CN110694100B - Visual drug-loaded embolism microsphere based on liquid metal and preparation method thereof - Google Patents
Visual drug-loaded embolism microsphere based on liquid metal and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a liquid metal-based visual drug-loaded embolism microsphere and a preparation method thereof. The visual drug-loaded embolic microsphere comprises: the liquid metal, the chitosan aqueous solution and the anti-tumor drug are mixed according to the mass ratio of 1: (10-100): (0.5-2). The visual drug-loaded embolization microsphere is formed by crosslinking chitosan and a crosslinking agent by adopting a physical crosslinking method, and the method is mild in preparation condition and simple in operation. The particle size of the visual drug-loaded embolism microsphere is 10-700 mu m, the size is controllable, the biocompatibility is good, the drug-loading capacity is strong, the drug-loading spectrum is wide, and the sustained drug release and tumor vascular embolism can be realized. The invention also has the performance of developing under DSA fluoroscopy or CT and the like, is convenient for timely evaluating the curative effect and supplementing embolism, and can be used for supplementary TACE treatment of tumors.
Description
Technical Field
The invention belongs to the technical field of medical materials, and particularly relates to a liquid metal-based visual drug-loaded embolism microsphere and a preparation method thereof.
Background
Interventional therapy is a new field developed in recent years, is a minimally invasive medical technology guided by image equipment, and has the characteristics of small wound, quick recovery, good curative effect and the like. Transcatheter arterial embolization is an important technique for interventional therapy, in which embolization material is injected into the supply vessel of a diseased organ in a controlled manner so as to prevent blood flow, resulting in a lack of oxygen and nutrient supply to the tumor tissue portion, thereby achieving the purpose of treating tumor and removing the diseased organ.
At present, the embolization microspheres commonly used in clinic mainly comprise DC beads, HeaSphere, CalliSpheres and the like, but the embolization microspheres commonly have the problems of poor developing effect, small drug loading amount, single drug loading and the like.
Disclosure of Invention
In order to overcome the defects of the prior art and solve the problems of the existing drug-loaded embolization microspheres, the invention aims to provide a liquid metal-based visual drug-loaded embolization microsphere and a preparation method thereof. In addition, the visualized drug-loaded embolization microsphere has the characteristic of developing under DSA or CT, and is favorable for observing the embolization effect of the microsphere in a blood vessel in real time.
In order to achieve the purpose, the invention adopts the technical scheme that:
a visual drug-loaded embolism microsphere based on liquid metal comprises a chitosan material 1, liquid metal nanoparticles 2 wrapped by the chitosan material 1 and an anti-tumor drug 3. The chitosan material 1 has good biocompatibility, strong drug-loading capacity and wide drug-loading spectrum, and the liquid metal nanoparticles 2 represented by gallium have X-ray absorption coefficient not lower than that of common metals, so that in DSA shooting or CT scanning, the drug-loaded embolism microspheres based on liquid metal can form bright contrast with surrounding tissues, excellent developing effect is achieved, real-time evaluation of embolism effect is facilitated, and therefore the visual drug-loaded embolism microspheres can be used for vascular embolism in tumor adjuvant therapy and have good slow release effect.
The mass ratio of the liquid metal nanoparticles 2 to the chitosan material 1 to the antitumor drug 3 is 1: (10-100): (0.5-2).
The anti-tumor drug 3 is a small-molecule anti-tumor drug, an anti-tumor angiogenesis drug or an immunotherapy drug, and the small-molecule anti-tumor drug is adriamycin, methotrexate or gemcitabine; the anti-tumor angiogenesis drug is bevacizumab, ramucirumab, apatinib, sorafenib, sunitinib, axitinib or pazopanib; the immunotherapy drug is PD-1 immunotherapy agent, IDO inhibitor, arginase inhibitor, adenosine A2AReceptor antagonists, ROR gamma T agonists, chemokine receptor inhibitors, transforming growth factor beta (TGF-beta), T cell activatedImmunoglobulin inhibits one or more of a type V domain (VISTA) inhibitor, a sting agonist, a Toll-like receptor agonist.
The liquid metal is selected from liquid metal with a melting point close to room temperature, such as liquid metal with a melting point of 15-30 ℃, and preferably a gallium simple substance or gallium-based alloy, such as gallium-indium alloy.
The invention also provides a preparation method of the visible medicine-carrying embolism microsphere based on the liquid metal, which comprises the following steps:
(1) preparing a liquid metal nanoparticle solution: adding liquid metal into the chitosan aqueous solution, performing ultrasonic dispersion, and centrifuging to remove large particles to prepare a nano-form uniformly dispersed liquid metal nanoparticle solution;
(2) preparing a liquid metal-based visual drug-loaded embolism microsphere: adding the chitosan aqueous solution and the dispersing agent into the oil phase, stirring, adding the uniformly dispersed liquid metal nanoparticle solution and the anti-tumor drug, stirring, and finally adding the cross-linking agent dissolved in the water phase for reaction.
