CN109125727A - A kind of preparation method of the nanocomposite based on poly-dopamine@graphene targeting-photo-thermal-light power synergistic treatment - Google Patents

A kind of preparation method of the nanocomposite based on poly-dopamine@graphene targeting-photo-thermal-light power synergistic treatment Download PDF

Info

Publication number
CN109125727A
CN109125727A CN201811041230.7A CN201811041230A CN109125727A CN 109125727 A CN109125727 A CN 109125727A CN 201811041230 A CN201811041230 A CN 201811041230A CN 109125727 A CN109125727 A CN 109125727A
Authority
CN
China
Prior art keywords
dopamine
poly
graphene
solution
targeting
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201811041230.7A
Other languages
Chinese (zh)
Inventor
王秉
姚舒婷
陈碧玲
胡锦华
万军民
胡智文
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Zhejiang Sci Tech University ZSTU
Zhejiang University of Science and Technology ZUST
Original Assignee
Zhejiang Sci Tech University ZSTU
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Zhejiang Sci Tech University ZSTU filed Critical Zhejiang Sci Tech University ZSTU
Priority to CN201811041230.7A priority Critical patent/CN109125727A/en
Publication of CN109125727A publication Critical patent/CN109125727A/en
Pending legal-status Critical Current

Links

Classifications

    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K41/00Medicinal preparations obtained by treating materials with wave energy or particle radiation ; Therapies using these preparations
    • A61K41/0052Thermotherapy; Hyperthermia; Magnetic induction; Induction heating therapy
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K41/00Medicinal preparations obtained by treating materials with wave energy or particle radiation ; Therapies using these preparations
    • A61K41/0057Photodynamic therapy with a photosensitizer, i.e. agent able to produce reactive oxygen species upon exposure to light or radiation, e.g. UV or visible light; photocleavage of nucleic acids with an agent
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/02Inorganic compounds
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/06Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
    • A61K47/22Heterocyclic compounds, e.g. ascorbic acid, tocopherol or pyrrolidones
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/30Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
    • A61K47/34Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polyesters, polyamino acids, polysiloxanes, polyphosphazines, copolymers of polyalkylene glycol or poloxamers
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P35/00Antineoplastic agents

Abstract

The present invention relates to pharmaceutical fields, disclose a kind of preparation method of nanocomposite based on poly-dopamine@graphene targeting-photo-thermal-light power synergistic treatment.The present invention passes through reaction synthesis poly-dopamine@graphene between graphene and poly-dopamine first;Then poly-dopamine@graphene reacts to obtain folic acid-poly-dopamine@graphene with folic acid, 1- ethyl-(3- dimethylamino-propyl) carbodiimides, nitrogen-HOSu NHS;Last and hypericin, 1- ethyl-(3- dimethylaminopropyl) carbodiimide hydrochloride and 4-dimethylaminopyridine react to obtain final goal object.The polymer material of this method preparation will can realize targeted therapy in the later period, and the synergistic effect of tumor thermotherapy and chemotherapy increases the stability of polymer material, be expected to be used for cancer cell treatment;This method will not make a significant impact cell in the experimentation in later period simultaneously, not influence the science of experimental result.

