20140112269 A KR 20140112269A KR 20160025262 A KR20160025262 A KR 20160025262A
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drug
titania nanotube
surface
titania
nanotube layer
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KR101640986B1 (en
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오승한
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원광대학교산학협력단
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61FFILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
    • A61F2/00Filters implantable into blood vessels; Prostheses, i.e. artificial substitutes or replacements for parts of the body; Appliances for connecting them with the body; Devices providing patency to, or preventing collapsing of, tubular structures of the body, e.g. stents
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION, OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS, OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS, OR SURGICAL ARTICLES
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/02Inorganic materials
    • A61L27/04Metals or alloys
    • A61L27/06Titanium or titanium alloys
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION, OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS, OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS, OR SURGICAL ARTICLES
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/40Composite materials, i.e. containing one material dispersed in a matrix of the same or different material
    • A61L27/44Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having a macromolecular matrix
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION, OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS, OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS, OR SURGICAL ARTICLES
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/50Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • A61L27/54Biologically active materials, e.g. therapeutic substances
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION, OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS, OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS, OR SURGICAL ARTICLES
    • A61L2420/00Materials or methods for coatings medical devices

Abstract

The present invention relates to a titania nanotube to which gold nanorods are bound and a method of preparing the same. More specifically, the present invention relates to a titania nanotube to which gold nanorods are bound and a titania nanotube layer on the surface of the titanium material. Replacing the SH group on the surface of the titania nanotube layer; And bonding the gold nanorods to the SH groups on the surface of the titania nanotube layer. The present invention relates to a method for preparing gold nanorod-coated titania nanotubes by releasing a drug for a desired period of time at a desired time, And at the same time minimize side effects from unnecessary dosing.

Description

Technical Field [0001] The present invention relates to a titania nanotube having gold nanorods bonded thereto,

More particularly, the present invention relates to an antimicrobial composite containing a gold nanorod-bonded titania nanotube, and a method of forming a titania nanotube layer on the surface of a titanium material. ; Replacing the SH group on the surface of the titania nanotube layer; And bonding the gold nanorod to the SH group on the surface of the titania nanotube layer.

The long-term clinical success of the implant is determined by the osseointegration of the implant between the initial implant and the bone tissue. In order to increase osseointegration, a method of adjusting the surface roughness of the implant or coating the growth factor or hormone was adopted, thereby improving the initial adhesion of bone marrow cells by changing the chemical characteristics, charge, microstructure and porosity of the implant surface . However, studies have shown that increasing bone adhesion is susceptible to bacterial infections. Bacteria bind to growth factors or protein-coated surfaces as easily as bone marrow cells. Once the bacteria penetrate into the coated surface, it is difficult to remove using conventional sterilization techniques.

Therefore, in order to prevent or treat bacterial infections, antibiotic treatment is required after about 2 months after implant surgery. In such a case, methods such as oral administration, intravenous administration, subcutaneous administration, topical administration and the like may be used for the subject.

In general, Drug delivery system (DDS) is a dosage form designed to minimize the side effects of existing medicines and to maximize efficacy and efficacy, thereby delivering the necessary amount of medication. This drug delivery system can be administered orally Or as a means of solving the inconvenience of scanning. For example, the drug delivery system is effective when the drug is administered orally to the antibiotics when the drug acts on the pathogen, but the adverse effects such as ulcers in the gastrointestinal tract are reduced, This means designing the body to maximize the effect.

In addition, by introducing a new method to the delivery route and delivery form of the drug taking into consideration the therapeutic method, the specific physicochemical properties of the drug, and the pharmacokinetic characteristics, it is developed and used for the purpose of obtaining an effective treatment method and reducing the inconvenience of the patient There is considerable research going on now.

However, for most of these drug delivery systems, there are few techniques involved in controlling drug release time and duration. For example, in the case of antibiotic treatment after implant surgery, it is not necessary that the antibiotic be eluted immediately after implant surgery, and it is necessary about two months after the operation as described above. Therefore, it is necessary to introduce a technique for controlling the elution time and duration of the drug, but the related art is not known.

