CN104645354A - Black titanium dioxide tumor diagnosis and treatment agent as well as preparation method and application thereof - Google Patents
Black titanium dioxide tumor diagnosis and treatment agent as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a black titanium dioxide tumor diagnosis and treatment agent as well as a preparation method and an application thereof. The black titanium dioxide tumor diagnosis and treatment agent is a polyethylene glycol modified black titanium dioxide nano-particle; black titanium dioxide is subjected to hydrophilic modification by using polyethylene glycol to obtain hydrophilic black titanium dioxide, so that the dispersibility and the stability of the black titanium dioxide nano-particle in aqueous solutions are obviously improved, the biocompatibility of the black titanium dioxide nano-particle is increased, the toxic or side effect is reduced, the blood circulation performance is promoted, and the distribution in tumor tissues is promoted.
Description
Technical field
The present invention relates to a kind of black titanium dioxide tumor diagnosis and treatment agent and its preparation method and application, belong to nano material and biomedical applications field.
Background technology
Titanium dioxide semiconductor is owing to having the advantages such as good chemical stability, photocatalytic activity, rich reserves, inexpensive low toxicity at the energy and environmental area, and the aspects such as such as DSSC, ultracapacitor, photodissociation Aquatic product hydrogen, degradation of organic substances dyestuff are widely applied.But due to the energy gap large (Anatase is 3.2eV, and Rutile Type is 3.0eV) of titanium dioxide, only can absorb the ultraviolet light in solar spectrum, device performance and efficiency are greatly limited.Within 2011, U.S. Lao Lunsi-Berkeley National Key Laboratory utilizes hydrogen reducing to obtain the black titanium dioxide of excellent performance first.The method makes the energy gap of titanium dioxide be reduced to 1.54eV, has greatly expanded the visible light-responded scope of titanium dioxide, has been widely applied in the fields such as photocatalysis, lithium battery, infrared wave-absorbing, ultracapacitor.The preparation method of current black titanium dioxide has H
2reducing process, thermit reduction, hydro-thermal method, sol-gal process etc.Wherein, thermit reduction obtains extensive concern due to simple to operate, reproducible, low cost and other advantages.
Cancer has become one of major disease threatening human health.The Diagnosis and Treat developing into cancer of modern nano meter biomaterial provides effectively auxiliary.Carry out early diagnosis also timely this target for the treatment of in order to realize effectively, accurately to cancer, the nanometer diagnosis and treatment agent that design and preparation have diagnosis and treatment integrated function is one of optimal approach.In recent years, the photoinduced near infrared imaging of near-infrared, photoacoustic imaging, photo-thermal therapy and photodynamic therapy get most of the attention in cancer diagnosis and treatment.
Black titanium dioxide reduces due to its energy gap, thus has full spectroscopic optics absorption characteristic near infrared light to UV light region, and be a kind of potential near infrared imaging and photoacoustic imaging contrast agent, be a kind of potential photo-thermal and photodynamic therapy agent simultaneously.
Due to black titanium dioxide bad dispersibility in water prepared at present, unstable in physiological environment, strongly limit its biologic applications.Therefore, developing is even more important in the application of biological field to expansion titanium dioxide for the hydrophilic modification method of a kind of black titanium dioxide of tumor diagnosis and treatment agent.
Summary of the invention
For above demand, the object of the present invention is to provide a kind of black titanium dioxide tumor diagnosis and treatment agent and preparation method thereof and the new opplication in biological field.
On the one hand, the invention provides a kind of black titanium dioxide tumor diagnosis and treatment agent, described black titanium dioxide tumor diagnosis and treatment agent is polyethyleneglycol modified black titanium dioxide nano-particle.