Description

A kind of receiving based on poly-dopamine@graphene targeting-photo-thermal-light power synergistic treatment The preparation method of nano composite material
Technical field
The present invention relates to pharmaceutical fields, more particularly to a kind of poly-dopamine@graphene targeting-photo-thermal-light power that is based on to assist With the preparation method of the nanocomposite for the treatment of.
Background technique
Cancer (malignant tumour) is one of the refractory disease for seriously endangering human health, every year disease incidence all with higher And the death rate.Therefore, tumour is formed and the research for the treatment of method, oneself current warp becomes the research emphasis and heat of researcher Point.In recent years, the biomedical treatment for being combined into cancer with nanotechnology brings new opportunities.With unique optics, magnetic The Nano medication of the physicochemical properties such as, electricity and acoustics brings new approaches for the prevention of major disease, diagnosing and treating.Its In, polymer nano material has excellent biocompatibility and degradability, programmable size and surface property, higher load Dose and drug delivery efficiency, good cyclical stability and EPR effect are realized high to improve the bioavilability of drug The drug targeting of effect and control release.Therefore, nowadays polymer nano material is widely used in drug delivery system.
How extensive use with polymer nano material as pharmaceutical carrier in terms of biological medicine, allow polymer nano Rice material has both the synergistic effect of targeting, tumor thermotherapy and chemotherapy simultaneously, improves it in drug targeting and metabolic stability side The problems such as deficiency in face, has become focus of attention.At the same time, various multifunctional polymer nano materials are as a kind of drug Delivery vehicles, will not only be such that the toxicity of drug minimizes, and also improve its stability and the retention time at required position.Cause This, it is extremely urgent to study polymer nano material that is a kind of while having both targeting, tumor thermotherapy and chemotherapy synergistic effect.
Summary of the invention
In order to solve the above-mentioned technical problems, the present invention provides one kind to be based on poly-dopamine@graphene targeting-photo-thermal-light The preparation method of the nanocomposite of power synergistic treatment.The present invention, which passes through to react between graphene and poly-dopamine first, to close At poly-dopamine@graphene;Then poly-dopamine@graphene and folic acid, two Asia of 1- ethyl-(3- dimethylamino-propyl) carbonization Amine, nitrogen-HOSu NHS react to obtain folic acid-poly-dopamine@graphene;Last and hypericin, 1- ethyl-(3- bis- Dimethylaminopropyl) carbodiimide hydrochloride and 4-dimethylaminopyridine react to obtain final goal object.This method preparation Polymer material will can realize targeted therapy in the later period, and the synergistic effect of tumor thermotherapy and chemotherapy increases the steady of polymer material It is qualitative, it is expected to be used for cancer cell treatment;This method will not make a significant impact cell in the experimentation in later period simultaneously, no The science of experimental result is influenced, experimental implementation process is simple, nontoxic, harmless, environmentally protective.
The specific technical proposal of the invention is: a kind of controlled based on the collaboration of poly-dopamine@graphene targeting-photo-thermal-light power The preparation method of the nanocomposite for the treatment of, in terms of mg and mL, comprising the following steps:
1) by graphene dispersion in the aqueous dopamine solution of 0.5-1.5mg/mL, it is ultrasonically treated 3 ~ 5min, it is spare.
2) the Tris buffer of pH=8.5 10mL is added rapidly in the solution that step 1) obtains, and connected at room temperature Continuous stirring 8-12h obtains the graphene of poly-dopamine mediation, i.e. poly-dopamine@stone then by centrifugation, washing, freeze-drying Black alkene, it is spare.
In step 2, dopamine and graphite alkene reaction are obtained into poly-dopamine graphene, its bio-compatible can be improved Property, itself toxicity is reduced, improves its pharmacokinetics behavior and improves itself and cell-interacting capabilities.