Korean Patent No. 1,219,471 discloses a method for surface treatment of dental implants and a dental implant surface treated by the method, comprising the steps of: a) forming a titania nanotube on the surface of a dental implant; b) converting the titania nanotubes into a crystalline phase by heat treating the dental implant; And c) coating carbon nanotubes on the titania nanotubes. The surface treatment method of the dental implant and the dental implant surface-treated by the method described above are disclosed.

Korean Patent No. 1,385,010 discloses a method for coating nano-sized titania on an implantable implant by anodic oxidation method. The nano-titania coating which is coated on the entire surface of the base by anodic oxidation method formed by Ca-P and Ti oxide system The present invention relates to an implantable implant coated with nano-titania by an anodic oxidation method characterized by containing particles.

However, the above documents only disclose a surface treatment method of a dental implant.

U.S. Published Patent Application No. 2010/0247611 relates to a composition containing a NO-emitting compound deposited on a titanium dioxide nanomaterial and a titanium dioxide nanomaterial that releases NO under photochemical conditions, wherein a composition comprising PbS, It is disclosed that a semiconductor material such as PbSe, CuS, Cu 2 S, FeS 2 , CdS, CdSe, CdTe, ZnS, Ag 2 S, CuInS 2 , Rh 2 S 3 and RuS 2 may be further contained.

Korean Patent No. 1,336,780 discloses a drug delivery device using an implant. More specifically, the drug delivery device includes an implant that is implanted in a human body and performs a support function, and a lid part that is coupled to the implant to perform a blocking function. And a medication part formed at an end of the diffusion part and adapted to inject the contents of the drug cartridge into the human body. The medication delivery device using the implant, .

Korean Patent Laid-Open Publication No. 2014-0098273 discloses a method of manufacturing an implant including a drug delivery layer and a bioactive implant composition comprising the same, more particularly, a method of preparing a chitosan-bioactive glass composite solution; Preparing a drug-containing composite coating composition by adding a drug to the chitosan-bioactive glass composite solution; And preparing a drug delivery layer by electrophoretically depositing the composite coating composition on the surface of the implant, and a bioactive implant composition containing the same.

Although the above references disclose titanium dioxide nanomaterials that emit NO, implants with drug doses, and implants capable of releasing drugs, there is a technology capable of controlling the release time and duration of drug release Is not specifically disclosed.

The inventors of the present invention have found that when a gold nano-rod is immobilized on the surface of a titania nanotube and the drug is injected thereinto, the release of the drug is turned on by the ultraviolet laser irradiation and the release time and duration of the drug can be controlled. Thereby completing the present invention.

Korean Patent No. 1,219,471 Korean Patent No. 1,385,010 U.S. Published Patent Application No. 2010/0247611 Korean Registered Patent No. 1,336,780 Korean Patent Publication No. 2014-0098273 Japanese Patent Laid-Open No. 2005-320616 Japanese Patent Laid-Open No. 2005-255582.

K. Gulati et al. Nanoscale Research Letters, vol. 6, article 571, 2011; S. Liu and A. Chen, Langmuir, Vol. 21, no. 18, pp. 8409-13, 2006; M. Paulose et al., Journal of Physical Chemistry B, vol. 110, no. 33, pp. 16179-184, 2006; H. Zhang et al., Langmuir, vol. 26, no. 13, pp. 11226-232, 2010; M. Bigerelle et al., Biomaterials, vol. 23, no. 7, pp. 1563-77, 2002; A. L. Linsebigler et al., Chemical Reviews, vol. 95, no. 3, pp. 735-58, 1995; S. Oh et al., Journal of Nanomaterials, vol. 2013, Article ID 802318, 7 pages, 2013; J. Choi et al., Small, vol. 8, no. 5, pp. 746-753, 2012.

The present invention provides a drug delivery system (DDS) capable of controlling the release time and the release period of a drug to release a drug for a desired period of time to prevent unnecessary dosing, To minimize the side effects of

The present invention relates to a titania nanotube composite to which gold nanorods are bonded, and a method of producing such a composite, that is, a method of forming a titania nanotube layer on a surface of a titanium material; Replacing the SH group on the surface of the titania nanotube layer; And a step of binding gold nanorods to the SH group on the surface of the titania nanotube layer, thereby providing drug delivery capable of controlling the release time and release time of the drug System (Drug Delivery System, DDS).

