CN107080844A - One kind carries medicine gauffer graphite nodule photo-thermal preparation and its preparation and application - Google Patents
One kind carries medicine gauffer graphite nodule photo-thermal preparation and its preparation and application Download PDFInfo
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- CN107080844A CN107080844A CN201710237255.3A CN201710237255A CN107080844A CN 107080844 A CN107080844 A CN 107080844A CN 201710237255 A CN201710237255 A CN 201710237255A CN 107080844 A CN107080844 A CN 107080844A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K41/00—Medicinal preparations obtained by treating materials with wave energy or particle radiation ; Therapies using these preparations
- A61K41/0052—Thermotherapy; Hyperthermia; Magnetic induction; Induction heating therapy
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/70—Carbohydrates; Sugars; Derivatives thereof
- A61K31/7028—Compounds having saccharide radicals attached to non-saccharide compounds by glycosidic linkages
- A61K31/7034—Compounds having saccharide radicals attached to non-saccharide compounds by glycosidic linkages attached to a carbocyclic compound, e.g. phloridzin
- A61K31/704—Compounds having saccharide radicals attached to non-saccharide compounds by glycosidic linkages attached to a carbocyclic compound, e.g. phloridzin attached to a condensed carbocyclic ring system, e.g. sennosides, thiocolchicosides, escin, daunorubicin
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Abstract
Medicine gauffer graphite nodule photo-thermal preparation and its preparation and application are carried the present invention relates to one kind, the aqueous solution of medicine will be added in the aqueous solution of graphene oxide, pH value is adjusted, vibration obtains carrying medicine compound；Prepare and carry medicine compound water solution, be then atomized, the aerosol droplets after atomization are collected by quartz ampoule, end with polytetrafluoroethylene PTFE filter membrane, are dried, are produced.Medicine compound will be carried to co-culture with cancer cell, be irradiated with infrared light, and compared with not carrying out illumination and pure DOX, material cancer cell lethal effect is detected.The new load medicine photo-thermal preparation of the present invention has unique Photothermal characterisation, and preparation method is simple, can industrialize a large amount of preparations, material can be used for antitumor research, there is good practical value.
Description
Technical field
It is more particularly to a kind of to carry medicine gauffer graphite nodule photo-thermal system the invention belongs to photo-thermal preparation and its preparation and application field
Agent and its preparation and application.
Background technology
Long-term consumption noxious material is easily caused cancer morbidity raising.Current treatment means mainly have chemotherapy, operation
Treatment and radiotherapy.Chemotherapy is using the propagation of chemicals prevention cancer cell, infiltration, transfer, until it is thin finally to kill cancer
A kind of therapeutic modality of born of the same parents, but its selectivity is not strong, and human normal also can be inevitably damaged while cancer cell is killed
Cell, makes patient adverse reaction occur；The patient that operative treatment can only not yet spread for early stage cancer cell, for tumour cell
Transferred patient's operative treatment can not generally be effected a radical cure, and cause secondary injury to patient；Radiotherapy utilizes X-ray, electricity
Sub-line etc. is irradiated to site of pathological change, but limited for transferred cancer cell effect.Photo-thermal therapy (PTT) is as safer
Novel tumor treatment method receives extensive concern.Wherein, the research and development core of photo-thermal therapy is with superpower photothermal conversion efficiency
Nano material research and development.In noble metal nanometer material, such as gold nano grain, due to having very strong surface plasma to light
Resonant absorption effects, are preferable photothermal conversion materiats.
Graphene (Graphene), be one kind by carbon atom with sp2The hexangle type of hybridized orbit composition is in honeycomb lattice
New Two Dimensional planar materials, thermal conductivity factor is up under 5300W/mK, normal temperature its electron mobility more than 15000cm2/ Vs,
There is minimum electron conductivity, with fractional quantum hall effect and ferromagnetism, graphene is still under the zero carrier concentration limit
Most thin in known materials in the world at present, thickness only has 0.335nm.The carbon materials such as graphene and golden nanometer particle and CNT
Material is compared, with small volume, photo-thermal efficiency high and the low advantage of cost.And gauffer graphene ball possesses finer and close structure,
And granular size is controllable, if may have effect more applied to photo-thermal therapy.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of load medicine gauffer graphite nodule photo-thermal preparation and its preparation and should
With the medicine-carrying method is simple to operate, reaction condition gentle, can largely prepare, can be used for antitumor research, there is good reality
With value.
The a kind of of the present invention carries medicine gauffer graphite nodule photo-thermal preparation, and graphene oxide is combined with medicine, then using super
Sound atomization-thermal reduction prepares load medicine gauffer graphite nodule photo-thermal preparation；Wherein medicine is adriamycin DOX.