3) 100 ~ 150 mg poly-dopamine@graphenes are weighed, are dispersed in 80-120mL deionized water, ultrasonic disperse is equal It is even, 5 ~ 7 g sodium hydroxides, 5 ~ 7 g sodium hypochlorite, ultra sonic bath 1-3 h, by the hydroxyl on poly-dopamine@graphene sheet layer is added It is converted into carboxyl;After fully reacting, is neutralized with dilute hydrochloric acid and is rinsed repeatedly, by centrifugal treating, collect the dark solution on upper layer, And with deionized water dialysis 40-50 h, unreacted water-soluble substances are removed.
In step 3), by poly-dopamine@graphene and sodium hydroxide, sodium hypochlorite reaction, make poly-dopamine@graphene On hydroxyl be converted into carboxyl, be conducive to next react with the amino on folic acid;It is to protect using dilute hydrochloric acid washing Card sample is always neutral;Dialysis treatment is concentration and the higher solution of purity in order to obtain.
4) 0.5 ~ 0.8 g folic acid is added into the solution that step 3) obtains, ultrasonic disperse is uniform, while stirring to addition 125 ~ 127 mg 1- ethyls-(3- dimethylamino-propyl) carbodiimides and 182.5 ~ 184.5 mg nitrogen-hydroxysuccinimidyl acyl are sub- Amine, carries out dialysis treatment with the sodium bicarbonate solution of pH=8 after 2 ~ 3 h of ultrasound, and every 3-5h changes a water, completes after 40-50h saturating Analysis, obtains dark solution.
In step 4), 1- ethyl-(3- dimethylamino-propyl) carbodiimides and nitrogen-HOSu NHS conduct Crosslinking agent acts on to activate poly-dopamine@graphene, reacts it sufficiently with folic acid, micro- by the way that folic acid is connected to polymer Grain surface, increases its associativity with receptor, the polymer particles of carrying medicament is made largely to be gathered in subject cell surface;It uses Sodium bicarbonate is to guarantee that solution is in neutrallty condition as dialyzate.
5) it using the moisture in rotary evaporation removal dark solution, is washed, and is placed at 40 ~ 50 DEG C repeatedly with acetone Vacuum drying obtains the poly-dopamine@graphene of modified with folic acid, remembers folic acid-poly-dopamine@graphene, spare.
In step 5), being washed repeatedly using acetone is to be close to synthetic environment to reduce solution zeta current potential.
6) take 64.8 ~ 66.8mg folic acid-poly-dopamine@graphene, be dispersed in 40-60mL deionization, then plus Enter 6.05 ~ 6.25mg hypericin, 2.76 ~ 2.96mg 1- ethyl-(3- dimethylaminopropyl) carbodiimide hydrochloride and 0.30 ~ 0.32mg 4-dimethylaminopyridine is stirred to react overnight.
In step 6), 1- ethyl-(3- dimethylamino joined in the reaction of folic acid-fluorinated graphene and hypericin Base propyl) carbodiimide hydrochloride and 4-dimethylaminopyridine, wherein 1- ethyl-(3- dimethylaminopropyl) carbonization two is sub- Amine hydrochlorate is as polypeptide condensing agent and crosslinking agent, it can be achieved that quickly polypeptide condensation reaction;4-dimethylaminopyridine has higher Catalytic capability, yield can be significantly improved.
7) solution that step 6) obtains is filtered using super filter tube, using freeze-drying, is obtained based on poly-dopamine@stone The nanocomposite of black alkene targeting-photo-thermal-light power synergistic treatment.
Preferably, in step 1), ultrasonic procedure are as follows: ultrasonic grinder is used, it is ultrasonically treated 3 under 500 W power ~ 5min。
Preferably, in step 2, centrifugation, washing, freezing dry process are as follows: high-speed refrigerated centrifuge is used, 8000 ~ 10 ~ 15 min are centrifuged under conditions of 10000r/min;Then it is washed with deionized repeatedly, then is placed in freeze drier and freezes It is dried to obtain poly-dopamine@graphene.
Preferably, acquired solution is pre-chilled before use, being placed in 3 ~ 5 DEG C of environment in step 6).
Preferably, in step 7), filtering, the concrete operations being freeze-dried are as follows: be centrifuged by 100 kDa screen pipes molten Then liquid repeatedly washs filtrate with deionized water to remove excessive hypericin, finally carry out freeze-drying process.
It is compared with the prior art, the beneficial effects of the present invention are:
1. obtaining poly-dopamine@graphene by being modified processing to graphene, poly-dopamine, which has, to be mentioned in step 2 Its high biocompatibility, reduces itself toxicity, improves its pharmacokinetics behavior and improve itself and cell-interacting capabilities etc. Advantage.
2. being reacted by poly-dopamine@graphene and sodium hydroxide, sodium hypochlorite makes poly- DOPA in step 3) Hydroxyl on amine@graphene is converted into carboxyl, guarantees that it is sufficiently reacted with folic acid.