When the gold nano-rod-coated titania nanotube composite according to the present invention is used, it is possible to release a drug for a desired period of time at a desired time, thereby preventing unnecessary dosing and minimizing side effects due to unnecessary dosing.

1 is a schematic diagram of a process for producing a gold nano-rod-coated titania nanotube.
2 is a photograph of a machined titanium plate (left) and an electrolytically polished titanium plate (right).
3 is a scanning electron microscope (SEM) image of a titania nanotube aligned vertically on a titanium plate by anodic oxidation.
4 is a TEM image (a) of a gold nano rod, respectively; Gold nano-rod UV-Vis spectrophotometer spectrum (b); And the gold nanorod aspect ratio analysis graph (c).
FIG. 5 is an FE-SEM image of gold nanorod-coated titania nanotubes surface-treated with (a) 0.1 M, (b) 0.5 M, Gt; EDX < / RTI > images of gold nanorod-coated titania nanotubes surface-treated with < RTI ID = 0.0 >
6 is an X-ray diffraction pattern of gold nanorod-coated 100 nm titania nanotubes according to the present invention.
FIG. 7 is a graph of the infrared laser irradiation photograph (a) and a graph of tetracycline leaching amount (b) between experimental groups.
8 is a photograph (a) showing the results of the antimicrobial agent diffusion experiment and a graph (b) showing the results of the measurement of the bacterial death zone between the experimental groups.

The present invention relates to a titania nanotube to which gold nanorods are bound and a method of preparing the same. More specifically, the present invention relates to a titania nanotube to which gold nanorods are bound and a titania nanotube layer on the surface of the titanium material. Replacing the SH group on the surface of the titania nanotube layer; And bonding the gold nanorod to the SH group on the surface of the titania nanotube layer.

Hereinafter, the present invention will be described in more detail.

The present invention relates to a titania nanotube layer formed on the surface of a titanium material; And gold nanorods bonded to the titania nanotube layer through an SH group.

The term " titania " in the present invention refers to an oxide of titanium.

In one aspect of the invention, the gold nanorods may be covalently bonded to the titania nanotube layer.

In one embodiment of the present invention, the gold nanorod may have an absorption peak wavelength within a range from 400 nm to 1,200 nm, and if the electromagnetic wave in the wavelength range is irradiated, it may cause absorption of light called plasmon absorption, have. The gold nanorods are different in shape or size, and their absorption wavelengths are also different. It is known that gold nanorods having an aspect ratio of 1.1 to 8.0 have a absorption range of 400 to 1,200 nm. However, it is preferable to use gold nano-rods having absorption peaks in the range of 600 to 1,000 nm which is a wavelength capable of penetrating the skin and tissues.

In one aspect of the present invention, the present invention provides a titania nanotube layer formed on a surface of a titanium material; A gold nanorod bonded to the titania nanotube layer through an SH group; And a drug layer wherein the drug layer is loaded into the titania nanotubes to which the gold nanorods are bound.

The complex exhibits antimicrobial activity by itself without loading a separate antibiotic. However, antibiotics may be additionally loaded to increase the antimicrobial effect. In addition to antibiotics, there may also be used antibiotics such as antiinflammatory agents, analgesics, anticancer agents, antidiabetic agents, therapeutic agents for cardiovascular diseases, agents for treatment of hyperlipidemia, drugs for metabolic syndrome, psychotropic drugs, central nervous system drugs, The drug may be loaded, but not limited thereto, and various drugs may be selectively loaded depending on the therapeutic purpose.

In one aspect of the present invention, there is provided a pharmaceutical composition comprising an antibiotic such as tetracycline, an aminoglycoside antibiotic, a macrolide antibiotic, a beta-lactam antibiotic, amphotericin, polymyxin, vancomycin, rifampin, quinolone antibiotics, Antibiotics can be loaded. Especially when loaded on a dental implant, it is possible to obtain a desired therapeutic effect by irradiating infrared rays and the like at a time when antibiotics need to be eluted after implant surgery. Thus, a desired therapeutic effect can be obtained, Is possible.

In one embodiment of the present invention, the drug may be released by infrared or ultraviolet radiation, and more specifically by infrared radiation.

In an embodiment of the present invention, the wavelength exhibiting the photothermal effect varies depending on the aspect ratio of the gold nano-rods, and therefore it is preferable to synthesize and apply gold nano-rods having an aspect ratio suitable for the wavelength to be used.