A kind of preparation method of load medicine gauffer graphite nodule photo-thermal preparation of the present invention, including：
(1) aqueous solution of medicine will be added in the aqueous solution of graphene oxide, pH value is adjusted, vibration obtains load medicine and is combined
Thing；It is kept in dark place, it is standby；Wherein the mass ratio of graphene oxide and medicine is 1:1~1:3；
(2) prepare and carry medicine compound water solution, be then atomized, the aerosol droplets after atomization pass through quartz ampoule, end
End is collected with polytetrafluoroethylene PTFE filter membrane, is dried, and produces load medicine gauffer graphene ball.
The concentration of the aqueous solution of graphene oxide is 0.5~2.0mg/ml in the step (1)；The concentration of aqueous solution of medicine
For 1.0~2.0mg/ml.
Medicine is adriamycin in the step (1).
Regulation pH value is in the step (1)：It is 7~10 with sodium hydroxide solution and/or salt acid for adjusting pH value；Wherein hydrogen
Sodium oxide molybdena, the concentration of hydrochloric acid are 0.05-2.0M.
Vibration is that 3~5h is vibrated on 35~40 DEG C of shaking table in the step (1).
The concentration that medicine compound water solution is carried in the step (2) is 0.5~1.5mg/ml.
The temperature of quartz ampoule is 150 DEG C -180 DEG C in the step (2)；The aperture of polytetrafluoroethylene PTFE filter membrane is 0.2 μ
m-0.3μm。
Drying is in the step (2)：12~24h is dried under the conditions of 60~70 DEG C.
A kind of application of load medicine gauffer graphite nodule photo-thermal preparation of the present invention, carries medicine gauffer graphene ball and is used as illumination preparation
Application.
Application method：Obtained load medicine gauffer graphene ball and Hela cells is co-cultured 10 in porocyte culture plates~
After 30h, it is irradiated with laser, detects material to cancer cell lethal effect with mtt assay.
Wherein laser power density is 1~3W/cm2, optical maser wavelength be 780~820nm, laser irradiation time be 5~
10min。
The nonmetal nano material of the research of the present invention is while with good photo-thermal effect, also with load medicine function.
Therefore the present invention selects to have tumour cell the adriamycin (DOX) of lethality as medicine, and graphene oxide is used as carrier, utilizes
Optimize load medicinal strip part DOX is supported on graphene oxide, load medicine gauffer graphite nodule then is made by being atomized thermal reduction
Crumpled-rGO/DOX.Using the excellent Photothermal characterisation of the composite with carrying medicine function, both act synergistically, and are cancer
Treatment provides a kind of brand-new method.
Beneficial effect
(1) present invention prepares graphite oxide containing adriamycin using the pi-pi accumulation effect between graphene oxide and adriamycin
Alkene, then prepares load medicine composite using ultrasonic atomizatio-thermal reduction, and preparation method is simple to operate, and experiment condition is gentle,
Raw material are cheap and easy to get, are easy to large-scale production.
(2) the graphene ball composite of gauffer containing adriamycin prepared by the present invention is a kind of photo-thermal preparation, can be by luminous energy
Efficient to be converted into heat energy, drug load is high, the potentiality with treating cancer.
Brief description of the drawings
The photo-thermal curve that the Crumpled-rGO-DOX composites of Fig. 1 various concentrations are changed over time；
The photo-thermal curve that Crumpled-rGO-DOX composites are changed over time under Fig. 2 different capacity density；
The stability analysis of Fig. 3 Crumpled-rGO-DOX composites；
Photo-thermal efficiency of Fig. 4 Crumpled-rGO-DOX composites to cell.
Embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention.In addition, it is to be understood that after the content of the invention lectured has been read, people in the art
Member can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Scope.
Embodiment 1
The preparation of GO/DOX compounds, comprises the following steps：
Weigh the GO solution that 40ml concentration is 1mg/ml to mix with the DOX solution that 40 concentration are 2.0mg/ml so that GO:
DOX=1:2, the sodium hydroxide solution for being then 0.1M with concentration adjusts the pH value of mixed liquor so that the pH=9 of mixed liquor.
Mixed liquor after regulating is placed on the shaking table that temperature is 37 DEG C and stirred 4 hours, obtains carrying medicine compound.By solution pour into from
Heart pipe, centrifuges 3min under 10000rmp centrifuge, gently removes supernatant, adds 10ml ultra-pure waters.Under the conditions of lucifuge
Freeze-drying, compound aluminium foil is wrapped and is placed on temperature to save backup in 4 DEG C of refrigerator.