4., by the way that folic acid is connected to surface of polymer material, increasing its associativity with receptor in step 4), making The polymer particles of carrying medicament are largely gathered in subject cell surface, thus increase the drug concentration of site of action, reduction pair The toxic side effect of normal cell.
5. the solution of preparation being placed in 3 ~ 5 DEG C of environment and being pre-chilled, avoid the shadow to subsequent experimental in step 6) It rings, improves the success rate of experiment.
6. will can be obtained after the poly-dopamine graphite alkene reaction of hypericin and modified with folic acid a kind of poly- in step 7) Object nano material is closed, wherein hypericin has photo-activity as a kind of photosensitizer, can be by destroying in tissue and cell Organelle, finally cause the death of cancer cell, achieve the purpose that treating cancer.
7. in the present invention, can realize efficient tumor thermotherapy and chemotherapy collaboration effect by preparing polymer nano material It answers, increases the stability of drug, realize active targeting, increase the binding ability with receptor, to greatly promote to cancer cell Therapeutic effect.
8. the present invention is by constructing a kind of safety, non-toxic, and is capable of the pharmaceutical carrier of efficient transportation photosensitizer, energy The stability of drug is improved, enough convenient for storage.
Specific embodiment
The present invention will be further described with reference to the examples below.
Embodiment 1:
1) by graphene dispersion in the aqueous solution of dopamine (1mg/mL), ultrasonication 3min, spare at 500 W;
2) 10mL Tris buffer (10mM, pH=8.5) is added rapidly in the solution that step 1) obtains, and by it in room temperature Under the conditions of continuously stir 10h.Then the graphite of poly-dopamine mediation can be obtained by operations such as centrifugation, washing, freeze-dryings Alkene, i.e. poly-dopamine@graphene, it is spare.Wherein, centrifugal rotational speed 8000r/min, centrifugation time are 10 min;
3) 100 mg poly-dopamine@graphenes are weighed, are dispersed in 100 mL deionized waters, ultrasonic 3min makes it be uniformly dispersed, Then 5 g sodium hydroxides, 5 g sodium hypochlorite are added, 2 h of ultra sonic bath converts the hydroxyl on poly-dopamine@graphene sheet layer to Carboxyl.After fully reacting, is neutralized and rinsed repeatedly, 15 min of centrifugal treating at 12000 r/min with dilute hydrochloric acid, collect upper layer Dark solution remove unreacted water-soluble substances and with 48 h of deionized water dialysis;
4) 0.5 g folic acid is added into the solution that step 3) obtains, 1 min of ultrasound makes it be uniformly dispersed, while stirring to mixing 125 mg1- ethyls-(3- dimethylamino-propyl) carbodiimides and 182.5 mg nitrogen-HOSu NHS are added in object, Dialysis treatment is carried out using sodium bicarbonate solution (pH=8) after 2 h of ultrasound, every 4 h changes a water, completes dialysis after 48 h, obtain Dark solution;
5) moisture in the solution that step 4) obtains is removed using rotary evaporation, is washed repeatedly with acetone, and is placed on 40 DEG C It is dry in vacuum oven, the poly-dopamine@graphene of modified with folic acid is obtained, remembers folic acid-poly-dopamine@graphene, it is spare;
6) folic acid for taking 64.8mg step 5) to obtain-poly-dopamine@graphene, is dispersed in 50mL deionization, then plus Enter 6.05mg hypericin, 2.76mg 1- ethyl-(3- dimethylaminopropyl) carbodiimide hydrochloride and 0.30mg 4- Dimethylamino naphthyridine is stirred to react overnight, and is placed in 4 DEG C of environment and is pre-chilled;
7) solution for obtaining step 6) is centrifuged solution by 100 kDa screen pipes and is then spent with removing excessive hypericin Ionized water repeatedly washs filtrate, finally carries out freeze-drying process, obtains final product.
Embodiment 2:
1) by graphene dispersion in the aqueous solution of dopamine (1mg/mL), 4 min of ultrasonication, spare at 500 W;
2) 10mL Tris buffer (10mM, pH=8.5) is added rapidly in the solution that step 1) obtains, and by it in room temperature Under the conditions of continuously stir 10h.Then the graphite of poly-dopamine mediation can be obtained by operations such as centrifugation, washing, freeze-dryings Alkene, i.e. poly-dopamine@graphene, it is spare.Wherein, centrifugal rotational speed 9000r/min, centrifugation time are 10 min;