The present invention adopts Polyethylene Glycol carry out hydrophilic modifying to black titanium dioxide and obtain hydrophilic black titanium dioxide, thus black titanium dioxide nano-particle dispersibility in aqueous and stability are significantly improved, and increase black titanium dioxide nano-particle biocompatibility, reduce toxic and side effects and blood circulation promoting performance, promote the distribution in tumor tissues.Meanwhile, this black titanium dioxide has strong absorption near infrared light place, adopts Same Wavelength laser excitation, can produce four large performances simultaneously: one is be used as near infrared imaging contrast agent, for strengthening near infrared imaging contrast, improves image sensitivity and speed; Two is be used as photoacoustic imaging contrast agent, for strengthening photoacoustic imaging contrast, obtains contrast high, the photoacoustic imaging picture of clear picture; Three is can be used as photo-thermal therapy agent, for strengthening photo-thermal therapy effect, up hill and dale, fully ablated tumor; Four is produce singlet oxygen, can be used as a kind of novel photosensitizer for photodynamic therapy.Therefore, black titanium dioxide prepared by the present invention can be used as a kind of novel tumor diagnosis and treatment agent, photo-thermal/photodynamics Synergistic treatment while under guiding for near-infrared heat/optoacoustic Double-mode imaging.
Preferably, the black titanium dioxide used in the described black titanium dioxide tumor diagnosis and treatment agent of preparation and the mass ratio of Polyethylene Glycol are 1:1 ~ 1:2.
Preferably, described Polyethylene Glycol is functional polyethylene glycol, and functionalization functional group is wherein at least one in amino, sulfydryl and carboxyl.
Preferably, the hydration kinetics particle diameter of described black titanium dioxide tumor diagnosis and treatment agent is 50 ~ 70nm, and the particle diameter of the black titanium dioxide in described black titanium dioxide tumor diagnosis and treatment agent is 20 ~ 30nm.
Preferably, the black titanium dioxide in described black titanium dioxide tumor diagnosis and treatment agent is Anatase.
On the other hand, the present invention also provides the preparation method of above-mentioned black titanium dioxide tumor diagnosis and treatment agent, is dissolved in by black titanium dioxide in water, adds functional polyethylene glycol, carry out ultrasonic with Aided Modification after mix homogeneously, described black titanium dioxide tumor diagnosis and treatment agent can be obtained.
The present invention adopts the Polyethylene Glycol of functionalization to carry out hydrophilic modifying to black titanium dioxide under ultrasonication, preparation technology's simple and fast, pollute little, reproducible.Ultrasonicly can reduce particle agglomeration, reduce particle diameter, strengthen dispersibility and stability.
Preferably, the mass ratio of black titanium dioxide and functional polyethylene glycol is 1:1 ~ 1:2.
Preferably, described black titanium dioxide is the black titanium dioxide that thermit reduction obtains.
Preferably, the described ultrasonic time is 0.5 ~ 2 hour, describedly ultrasonicly to carry out in ultrasonic cell disrupte machine under condition of ice bath.
Another aspect, the present invention also provides above-mentioned black titanium dioxide tumor diagnosis and treatment agent to apply in biological field.
Further, the invention provides the application of above-mentioned black titanium dioxide tumor diagnosis and treatment agent in preparation tumor diagnosis and treatment agent.
Further, the invention provides above-mentioned black titanium dioxide tumor diagnosis and treatment agent and prepare the application in near-infrared heat/optoacoustic Double-mode imaging contrast agent.
Further, the invention provides the application of above-mentioned black titanium dioxide tumor diagnosis and treatment agent in preparation photo-thermal/photodynamic therapy agent simultaneously.
Further, the invention provides the application of above-mentioned black titanium dioxide tumor diagnosis and treatment agent while preparing under near-infrared heat/optoacoustic Double-mode imaging guiding in photo-thermal/photodynamics nanometer diagnosis and treatment agent.