The aspect ratio of the gold nano-rods suitable for the wavelength (830 nm) of the infrared laser used in the present invention is about 3.83. When it is intended to emit the drug by irradiation with infrared rays, the aspect ratio of the gold nano- .

In one embodiment of the invention, the drug may be a drug-biodegradable polymer composite.

In one embodiment of the present invention, when the drug-biodegradable polymer composite material is used, the biodegradable polymer is gradually biodegraded and the drug can be slowly eluted / released, which is more preferable.

In one embodiment of the present invention, the biodegradable polymer includes polylactic acid, polyglycolic acid, polylactic acid-glycolic acid copolymer, poly-epsilon -caprolactone, polylactide caprolactone, polyamino acid, polyanhydride, aliphatic poly There may be used any one selected from the group consisting of esters, cellulose, lignin, starch, alginic acid, bio-polyester, bio-cellulose, polysaccharide and polyamic acid. More specifically, polylactic acid may be used.

In one aspect of the invention, the complex may be in the form of a medical implant, and more particularly in the form of a dental implant.

According to another aspect of the present invention, there is provided a method of manufacturing a semiconductor device, comprising: (a) forming a titania nanotube layer on a surface of a titanium material; (b) substituting an SH group on the surface of the titania nanotube layer; And (c) bonding the gold nanorod to the SH group on the surface of the titania nanotube layer.

In one embodiment of the present invention, the gold nanorods may be covalently bonded to the SH group on the surface of the titania nanotube layer.

In one embodiment of the present invention, in step (b), one or more selected from the group consisting of thiolactic acid, thioxanthene, thiosalicylic acid, thiopropionic acid and thioglycolic acid may be used to replace the SH group More specifically, the SH group can be substituted on the surface of the titania nanotube layer by using thiolactic acid.

In one embodiment of the present invention, in step (b), at least one thio compound selected from the group consisting of thiolactic acid, thioxanthate, thiosalicylic acid, thiopropionic acid and thioglycolic acid is reacted at 0.1 to 1 M , And more specifically, a concentration of about 1 M, for example. The structure change and collapse of the titania nanotubes by the surface treatment of the thio compound did not occur.

In one embodiment of the present invention, the step (c) may further include a step of injecting a drug into the titania nanotube layer.

In one aspect of the present invention, the drug may be a drug-biodegradable polymer composite.

In an embodiment of the present invention, when the drug is loaded alone on the titania nanotube, the problem of eluting may occur. However, when the biodegradable polymer is loaded in a state in which the biodegradable polymer is combined with the biodegradable polymer, Drug can be slowly released / released with biodegradation.

In one embodiment of the present invention, the biodegradable polymer includes polylactic acid, polyglycolic acid, polylactic acid-glycolic acid copolymer, poly-epsilon -caprolactone, polylactide caprolactone, polyamino acid, polyanhydride, aliphatic poly There may be used any one selected from the group consisting of esters, cellulose, lignin, starch, alginic acid, bio-polyester, bio-cellulose, polysaccharide and polyamic acid. More specifically, polylactic acid may be used.

The reason for using biodegradable polymer is that when the drug is carried on a nanotube by itself, there is no entrapping substance. Therefore, when the drug is mixed with the biodegradable polymer, the slow degradation rate of the biodegradable polymer This is because the drug can be slowly eluted with a small amount.

In addition, when all materials on the surface are removed due to the photothermal effect of gold nano-rods when irradiated with an infrared laser, the biodegradable polymer is coated on the drug even if it is eluted all at once, so that the eluted drug does not randomly move, And it is continuously present together with the polymer. Biodegradable polymers such as polylactic acid are biodegradable polymers that have already been proven, so they dissolve slowly in the human body and are harmless to human body. For this reason, in the present invention, a composite obtained by mixing a biodegradable polymer and a drug is supported on a titania nanotube.

However, in an embodiment of the present invention, even if the drug is not loaded, the antimicrobial property can be exhibited due to the presence of the gold nanorod.

In one embodiment of the present invention, specifically, a homogenized titania nanotube is prepared, and a titania nanotube surface on which the SH group is activated by surface treatment with titanic acid on the surface of the titania nanotube for gold nano rod coating is prepared, By attaching gold nanorods chemically to the surface of titania nanotubes, gold nanorod-coated titania nanotubes can be fabricated.