3) 125 mg poly-dopamine@graphenes are weighed, are dispersed in 100 mL deionized waters, 4 min of ultrasound keep its dispersion equal It is even, 6 g sodium hydroxides, 6 g sodium hypochlorite are then added, 2 h of ultra sonic bath turns the hydroxyl on poly-dopamine@graphene sheet layer Turn to carboxyl.After fully reacting, is neutralized and rinsed repeatedly, 15 min of centrifugal treating at 13000 r/min with dilute hydrochloric acid, collected The dark solution on upper layer, and with 48 h of deionized water dialysis, remove unreacted water-soluble substances;
4) 0.6 g folic acid is added into the solution that step 3) obtains, 2 min of ultrasound make it be uniformly dispersed, while stirring to mixing 126 mg1- ethyls-(3- dimethylamino-propyl) carbodiimides and 183.5 mg nitrogen-HOSu NHS are added in object, Dialysis treatment is carried out using sodium bicarbonate solution (pH=8) after 3 h of ultrasound, every 4 h changes a water, completes dialysis after 48 h, obtain Dark solution;
5) moisture in the solution that step 4) obtains is removed using rotary evaporation, is washed repeatedly with acetone, and is placed on 45 DEG C It is dry in vacuum oven, the poly-dopamine@graphene of modified with folic acid is obtained, remembers folic acid-poly-dopamine@graphene, it is spare;
6) folic acid for taking 65.8mg step 5) to obtain-poly-dopamine@graphene, is dispersed in 50mL deionization, then plus Enter 6.15mg hypericin, 2.86mg 1- ethyl-(3- dimethylaminopropyl) carbodiimide hydrochloride and 0.31 mg 4- Dimethylamino naphthyridine is stirred to react overnight, and is placed in 35 DEG C of environment and is pre-chilled;
7) solution for obtaining step 6) is centrifuged solution by 100 kDa screen pipes and is then spent with removing excessive hypericin Ionized water repeatedly washs filtrate, finally carries out freeze-drying process, obtains final product.
Embodiment 3:
1) by graphene dispersion in the aqueous solution of dopamine (1mg/mL), ultrasonication 5min, spare at 500 W;
2) 10mL Tris buffer (10mM, pH=8.5) is added rapidly in the solution that step 1) obtains, and by it in room temperature Under the conditions of continuously stir 10h.Then the graphite of poly-dopamine mediation can be obtained by operations such as centrifugation, washing, freeze-dryings Alkene, i.e. poly-dopamine@graphene, it is spare.Wherein, centrifugal rotational speed 10000r/min, centrifugation time are 15 min;
3) 150 mg poly-dopamine@graphenes are weighed, are dispersed in 100 mL deionized waters, ultrasonic 5min makes it be uniformly dispersed, Then 7 g sodium hydroxides, 7 g sodium hypochlorite are added, 2 h of ultra sonic bath converts the hydroxyl on poly-dopamine@graphene sheet layer to Carboxyl.After fully reacting, is neutralized and rinsed repeatedly, 20 min of centrifugal treating at 13000 r/min with dilute hydrochloric acid, collect upper layer Dark solution remove unreacted water-soluble substances and with 48 h of deionized water dialysis;
4) 0.8 g folic acid is added into the solution that step 3) obtains, 2 min of ultrasound make it be uniformly dispersed, while stirring to mixing 127 mg1- ethyls-(3- dimethylamino-propyl) carbodiimides and 184.5 mg nitrogen-HOSu NHS are added in object, Dialysis treatment is carried out using sodium bicarbonate solution (PH=8) after 3 h of ultrasound, every 4 h changes a water, completes dialysis after 48 h, obtain Dark solution;
5) moisture in the solution that step 4) obtains is removed using rotary evaporation, is washed repeatedly with acetone, and is placed on 50 DEG C It is dry in vacuum oven, the poly-dopamine@graphene of modified with folic acid is obtained, remembers folic acid-poly-dopamine@graphene, it is spare;
6) folic acid for taking 66.8mg step 5) to obtain-poly-dopamine@graphene, is dispersed in 50mL deionization, then plus Enter 6.25mg hypericin, 2.96mg 1- ethyl-(3- dimethylaminopropyl) carbodiimide hydrochloride and 0.32mg 4- Dimethylamino naphthyridine is stirred to react overnight, and is placed in 5 DEG C of environment and is pre-chilled;
7) solution for obtaining step 6) is centrifuged solution by 100 kDa screen pipes and is then spent with removing excessive hypericin Ionized water repeatedly washs filtrate, finally carries out freeze-drying process, obtains final product.
Raw materials used in the present invention, equipment is unless otherwise noted the common raw material, equipment of this field;In the present invention Method therefor is unless otherwise noted the conventional method of this field.
The above is only presently preferred embodiments of the present invention, is not intended to limit the invention in any way, it is all according to the present invention Technical spirit any simple modification, change and equivalent transformation to the above embodiments, still fall within the technology of the present invention side The protection scope of case.