Chemical reagent used in the present invention is cheap and easy to get, modified technique is simple, reproducible, the black titanium dioxide of poorly water-soluble is passed through ultrasonic wave added method hydrophilic modifying by success, improve its dispersibility, stability and biocompatibility in aqueous, and expand the new opplication of black titanium dioxide at biological field.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope photo that is dispersed in water respectively of the obtained black titanium dioxide (a, b) of embodiment 1 and hydrophilic black titanium dioxide (c, d) and corresponding digital photograph;
Fig. 2 is the EDS energy spectrogram of the black titanium dioxide that embodiment 1 obtains;
Fig. 3 is the XRD figure spectrum of the obtained black titanium dioxide (a) of embodiment 1 and hydrophilic black titanium dioxide (b);
Fig. 4 is the Raman collection of illustrative plates of the obtained black titanium dioxide (a) of embodiment 1 and hydrophilic black titanium dioxide (b);
Fig. 5 is DLS particle diameter and the Zeta potential figure of the obtained black titanium dioxide (a) of embodiment 1 and hydrophilic black titanium dioxide (b).Wherein, a is grain size distribution, and b is Zeta potential figure;
Fig. 6 is the FTIR collection of illustrative plates of the obtained black titanium dioxide (a) of embodiment 1 and hydrophilic black titanium dioxide (b);
Fig. 7 is the UV-Vis collection of illustrative plates of the variable concentrations hydrophilic black titanium dioxide aqueous solution that embodiment 1 obtains;
Fig. 8 is the near infrared imaging picture of variable concentrations hydrophilic black titanium dioxide aqueous solution under 808nm different capacity density laser irradiates that embodiment 1 obtains;
Fig. 9 is the obtained photoacoustic signal of variable concentrations hydrophilic black titanium dioxide aqueous solution of embodiment 1 and the curve of concentration and corresponding photoacoustic imaging picture;
Figure 10 is the heating curve of variable concentrations hydrophilic black titanium dioxide aqueous solution under 808nm laser irradiates that embodiment 1 obtains;
Figure 11 is the quantum yield curve that the obtained black titanium dioxide of embodiment 1 produces singlet oxygen under 808nm laser irradiates.
Detailed description of the invention
Further illustrate the present invention below in conjunction with accompanying drawing and following embodiment, should be understood that accompanying drawing and following embodiment are only for illustration of the present invention, and unrestricted the present invention.
Black titanium dioxide tumor diagnosis and treatment agent of the present invention is polyethyleneglycol modified black titanium dioxide nano-particle.By Polyethylene Glycol hydrophilic modifying, thus obtain hydrophilic black titanium dioxide nano-particle.Black titanium dioxide wherein can be pass through H
2the black titanium dioxide that the methods such as reducing process, thermit reduction, hydro-thermal method, sol-gal process are obtained.In preparation process, the mass ratio of black titanium dioxide used and Polyethylene Glycol can be 1:1 ~ 1:2.By the mass ratio of both adjustments, the hydrophilic of nano-particle can be regulated.
The Polyethylene Glycol carrying out modifying can be functional polyethylene glycol.Functionalization functional group wherein includes but not limited at least one in amino, sulfydryl and carboxyl.Like this, the Ti in black titanium dioxide can form coordination with functionalization functional group, thus strengthens the connective stability between PEG.In addition, the molecular weight of Polyethylene Glycol can be 2000,4000 or 5000 dalton.
The particle diameter of hydrophilic black titanium dioxide nano-particle of the present invention is little, narrowly distributing, and such as hydration kinetics particle diameter is 50 ~ 70nm.The particle diameter of black titanium dioxide is wherein 20 ~ 30nm.
Hydrophilic black titanium dioxide in the present invention has identical crystalline phase with unmodified front black titanium dioxide, such as, be Anatase.
Hydrophilic black titanium dioxide of the present invention, on the one hand, black titanium dioxide has strong absorption near infrared light place, adopt Same Wavelength laser excitation, four large performances can be produced: one is be used as near infrared imaging contrast agent simultaneously, for strengthening near infrared imaging contrast, improve image sensitivity and speed; Two is be used as photoacoustic imaging contrast agent, for strengthening photoacoustic imaging contrast, obtains contrast high, the photoacoustic imaging picture of clear picture; Three is can be used as photo-thermal therapy agent, for strengthening photo-thermal therapy effect, up hill and dale, fully ablated tumor; Four is produce singlet oxygen, can be used as a kind of novel photosensitizer for photodynamic therapy; On the other hand, due to by PEG hydrophilic modifying, black titanium dioxide dispersibility in aqueous and stability are significantly improved, and increase biocompatibility, reduce toxic and side effects and blood circulation promoting performance, promote the distribution in tumor tissues.Therefore, hydrophilic black titanium dioxide of the present invention can be used as a kind of novel tumor diagnosis and treatment agent, photo-thermal/photodynamics Synergistic treatment while under guiding for near-infrared heat/optoacoustic Double-mode imaging.Hydrophilic black titanium dioxide of the present invention has good biological safety and significant imaging, therapeutic effect, can be used as a kind of diagnosis and treatment agent of excellent performance, the Diagnosis and Treat of various diseases especially cancer can be realized simultaneously, substantially increase therapeutic efficiency and safety, have very important significance in materialogy and medical science.