In one aspect of the invention, the gold nanorods can be prepared using conventional methods known in the art.

For example, gold nanorods with a high aspect ratio can be synthesized by using cetyltrimethylammonium bromide (CTAB) and benzyldimethylammonium chloride (BDAC) together in a growth solution B. Nikoobakht and MA El-Sayed, Chem. Mater. 15, 1957-1962, 2003). CTAB and BDAC have very similar structure and have selective binding force on the surface of gold. In this paper, as the amount of the BDAC relative to the CTAB increases, that is, as the BDAC / CTAB value increases, the width of the gold nano rod becomes narrower, and the aspect ratio of the gold nano rod becomes larger. ) Is shifted to a long wavelength. Accordingly, it is disclosed that the case where the BDAC / CTAB value is 6 or more is preferably used.

In one embodiment of the present invention, a specific method for producing gold nano-rods is as follows:

HAuCl 4 and NaBH 4 were mixed and CTAB was added to prepare a seed solution. AgNO 3 , HAuCl 4 and CTAB were mixed to prepare gold nanorods. L-ascorbic acid is added while mixing seed solution and growth solution to prepare gold nanorods. The aspect ratio of gold nanorods can be varied by controlling the amount of growth solution and L-ascorbic acid added.

The titania nanotube composite with gold nanorods according to the present invention can be applied not only to drug carriers for drug delivery systems (DDS), but also to in vivo diagnostic kits, therapeutic compositions, cosmetics, biosensors and the like.

Hereinafter, the present invention will be described in more detail with reference to Production Examples and Experimental Examples. It is to be understood, however, that the following Preparation Examples are intended to assist the understanding of the present invention and are not intended to limit the scope of the present invention thereto.

Manufacturing example  One. Titania  Fabrication of Nanotube Specimen

(Perchloric acid, Sigma, USA), 37, and the plate was washed with acetone, ethanol, and distilled water, Surface treatment with electrolysis using 59% methanol (Sigma, USA) in butoxy ethylene glycol (Junsei I, Japan) and polishing was carried out to obtain a clean surface having flatness of 5 nm or less Titanium plates were prepared (Shin et al., 2008).

The electrolytically polished titanium plate was subjected to anodic oxidation in the range of 5 - 20 V for 30 minutes using 0.5 wt% hydrofluoric acid (purity: 48%, Sigma, USA) as the electrolyte solution. After completion of the anodic oxidation, the specimens were washed in distilled water, dried in an oven at 60 ° C. for 24 hours, and then heat-treated at 500 ° C. for 2 hours (heat treatment in air, heating and cooling rate = 1 K / min).

Manufacturing example  2. Gold Nanorod  synthesis

The gold nanorods were synthesized by modifying already known techniques.

A seed solution was prepared by adding CTAB while mixing HAuCl 4 and NaBH 4 , which are starting materials of gold nano-rods. A growth solution was prepared by mixing AgNO 3 , HAuCl 4 , and CTAB to grow gold nanorods of the seed solution. Gold nanorods were synthesized by adding L-ascorbic acid while mixing seed solution and growth solution. The aspect ratio of the gold nanorods was changed according to the amount of the growth solution and L-ascorbic acid added. Then, the wavelength showing the photothermal effect changes according to the aspect ratio of the gold nano-rod, so that a gold nano rod suitable for the wavelength of the infrared laser used in the present invention (830 nm) was synthesized.

The shape and optical characteristics of the gold nano-rods were analyzed by transmission electron microscopy (TEM) and ultraviolet-visible spectrophotometer, respectively.

As a result of TEM image analysis, a gold nanorod having an aspect ratio of 3.83 was synthesized. As a result of ultraviolet-visible light spectrophotometer, light activity was observed at 830 nm.

Manufacturing example  3. Gold Nanorod  Coated Titania  Nanotube manufacturing

In order to chemically coat gold nanorods on the surface of titania nanotubes, SH groups must be present on the surface of the nanotubes. Therefore, nanotube surfaces were treated with thiolactic acid at three concentrations (0.1, 0.5 and 1.0 M) to replace the surface of the nanotubes with the SH group. As a result of analysis by FE-SEM (Field Emission Scanning Electron Microscopy) and EDX (Energy Dispersive X-ray Spectroscopy) in order to find the optimum concentration of thiolactic acid, as shown in FIG. 5 and Table 1, And no structural change or collapse of the titania nanotubes was observed by the surface treatment with thiolactic acid.