In the step (1), ultrasonic dispersion is carried out for more than 10min to obtain nanoscale liquid metal particles with the particle size of 500-800 nm; in the step (2), the temperature is set to be 30-40 ℃, the stirring speed is 100-1000 rpm, and the reaction is carried out for 0.5-2 h after the cross-linking agent is added.
In the steps (1) and (2), the mass concentration of the chitosan aqueous solution is 1-5%, the dosage ratio is 1: 2-4, and the mass ratio of the liquid metal nanoparticles (2), the chitosan material (1) and the antitumor drug (3) used in the whole process is 1: (10-100): (0.5-2).
In the step (2), the temperature is set to be 30-40 ℃, the stirring speed is 100-1000 rpm, and the reaction is carried out for 0.5-2 h after the cross-linking agent is added.
In the step (2), the dispersant is sorbitan fatty acid ester and is used in an amount of about 0.1 part by weight; the cross-linking agent is sodium tripolyphosphate, genipin or beta-sodium glycerophosphate, the concentration is 0.1g/mL, and the dosage is 0.1-1 part by weight.
And (3) after the step (2), centrifuging the obtained microspheres to remove the reaction solvent, washing the microspheres with solvents such as water, ether, ethanol and the like for many times, removing the cross-linking agent and the dispersing agent, and drying the microspheres for later use.
The method for vascular embolization in tumor adjuvant therapy comprises the following steps: the visual medicine-carrying embolism microsphere is injected into tumor blood vessels through a catheter to block the tumor blood vessels, so that the oxygen and nutrient supply of the tumor tissues by blood flow is prevented. The visualized drug-loaded embolization microsphere has the characteristic of developing under DSA or CT, and is favorable for observing the embolization effect of the microsphere in a blood vessel in real time.
Compared with the prior art, the invention adopts chitosan as the wrapping material of the liquid metal and the anti-tumor drug, the prepared microsphere has excellent biocompatibility, more importantly, the liquid metal has the characteristic of developing under DSA or CT, and is more beneficial to judging the position, distribution condition, embolism effect and the like of the microsphere in the blood vessel in the using process.
Drawings
Fig. 1 is a schematic structural diagram of a visualized drug-loaded embolization microsphere according to the present invention.
In the figure: 1 is chitosan material, 2 is liquid metal nano-particles, and 3 is anti-tumor drug.
Detailed Description
The following detailed description of the embodiments of the present invention is provided with reference to the drawings and examples, but not intended to limit the scope of the invention.
A visualized medicine-carrying embolism microsphere based on liquid metal is prepared from the following components in parts by weight: 1 part of liquid metal (EGaIn, the mass ratio of metal gallium to metal indium is 75.5:24.5), 50 parts of chitosan aqueous solution and 1 part of anti-tumor drug, wherein the obtained product is solid powder, and as shown in figure 1, liquid metal nanoparticles 2 and anti-tumor drug 3 are wrapped by solid chitosan material 1.
The preparation method comprises the following steps:
(1) preparing a liquid metal nano solution: adding 1g of liquid metal into 50ml of chitosan aqueous solution, performing ultrasonic dispersion, and centrifuging to remove large particles to prepare a nano-form uniformly dispersed liquid metal nanoparticle solution, wherein the concentration of the liquid metal is 0.02 g/ml.
(2) Preparing a liquid metal-based visual drug-loaded embolism microsphere: firstly adding a chitosan aqueous solution and a dispersing agent into an oil phase, stirring at the set temperature of 30 ℃ and the stirring speed of 100rpm, then adding a uniformly dispersed liquid metal nanoparticle solution and an antitumor drug adriamycin into the solution, stirring at the set temperature of 30 ℃ and the stirring speed of 100rpm, finally dissolving a cross-linking agent into a water phase, adding the water phase into the solution, setting the temperature of 30 ℃, and stirring for reaction for 1 h.
(3) Centrifuging the microspheres obtained in the step (2) to remove the reaction solvent, washing the microspheres with solvents such as water, ether and ethanol for many times to remove the cross-linking agent and the dispersing agent, and drying the microspheres for 48 hours at 37 ℃ for later use.
In the method, a physical crosslinking method is adopted, chitosan and a crosslinking agent are used for crosslinking to form the microsphere, the preparation condition is mild, the operation is simple, the particle size of the obtained visual drug-loaded embolism microsphere is 10-700 mu m, and the size of the microsphere can be controlled by the stirring rate in the microsphere preparation process.
The prepared visual drug-loaded embolization microsphere is injected into a tumor blood vessel through a catheter in a rabbit liver cancer model, on one hand, the microsphere can carry out blood vessel embolization and prevent the blood from flowing to supply oxygen and nutrients to tumor tissues; on the other hand, the anti-tumor drug carried in the microspheres can be slowly released into tumor tissues to kill tumor cells. The microsphere can be used for the synergistic treatment of tumor embolism and chemotherapy. After the microsphere treatment, part of tumor cells can be killed or tumor tissues can be subjected to ischemic necrosis.