< preparation method >
The present invention can adopt functional polyethylene glycol to carry out hydrophilic modifying to black titanium dioxide under ultrasonication.
The functional polyethylene glycol adopted can be the Polyethylene Glycol such as band amino, sulfydryl, carboxyl.Black titanium dioxide to be modified can pass through H
2the preparations such as reducing process, thermit reduction, hydro-thermal method, sol-gal process.As the example of thermit reduction, such as can see Chinese patent CN103191707A.
In one example, the black titanium dioxide obtained that high temperature aluminum reduced dissolves in deionized water, adds the Polyethylene Glycol of appropriate functionalization, stirring and dissolving, then mixed solution is placed in ice bath, with ultrasonic cell disrupte machine ultrasonic a period of time with Aided Modification.By the effect of ultrasonic cell disrupte machine, can tear black titanium dioxide, thus its particle diameter is reduced, distribution narrow.
Wherein, the mass ratio of black titanium dioxide and functional polyethylene glycol can be 1:1 ~ 1:2.Ultrasonic time can be 0.5 ~ 2 hour.
Before and after hydrophilic modifying, the crystalline phase of black titanium dioxide remains unchanged.That is, hydrophilic modification method of the present invention can not change the crystalline phase of black titanium dioxide.
Black titanium dioxide after hydrophilic modifying can be uniformly dispersed in aqueous solution, without obviously reuniting, occurs obvious Tyndall effect when laser beam irradiation.
Exemplify embodiment below further to describe the present invention in detail.Should understand equally; following examples are only used to further illustrate the present invention; can not be interpreted as limiting the scope of the invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.The technological parameters such as the proportioning that following example is concrete, time, temperature are also only examples in OK range, and namely those skilled in the art can be done in suitable scope by explanation herein and select, and do not really want the concrete numerical value being defined in Examples below.
Embodiment 1
The original black titanium dioxide prepared by 100mg aluminum reduction method is dispersed in 20mL water, adds the Polyethylene Glycol that 100mg is with amino functional group, stirring and dissolving;
Above-mentioned mixed solution is transferred in ice bath, with ultrasonic cell disrupte machine Ultrasonic Pulverization 0.5h-2h.Reacted solution centrifugal is collected, then is dispersed in water or phosphate buffered solution for subsequent use.
Fig. 1 a is the transmission electron microscope photo of original black titanium dioxide prepared by the present embodiment, and in figure, black titanium dioxide is reunited serious, and bad dispersibility, is about 20-30nm.
Fig. 1 b is the digital photograph that original black titanium dioxide prepared by the present embodiment is dispersed in water.In figure, black titanium dioxide is deposited in bottom cuvette, and upper liquid is transparent aqueous solution.
Fig. 1 c is the transmission electron microscope photo of hydrophilic black titanium dioxide prepared by the present embodiment, and in figure, black titanium dioxide is uniformly dispersed, and without obviously reuniting, particle diameter is 20 ~ 30nm.
Fig. 1 d is the digital photograph that hydrophilic black titanium dioxide prepared by the present embodiment is dispersed in water.In figure, black titanium dioxide is in aqueous dispersed, occurs obvious Tyndall effect during laser beam irradiation.
Fig. 2 is the EDS energy spectrogram of black titanium dioxide prepared by the present embodiment, proves the existence of Ti and O.