Claims (5)

1. a kind of preparation side of the nanocomposite based on poly-dopamine@graphene targeting-photo-thermal-light power synergistic treatment Method, which is characterized in that in terms of mg and mL, comprising the following steps:
1) by graphene dispersion in the aqueous dopamine solution of 0.5-1.5mg/mL, it is ultrasonically treated 3 ~ 5min, it is spare;
2) the Tris buffer of pH=8.5 10mL is added rapidly in the solution that step 1) obtains, and continuously stirred at room temperature 8-12h is mixed, then by centrifugation, washing, freeze-drying, obtains the graphene of poly-dopamine mediation, i.e. poly-dopamine@graphite Alkene, it is spare;
3) 100 ~ 150 mg poly-dopamine@graphenes are weighed, are dispersed in 80-120mL deionized water, ultrasonic disperse is uniform, adds Enter 5 ~ 7 g sodium hydroxides, 5 ~ 7 g sodium hypochlorite, ultra sonic bath 1-3 h converts the hydroxyl on poly-dopamine@graphene sheet layer to Carboxyl;After fully reacting, is neutralized with dilute hydrochloric acid and rinsed repeatedly, by centrifugal treating, collect the dark solution on upper layer, and spend Ionized water dialysis 40-50 h, removes unreacted water-soluble substances;
4) into the solution that step 3) obtains be added 0.5 ~ 0.8 g folic acid, ultrasonic disperse is uniform, while stirring to be added 125 ~ 127 mg 1- ethyls-(3- dimethylamino-propyl) carbodiimides and 182.5 ~ 184.5 mg nitrogen-HOSu NHS surpass Dialysis treatment is carried out with the sodium bicarbonate solution of pH=8 after 2 ~ 3 h of sound, every 3-5h changes a water, completes dialysis after 40-50h, obtain Dark solution;
5) it using the moisture in rotary evaporation removal dark solution, is washed repeatedly with acetone, and is placed on vacuum at 40 ~ 50 DEG C It is dry, the poly-dopamine@graphene of modified with folic acid is obtained, remembers folic acid-poly-dopamine@graphene, it is spare;
6) 64.8 ~ 66.8mg folic acid-poly-dopamine@graphene is taken, is dispersed in 40-60mL deionization, is then added 6.05 ~ 6.25mg hypericin, 2.76 ~ 2.96mg 1- ethyl-(3- dimethylaminopropyl) carbodiimide hydrochloride and 0.30 ~ 0.32mg 4-dimethylaminopyridine is stirred to react overnight;
7) solution that step 6) obtains is filtered using super filter tube, using freeze-drying, is obtained based on poly-dopamine@graphene Targeting-photo-thermal-light power synergistic treatment nanocomposite.
2. a kind of nanometer based on poly-dopamine@graphene targeting-photo-thermal-light power synergistic treatment as described in claim 1 The preparation method of composite material, which is characterized in that in step 1), ultrasonic procedure are as follows: ultrasonic grinder is used, in 500 W function 3 ~ 5min is ultrasonically treated under rate.
3. a kind of nanometer based on poly-dopamine@graphene targeting-photo-thermal-light power synergistic treatment as described in claim 1 The preparation method of composite material, which is characterized in that in step 2, centrifugation, washing, freezing dry process are as follows: use freezing high speed Centrifuge is centrifuged 10 ~ 15 min under conditions of 8000 ~ 10000r/min;Then it is washed with deionized repeatedly, then is placed in cold Freeze-drying obtains poly-dopamine@graphene in lyophilizer.
4. a kind of nanometer based on poly-dopamine@graphene targeting-photo-thermal-light power synergistic treatment as described in claim 1 The preparation method of composite material, which is characterized in that acquired solution is pre-chilled before use, being placed in 3 ~ 5 DEG C of environment in step 6).
5. a kind of nanometer based on poly-dopamine@graphene targeting-photo-thermal-light power synergistic treatment described in claim 1 is multiple The preparation method of condensation material, which is characterized in that in step 7), filtering, the concrete operations being freeze-dried are as follows: pass through 100 kDa mistakes Chimney filter is centrifuged solution and then repeatedly washs filtrate with deionized water to remove excessive hypericin, finally carries out at freeze-drying Reason.
CN201811041230.7A 2018-09-07 2018-09-07 A kind of preparation method of the nanocomposite based on poly-dopamine@graphene targeting-photo-thermal-light power synergistic treatment Pending CN109125727A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811041230.7A CN109125727A (en) 2018-09-07 2018-09-07 A kind of preparation method of the nanocomposite based on poly-dopamine@graphene targeting-photo-thermal-light power synergistic treatment