In addition, the visualized drug-loaded embolism microsphere has the characteristic of DSA (digital radiography) fluoroscopy or CT (computed tomography) visualization, and is favorable for observing the embolism position and the embolism condition of the microsphere in a blood vessel in real time, evaluating the curative effect in real time and supplementing embolism. Meanwhile, the drug-loaded microspheres can slowly release anti-tumor drugs in blood vessels to assist in embolization treatment of tumors.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (9)
1. The visible drug-loaded embolism microsphere based on the liquid metal is characterized by comprising a chitosan material (1), liquid metal nanoparticles (2) and anti-tumor drugs (3), wherein the liquid metal nanoparticles (2) are wrapped by the chitosan material (1), the liquid metal nanoparticles (2) are nanoscale, the particle size diameter is 500-800nm, and the mass ratio of the liquid metal nanoparticles (2), the chitosan material (1) and the anti-tumor drugs (3) is 1: (10-100): (0.5-2).
2. The liquid metal-based visual drug-loaded embolic microsphere of claim 1, wherein the anti-tumor drug (3) is a small molecule anti-tumor drug, an anti-tumor angiogenesis drug or an immunotherapy drug, and the small molecule anti-tumor drug is doxorubicin, methotrexate or gemcitabine; the anti-tumor angiogenesis drug is bevacizumab, ramucirumab, apatinib, sorafenib, sunitinib, axitinib or pazopanib; the immunotherapy drug is PD-1 immunotherapy agent, IDO inhibitor, arginase inhibitor, adenosine A2AReceptor antagonists, ROR γ T agonists, chemokine receptor inhibitors, transforming growth factor beta (TGF- β), inhibitors of the immunoglobulin suppressor type V domain of T cell activation (VISTA), sting agonists, Toll-like receptor agonists.
3. The liquid metal-based visual drug-loaded embolization microsphere according to claim 1, wherein the liquid metal is selected from liquid metals with a melting point of 15-30 ℃.
4. The visible drug-loaded embolic microsphere based on liquid metal of claim 1, wherein the liquid metal is elemental gallium or an alloy based on gallium.
5. The preparation method of the visible medicine-carrying embolism microsphere based on the liquid metal is characterized by comprising the following steps:
(1) preparing a liquid metal nanoparticle solution: adding liquid metal into the chitosan aqueous solution, performing ultrasonic dispersion, and centrifuging to remove large particles to prepare a nano-form uniformly dispersed liquid metal nanoparticle solution;
(2) preparing a liquid metal-based visual drug-loaded embolism microsphere: adding the chitosan aqueous solution and the dispersing agent into the oil phase, stirring, adding the uniformly dispersed liquid metal nanoparticle solution and the anti-tumor drug, stirring, and finally adding the cross-linking agent dissolved in the water phase for reaction.
6. The preparation method of the visualized medicine-carrying embolism microsphere based on the liquid metal as claimed in claim 5, wherein in the step (1), the liquid metal particles with the size of 500-800nm are obtained by ultrasonic dispersion for more than 10 min; in the step (2), the temperature is set to be 30-40 ℃, the stirring speed is 100-1000 rpm, and the reaction is carried out for 0.5-2 h after the cross-linking agent is added.
7. The preparation method of the visible medicine-carrying embolism microsphere based on the liquid metal as claimed in claim 5, wherein in the steps (1) and (2), the chitosan aqueous solution has a mass concentration of 1-5%, the dosage ratio is 1: 2-4, and the liquid metal nanoparticles (2), the chitosan material (1) and the antitumor drug (3) used in the whole process have a mass ratio of 1: (10-100): (0.5-2).
8. The preparation method of the visible medicine-carrying embolism microsphere based on the liquid metal as claimed in claim 7, wherein in the step (2), the dispersant is sorbitan fatty acid ester, and the amount is 0.1 part by weight; the cross-linking agent is sodium tripolyphosphate, genipin or beta-sodium glycerophosphate, the concentration is 0.1g/mL, and the dosage is 0.1-1 part by weight.
9. The preparation method of the visible medicine-carrying embolism microsphere based on the liquid metal as claimed in claim 8, wherein after the step (2), the obtained microsphere is centrifuged to remove the reaction solvent, washed with water, ether and ethanol for multiple times to remove the cross-linking agent and the dispersing agent, and dried for later use.
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| CN113501860B (en) * | 2020-03-24 | 2023-06-16 | 国家纳米科学中心 | Assembled nano liquid metal particles and preparation method and application thereof |
| CN112043859A (en) * | 2020-09-10 | 2020-12-08 | 穆永旭 | Visual composite microsphere for embolism and preparation method thereof |
| CN118215510A (en) * | 2021-11-12 | 2024-06-18 | 重庆百迈腾世医药科技有限公司 | Active metal microsphere and composite embolic agent based on active metal microsphere |
| CN114933867B (en) * | 2022-04-28 | 2023-03-10 | 北京航空航天大学 | Anisotropic conductive adhesive based on liquid metal-porous microsphere skeleton and preparation method thereof |
| CN116077711A (en) * | 2022-11-09 | 2023-05-09 | 北京航空航天大学 | Liquid metal embolic agent |
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| CN1607033A (en) * | 2003-10-15 | 2005-04-20 | 中国科学院过程工程研究所 | Chitose microsphere and microcapsule with uniform size and its preparation method |
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