Figure pat00001

As a result of crystal structure analysis by X-ray diffractometer (XRD), the crystal lattice of Au (111) and (200) was confirmed and it was confirmed that the gold nanorods were reliably coated on the titania nanotubes.

Experimental Example  1. Remote controlled drug elution experiment by infrared laser irradiation

10 g of tetracycline was dissolved in 50 ml of DMSO, 4 g of polylactic acid (PLA) was dissolved in 50 ml of tetrahydrofuran, and each of the solutions was mixed to prepare a tetracycline-PLA complex solution Respectively. The prepared solution was injected into titania nanotubes using a vacuum injection method. The titania nanotube specimens were dried at room temperature for 24 hours and irradiated with a hand-held infrared laser (output: 200 mW, RaeHwa LMA, Korea) at 830 nm for 1 minute. The elution rate of the drug eluted by remote control of the infrared laser was measured at a wavelength of 405 nm using a microplate ELISA reader (Spectra Max 250, Thermo Electron Co., USA).

As a result of the measurement of the amount of elution, the results of the experimental group irradiated with the infrared laser were significantly higher than those of the other experimental groups (p <0.05).

Experimental Example  2. Antibacterial Agar diffusion experiment Antimicrobial Agar Diffusion Test )

Streptococcus mutans mutans , ATCC 25176, ATCC, USA). 1 * 10 &lt; 5 &gt; CFU / ml of bacteria were inoculated into agar medium and cultured at 37 DEG C for 24 hours. After 24 hours of incubation, 1 * 1 cm 2 of the specimen was placed on solid agar medium and the experiment was carried out. Infrared laser irradiation group was irradiated with infrared laser for 1 minute, other experimental group was allowed to stand alone, and then incubated at 37 ° C. for 24 hours. After 24 hours of secondary culture, the diameter of the rounded area (bacterium death zone) of the bacteria killed around the specimen was measured at 4 sites and the average value was calculated.

As a result of antimicrobial agent diffusion experiment, it was confirmed that the remote controlled drug elution function of the gold nanorod coated titania nanotube by the infrared laser was clearly exhibited, and the antibacterial characteristic was also excellent. It was observed that the gold nano-rod alone showed some antimicrobial activity.

Claims (9)

  1. A titania nanotube layer formed on a surface of a titanium material; And
    And a gold nanorod bonded to the titania nanotube layer through an SH group.
    Antimicrobial complex.
  2. The method according to claim 1,
    Further comprising a drug layer,
    Wherein the drug layer is a complex in which the drug is loaded into titania nanotubes bound with gold nanorods.
  3. The method according to claim 1,
    Wherein said drug is released by irradiation with ultraviolet or infrared radiation.
  4. The method according to claim 1,
    Wherein the drug is a drug-biodegradable polymer composite.
  5. Wherein said complex is a medical implant.
  6. (a) forming a titania nanotube layer on a surface of a titanium material;
    (b) substituting an SH group on the surface of the titania nanotube layer; And
    (c) bonding the gold nanorod to the SH group on the surface of the titania nanotube layer.
  7. The method according to claim 6,
    Wherein at least one selected from the group consisting of thiolactic acid, thioxanthate, thiosalicylic acid, thiopropionic acid and thioglycolic acid is used in step (b) to replace the SH group. Method for manufacturing coated titania nanotubes.
  8. The method according to claim 6,
    The method of claim 1, further comprising, after step (c), injecting a drug into the titania nanotube layer.
  9. 9. The method of claim 8,
    Wherein the drug is a drug-biodegradable polymer composite. &Lt; RTI ID = 0.0 &gt; 15. &lt; / RTI &gt;
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Cited By (1)

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Publication number Priority date Publication date Assignee Title
CN106824184A (en) * 2017-03-27 2017-06-13 国家纳米科学中心 A kind of gold nanorods nano-titanium oxide catalysis material of mushroom-shaped structure and its preparation method and application

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