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811041230.7A CN109125727A (en) 2018-09-07 2018-09-07 A kind of preparation method of the nanocomposite based on poly-dopamine@graphene targeting-photo-thermal-light power synergistic treatment

Publications (1)

Publication Number Publication Date
CN109125727A true CN109125727A (en) 2019-01-04

Family

ID=64827609

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201811041230.7A Pending CN109125727A (en) 2018-09-07 2018-09-07 A kind of preparation method of the nanocomposite based on poly-dopamine@graphene targeting-photo-thermal-light power synergistic treatment

Country Status (1)

Country Link
CN (1) CN109125727A (en)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110302378A (en) * 2019-07-04 2019-10-08 浙江理工大学 A kind of preparation method of the targeting photo-thermal nanocomposite based on graphene oxide
CN110404069A (en) * 2019-08-19 2019-11-05 浙江理工大学 A kind of nanocomposite based on poly-dopamine@MOF-Al complex carries targeting-photo-thermal-light power synergistic treatment
CN110488021A (en) * 2019-08-21 2019-11-22 浙江理工大学 It is a kind of based on poly-dopamine-composite titania material modified glassy carbon electrode fibroin albumen electrochemical immunosensor
CN111000826A (en) * 2019-12-31 2020-04-14 江南大学附属医院(无锡市第四人民医院) Medicine for synergistic chemical photothermal therapy and targeted treatment of liver cancer and preparation method
CN111529682A (en) * 2020-05-11 2020-08-14 中国人民解放军陆军军医大学第一附属医院 Chemotaxis antibacterial nano material and preparation method and application thereof
CN112772670A (en) * 2020-12-17 2021-05-11 南京师范大学 Preparation method of quaternary composite nano controlled release system
CN114249371A (en) * 2021-12-20 2022-03-29 盐城工学院 Preparation method of photo-thermal water evaporation material

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
DEHONG HU等: ""Indocyanine Green-Loaded Polydopamine-Reduced Graphene Oxide Nanocomposites with Amplifying Photoacoustic and Photothermal Effects for Cancer Theranostics"", 《THERANOSTICS》 *
PENG HUANG等: ""Folic Acid-conjugated Graphene Oxide loaded with Photosensitizers for Targeting Photodynamic Therapy"", 《THERANOSTICS》 *
徐兴英: ""功能化氧化石墨烯的制备及其载药性能"", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110302378A (en) * 2019-07-04 2019-10-08 浙江理工大学 A kind of preparation method of the targeting photo-thermal nanocomposite based on graphene oxide
CN110404069A (en) * 2019-08-19 2019-11-05 浙江理工大学 A kind of nanocomposite based on poly-dopamine@MOF-Al complex carries targeting-photo-thermal-light power synergistic treatment
CN110488021A (en) * 2019-08-21 2019-11-22 浙江理工大学 It is a kind of based on poly-dopamine-composite titania material modified glassy carbon electrode fibroin albumen electrochemical immunosensor
CN111000826A (en) * 2019-12-31 2020-04-14 江南大学附属医院(无锡市第四人民医院) Medicine for synergistic chemical photothermal therapy and targeted treatment of liver cancer and preparation method
CN111529682A (en) * 2020-05-11 2020-08-14 中国人民解放军陆军军医大学第一附属医院 Chemotaxis antibacterial nano material and preparation method and application thereof
CN112772670A (en) * 2020-12-17 2021-05-11 南京师范大学 Preparation method of quaternary composite nano controlled release system
CN114249371A (en) * 2021-12-20 2022-03-29 盐城工学院 Preparation method of photo-thermal water evaporation material