Embodiment 2
Crumpled-rGO/DOX preparation, comprises the following steps：
It is dissolved in 20ml ultra-pure waters, is configured to dense with the GO/DOX compounds 20mg in balance accurate weighing embodiment (1)
The solution for 1.0mg/ml is spent, solution is placed in the ultrasonic atomizer for being connected with quartz ampoule to (materialization concussion frequency is 1.7MHz
~2.1MHz) it is atomized into aerosol droplets, by being heated to 180 DEG C of stone under atomization air flow and the driving of suction filtration vavuum pump
Ying Guanhou, is collected for 0.22 μm of PTFE filter membranes with aperture, dries 3 hours at room temperature, be then placed in vacuum desiccator 60 DEG C
Dry after 24h, produce Crumpled-rGO/DOX.
Embodiment 3
Accurate Crumpled-rGO (embodiment 2) aqueous solution 10mL for preparing 200 μ g/mL concentration, uses varying strength
Laser is irradiated, and laser intensity is respectively：0.5、1、1.5、2W/cm2.5min is irradiated for 808nm laser using wavelength, it is molten
The temperature change of liquid carries out thermograph using infrared thermography, may finally obtain heating of the solution under laser irradiation bent
The real-time recording of line and solution, is shown in Fig. 1 and Fig. 2.
For the photo and thermal stability of research material, determine the material aqueous solution that concentration is 200 μ g/mL is in laser intensity
1W/cm2, irradiation time 5min, measure it is continuous No. 5 times switch irradiation under the conditions of heating down cycles curve, further study material
The photo and thermal stability of material, stability curve is shown in Fig. 3.
The light thermal property of gauffer graphene ball as shown in Figure 1, 2, it can be found that under the same conditions, Crumpled-rGO's
Light thermal property is better than GO, and heating degree is directly proportional to solution concentration and laser intensity, and concentration is higher, and laser intensity is higher, temperature
What is risen is higher；Using the heating temperature lowering curve of continuous No. 5 times switch irradiation monitoring materials, as a result find that material heats up cooling journey every time
Degree is substantially the same, and implys that material has good stability.These data show that Crumpled-rGO may serve as
The optothermal material of one new excellent.
Embodiment 4
Using the cell for growing into logarithmic phase, cell is counted using blood counting chamber, cell is added to 96 holes
Tissue Culture Plate, makes every μ L of pore volume 200, number of cells is 10000, in CO224h is cultivated in incubator.Work as cell attachment
Nutrient solution is absorbed after completely, be separately added into per hole DOXs (be respectively 0.5 μM, 1 μM, 2 μM, 4 μM) of the 200 μ L containing various concentrations and
Crumpled-rGO/DOX (embodiment 2) (it is respectively 0.5 μM, 1 μM, 2 μM, 4 μM wherein to correspond to DOX concentration) fresh cultured
It is incubated in liquid, incubator.Cultivate after 24h, with power density be that the laser that 1W/cm2, wavelength are 808nm irradiates 5min per hole, and
Set addition Crumpled-rGO/DOX and without the control group of illumination.The nutrient solution in orifice plate is removed in irradiation after finishing, per hole
20 μ L w=0.5% MTT solution is added, solution is sucked after cultivating 4h in lucifuge in incubator, 200 μ L are added per hole
DMSO solution, lucifuge vibrates 30min on rotating speed 90rpm shaking tables, crystal is fully dissolved, is existed using enzyme-linked immunosorbent assay instrument
The ultraviolet absorption value of each hole solution is determined at 570nm.Experiment compares group with the PBS cells handled, and every group of setting 3 is parallel
Sample.
As a result it is as shown in Figure 4.From figure it can be found that compared with control group, the material containing DOX has certain to cell
Lethal effect, and increase with the increase of DOX concentration.When not carrying out illumination, DOX compares Crumpled- under same concentrations
RGO/DOX possesses stronger lethal effect.After illumination is carried out, the cell number of the material containing Crumpled-rGO/DOX subtracts rapidly
It is few, and increase with the increase of material concentration, when material addition is 4 μM, the survival rate of cell only has 47%, much
Less than depositing DOX and Crumpled-rGO/DOX without photo-irradiation treatment.Illustrate that Crumpled-rGO/DOX has excellent photo-thermal
Efficiency is changed, this effect and DOX effect are superimposed, generate stronger lethality, play the purpose of oncotherapy.Cause
This, the present invention is prepared for a kind of excellent photo-thermal preparation with load medicine function, can perform well in oncotherapy.