Fig. 3 is the XRD figure spectrum of the original black titanium dioxide prepared of the present embodiment and hydrophilic black titanium dioxide, and both are all shown as Anatase, illustrates that the black titanium dioxide after hydrophilic modifying crystalline phase does not occur and changes.
Fig. 4 is the Raman collection of illustrative plates of the original black titanium dioxide prepared of the present embodiment and hydrophilic black titanium dioxide, both are all shown as Anatase, main Raman peak is not subjected to displacement, and reconfirms that crystalline phase change does not occur the black titanium dioxide after hydrophilic modifying.
Fig. 5 a is the DLS grain size distribution of the original black titanium dioxide prepared of the present embodiment and hydrophilic black titanium dioxide.After hydrophilic modifying described in figure, black titanium dioxide particle diameter reduces, distribution narrow, and distribution of peaks particle diameter is reduce 59nm from 124nm, and this is attributed to the role of tear of ultrasonic cell disrupte machine.
Fig. 5 b is the Zeta potential figure of the original black titanium dioxide prepared of the present embodiment and hydrophilic black titanium dioxide.After hydrophilic modifying described in figure, black titanium dioxide causes current potential to reduce due to Ti and amino coordination.
Fig. 6 is the FTIR collection of illustrative plates of the original black titanium dioxide prepared of the present embodiment and hydrophilic black titanium dioxide.There is Ti-N-O characteristic absorption peak in figure, illustrated that the Polyethylene Glycol that amino functional is rolled into a ball is successful to black titanium dioxide modification.
Fig. 7 is the UV-Vis collection of illustrative plates of variable concentrations hydrophilic black titanium dioxide prepared by the present embodiment.Black titanium dioxide described in figure to have a wider absorption near infrared light to UV light region, present full spectroscopic optics absorption characteristic.And along with concentration increases, absorbance increases thereupon.
Fig. 8 is that (C1 concentration is 0.16mgmL for the hydrophilic black titanium dioxide aqueous solution of variable concentrations prepared by the present embodiment
-1, C2 concentration is 0.64mg mL
-1) and water, at 808nm laser, (power density is 0.48W cm
-2) irradiate under thermal imaging picture.The solution of black titanium dioxide described in figure compares water, near infrared imaging effect highly significant.
Fig. 9 is the external photoacoustic imaging signal graph of variable concentrations hydrophilic black titanium dioxide aqueous solution prepared by the present embodiment.Figure cathetus be the photoacoustic signal value of variable concentrations black titanium dioxide aqueous solution under 808nm laser excitation along with concentration curve, illustration is the photoacoustic signal figure that variable concentrations hydrophilic black titanium dioxide is embedded in agar gel.Along with concentration increases, photoacoustic signal value linearly increases, and the photoacoustic signal brightness of agar gel increases.
Figure 10 is variable concentrations hydrophilic black titanium dioxide aqueous solution prepared by the present embodiment, and at 808nm laser, (power density is 1.41Wcm
-2) irradiate under heating curve.The aqueous solution of black titanium dioxide described in figure increases along with concentration, and the temperature of rising increases.
Figure 11 is hydrophilic black titanium dioxide prepared by the present embodiment, and at 808nm laser, (power density is 1.41Wcm
-2) irradiate the lower quantum yield curve producing singlet oxygen.Black titanium dioxide described in figure compares simple irradiating laser, the singlet oxygen content showed increased of generation.
In sum, the invention provides one simply, black titanium dioxide hydrophilic modification method efficiently.After hydrophilic modifying, this black titanium dioxide is significantly improved at the dispersibility of aqueous solution, stability and biocompatibility.Because it has full spectroscopic optics absorption characteristic, therefore, can be used as potential tumor diagnosis and treatment agent.The present invention has expanded the application of black titanium dioxide at biological field further.Adopt Same Wavelength laser excitation, four large performances can be realized simultaneously: one is be used as near infrared imaging contrast agent, for strengthening near infrared imaging contrast, improves image sensitivity and speed; Two is be used as photoacoustic imaging contrast agent, for strengthening photoacoustic imaging contrast, obtains contrast high, the photoacoustic imaging picture of clear picture; Three is can be used as photo-thermal therapy agent, for strengthening photo-thermal therapy effect, up hill and dale, fully ablated tumor; Four is produce singlet oxygen, can be used as a kind of novel photosensitizer for photodynamic therapy.This is significant for promoting the development of nano meter biomaterial in medical science.