Similar Documents

Publication Publication Date Title
CN109125727A (en) A kind of preparation method of the nanocomposite based on poly-dopamine@graphene targeting-photo-thermal-light power synergistic treatment
CN106139144B (en) A kind of hyaluronic acid decorated gold-Nano carbon balls and the preparation method and application thereof with synergistic antitumor characteristic
CN109045298A (en) A kind of preparation method of the photodynamic hypericin-folic acid-fluorinated graphene polymer nanocomposites of targeting-photo-thermal-
Liu et al. Combined photothermal and photodynamic therapy delivered by PEGylated MoS 2 nanosheets
CN104530263B (en) A kind of preparation method of gallic acid bagasse xylan ester
Mousavi et al. Shape-controlled synthesis of zinc nanostructures mediating macromolecules for biomedical applications
CN108785275A (en) A kind of preparation method of the targeting being embedded with anticancer drug-optothermal polymerization object particle
Qian et al. Injectable self-healing polysaccharide hydrogel loading CuS and pH-responsive DOX@ ZIF-8 nanoparticles for synergistic photothermal-photodynamic-chemo therapy of cancer
Espinoza et al. Synthesis and characterization of silica nanoparticles from rice ashes coated with chitosan/cancer cell membrane for hepatocellular cancer treatment
Liao et al. Small-size Ti3C2Tx MXene nanosheets coated with metal-polyphenol nanodots for enhanced cancer photothermal therapy and anti-inflammation
CN103936883A (en) Mercapto-containing chitosan derivative, compound nano particle and preparation method
Lin et al. Design and evaluation of pH-responsive hydrogel for oral delivery of amifostine and study on its radioprotective effects
CN109320993A (en) A kind of preparation method of natural black pigment nano particle
CN114163547B (en) Pharmaceutical composition for mild photothermal treatment of tumor as well as preparation method and application thereof
CA2940611C (en) A method for the treatment of cancer based on metallofullerene monocrystalline nanoparticles specifically disrupting tumor vessels
Du et al. A bright future: Advanced nanotechnology-assisted microwave therapy
CN106215196B (en) Carbon/calcium phosphate/ferroso-ferric oxide composite construction nanoparticle preparation method
Pan et al. A superior preparing method for daidzein-hydroxypropyl-β-cyclodextrin complexes with improved solubility and dissolution: supercritical fluid process
Nasiri et al. Synthesis, functionalization, characterization, and in vitro evaluation of robust pH-sensitive CFNs–PA–CaCO 3
CN108295267A (en) The preparation of more targeted nano pharmaceutical carriers and the methods and applications for loading camptothecine
Feng et al. Microwave-activated Cu-doped zirconium metal-organic framework for a highly effective combination of microwave dynamic and thermal therapy
CN115645371A (en) Self-generated active oxygen nanoparticles for precise non-invasive colon cancer dynamic immunotherapy and preparation method and application thereof
CN108610460B (en) Active oxygen stimulation response type nano gel drug carrier and preparation method and application thereof
Song et al. Imidazolium-based ionic liquid-assisted preparation of nano-spheres loaded with bio-active peptides to decrease inflammation in an osteoarthritis model: ex vivo evaluations
CN110404069A (en) A kind of nanocomposite based on poly-dopamine@MOF-Al complex carries targeting-photo-thermal-light power synergistic treatment

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20190104

RJ01 Rejection of invention patent application after publication