Claims (10)
1. one kind carries medicine gauffer graphite nodule photo-thermal preparation, it is characterised in that：Graphene oxide is combined with medicine, then using super
Sound atomization-thermal reduction prepares load medicine gauffer graphite nodule photo-thermal preparation.
2. a kind of preparation method as claimed in claim 1 for carrying medicine gauffer graphite nodule photo-thermal preparation, including：
(1) aqueous solution of medicine will be added in the aqueous solution of graphene oxide, pH value is adjusted, vibration obtains carrying medicine compound；
(2) prepare and carry medicine compound water solution, be then atomized, the aerosol droplets after atomization are used by quartz ampoule, end
Polytetrafluoroethylene PTFE filter membrane is collected, and is dried, and produces load medicine gauffer graphene ball.
3. a kind of preparation method for carrying medicine gauffer graphite nodule photo-thermal preparation according to claim 2, it is characterised in that：It is described
The concentration of the aqueous solution of graphene oxide is 0.5~2.0mg/ml in step (1)；The concentration of aqueous solution of medicine be 1.0~
2.0mg/ml。
4. a kind of preparation method for carrying medicine gauffer graphite nodule photo-thermal preparation according to claim 2, it is characterised in that：It is described
Medicine is adriamycin in step (1).
5. a kind of preparation method for carrying medicine gauffer graphite nodule photo-thermal preparation according to claim 2, it is characterised in that：It is described
Regulation pH value is in step (1)：It is 7~10 with sodium hydroxide solution and/or salt acid for adjusting pH value；Wherein sodium hydroxide, hydrochloric acid
Concentration be 0.05-2.0M.
6. a kind of preparation method for carrying medicine gauffer graphite nodule photo-thermal preparation according to claim 2, it is characterised in that：It is described
Vibration is that 3~5h is vibrated on 35~40 DEG C of shaking table in step (1).
7. a kind of preparation method for carrying medicine gauffer graphite nodule photo-thermal preparation according to claim 2, it is characterised in that：It is described
The concentration that medicine compound water solution is carried in step (2) is 0.5~1.5mg/ml.
8. a kind of preparation method for carrying medicine gauffer graphite nodule photo-thermal preparation according to claim 2, it is characterised in that：It is described
The temperature of quartz ampoule is 150 DEG C -180 DEG C in step (2)；The aperture of polytetrafluoroethylene PTFE filter membrane is 0.2 μm -0.3 μm.
9. a kind of preparation method for carrying medicine gauffer graphite nodule photo-thermal preparation according to claim 2, it is characterised in that：It is described
Drying is in step (2)：12~24h is dried under the conditions of 60~70 DEG C.
10. a kind of application as claimed in claim 1 for carrying medicine gauffer graphite nodule photo-thermal preparation, it is characterised in that：Carry medicine gauffer
Graphene ball shines preparation as infrared ray.
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| CN201710237255.3A CN107080844A (en) | 2017-04-12 | 2017-04-12 | One kind carries medicine gauffer graphite nodule photo-thermal preparation and its preparation and application |
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| CN201710237255.3A CN107080844A (en) | 2017-04-12 | 2017-04-12 | One kind carries medicine gauffer graphite nodule photo-thermal preparation and its preparation and application |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110093776A (en) * | 2018-08-30 | 2019-08-06 | 东华大学 | A kind of preparation method of photothermal conversion heat-accumulation temperature-adjustment cotton fabric |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103623419A (en) * | 2013-11-28 | 2014-03-12 | 首都医科大学 | Chlorotoxin-targeted oxidized graphene nanometer material used for transporting antitumor drug |
| CN106176620A (en) * | 2016-08-05 | 2016-12-07 | 东华大学 | A kind of Graphene medicament slow-release microsphere and preparation method thereof |
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2017
- 2017-04-12 CN CN201710237255.3A patent/CN107080844A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103623419A (en) * | 2013-11-28 | 2014-03-12 | 首都医科大学 | Chlorotoxin-targeted oxidized graphene nanometer material used for transporting antitumor drug |
| CN106176620A (en) * | 2016-08-05 | 2016-12-07 | 东华大学 | A kind of Graphene medicament slow-release microsphere and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 蒋晨: "《纳米药物》", 31 August 2015, 华东理工大学出版社有限公司 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110093776A (en) * | 2018-08-30 | 2019-08-06 | 东华大学 | A kind of preparation method of photothermal conversion heat-accumulation temperature-adjustment cotton fabric |
| CN110093776B (en) * | 2018-08-30 | 2021-04-02 | 东华大学 | Preparation method of photothermal conversion heat storage and temperature regulation cotton fabric |
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Application publication date: 20170822 |