Claims (10)
1. a black titanium dioxide tumor diagnosis and treatment agent, is characterized in that, described black titanium dioxide tumor diagnosis and treatment agent is polyethyleneglycol modified black titanium dioxide nano-particle.
2. black titanium dioxide tumor diagnosis and treatment agent according to claim 1, is characterized in that, the black titanium dioxide used in the described black titanium dioxide tumor diagnosis and treatment agent of preparation and the mass ratio of Polyethylene Glycol are 1:1 ~ 1:2.
3. black titanium dioxide tumor diagnosis and treatment agent according to claim 1 and 2, it is characterized in that, described Polyethylene Glycol is functional polyethylene glycol, and functionalization functional group is wherein at least one in amino, sulfydryl and carboxyl.
4. black titanium dioxide tumor diagnosis and treatment agent according to any one of claim 1 to 3, it is characterized in that, the hydration kinetics particle diameter of described black titanium dioxide tumor diagnosis and treatment agent is 50 ~ 70 nm, and the particle diameter of the black titanium dioxide in described black titanium dioxide tumor diagnosis and treatment agent is 20 ~ 30 nm.
5. black titanium dioxide tumor diagnosis and treatment agent according to any one of claim 1 to 4, is characterized in that, the black titanium dioxide in described black titanium dioxide tumor diagnosis and treatment agent is Anatase.
6. the preparation method of the black titanium dioxide tumor diagnosis and treatment agent according to any one of a claim 1 to 5, it is characterized in that, black titanium dioxide is dissolved in water, add functional polyethylene glycol, carry out ultrasonic with Aided Modification after mix homogeneously, described black titanium dioxide tumor diagnosis and treatment agent can be obtained.
7. preparation method according to claim 6, is characterized in that, the mass ratio of black titanium dioxide and functional polyethylene glycol is 1:1 ~ 1:2.
8. the preparation method according to claim 6 or 7, is characterized in that, described black titanium dioxide is the black titanium dioxide that thermit reduction obtains.
9. the preparation method according to any one of claim 6 to 8, is characterized in that, the described ultrasonic time is 0.5 ~ 2 hour, describedly ultrasonicly to carry out in ultrasonic cell disrupte machine under condition of ice bath.
10. the application of the black titanium dioxide tumor diagnosis and treatment agent according to any one of a claim 1 to 5 while preparing under near-infrared heat/optoacoustic Double-mode imaging guiding in photo-thermal/photodynamics nanometer diagnosis and treatment agent.
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| CN105125576A (en) * | 2015-09-23 | 2015-12-09 | 广东省第二人民医院 | Pharmaceutical composition containing titanium dioxide nanoparticles for preventing or treating cancer and application thereof |
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| CN108514636B (en) * | 2018-03-30 | 2021-04-20 | 张晗 | Nano titanium photo-thermal preparation based on titanium quantum dots and preparation method thereof |
| CN110448692A (en) * | 2018-05-08 | 2019-11-15 | 中国科学院宁波材料技术与工程研究所 | A kind of nanocomposite, preparation method and the application in HIFU synergist |
| CN110448692B (en) * | 2018-05-08 | 2022-06-21 | 中国科学院宁波材料技术与工程研究所 | Nano composite material, preparation method thereof and application of nano composite material in HIFU synergist |
| CN111359642A (en) * | 2020-03-17 | 2020-07-03 | 北京大学 | Semiconductor broad-spectrum bactericidal antiviral composite material, preparation method and preparation method |
| CN111359642B (en) * | 2020-03-17 | 2021-06-11 | 北京大学 | Semiconductor broad-spectrum bactericidal antiviral composite material, preparation method and preparation method |
| CN115845849A (en) * | 2022-11-24 | 2023-03-28 | 华东师范大学 | Ferrous ion doped black titanium dioxide nanosheet and preparation method thereof |
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