CN109125272A - It is a kind of with fluorinated graphene be the carrier loaded nanoparticle for having mitoxantrone preparation method - Google Patents
It is a kind of with fluorinated graphene be the carrier loaded nanoparticle for having mitoxantrone preparation method Download PDFInfo
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Abstract
The present invention relates to field of medicaments, disclose a kind of preparation method with fluorinated graphene for the carrier loaded nanoparticle for having mitoxantrone.Graphene oxide is made by raw material of crystalline flake graphite first in the present invention, then it is fluorinated by diethylaminosulfurtrifluoride, fluoro-containing group is converted by part oxygen-containing group, partially fluorinated graphene is made, its surface possesses a large amount of oxygen containing hydrophilic functional groups, facilitates it and is loaded and improved biocompatibility to drug by hydrogen bond.By partially fluorinated graphene dispersion in the phosphate buffer that pH is 7.4, partially fluorinated graphene solution is obtained, with mitoxantrone by reacting to obtain nanoparticle.The nanoparticle of this method preparation will not make a significant impact cell in the experimentation in later period, not influence the science of experimental result, and experiment flow is simple and convenient to operate, does not need harsh reaction condition and special reaction unit.
Description
Technical field
The present invention relates to field of medicaments more particularly to it is a kind of with fluorinated graphene be the carrier loaded nanometer for having mitoxantrone
The preparation method of particle.
Background technique
Fluorinated graphene just spreads out as the novel of graphene after 2010 are successfully prepared for the first time by Geim seminar
Biology, by people's extensive concern, it is similar with its, still has good mechanical property, while fluorine original is introduced on the basis of it
Son, to obtain many uniquenesses and excellent performance.It possesses outstanding electronics, optically and mechanically performance, while also
The effect of interface energy is reduced, and thermal stability and inoxidizability well.This allows the main research hotspot of fluorinated graphene
In fields such as optics, electronics and theoretical calculations.
Fluorinated graphene not only inherits the excellent properties of grapheme material, but also has not available for other carbon materials
Significant advantage (such as: stable paramagnetism, stable luminescence generated by light, fluorine medically special effect), has as novel swollen
The potential value of the carrier of tumor medicine.But poor biocompatibility caused by its hydrophobicity, harsh preparation condition and cumbersome
The factors such as synthesis step seriously limit fluorinated graphene in the application of biological field.How fluorinated graphene to be answered so probing into
It is very significant for biological field.
Summary of the invention
In order to solve the above-mentioned technical problems, the present invention provides one kind to have mitoxantrone with fluorinated graphene to be carrier loaded
Nanoparticle preparation method.The present invention first using crystalline flake graphite as raw material, by improve hummers method and it is a series of after
Graphene oxide is prepared in processing, then passes through the fluorination of fluorization agent diethylaminosulfurtrifluoride, by graphene oxide
Part oxygen-containing group is converted into fluoro-containing group, is prepared for hydrophilic partially fluorinated graphene, and can be stable be dispersed in
In water.A large amount of oxygen containing hydrophilic functional groups that oxidation fluorinated graphene sheet surfaces are possessed, this helps to make it through hydrogen bond
Biocompatibility is loaded and improved to drug.The phosphoric acid for being then 7.4 in pH by obtained partially fluorinated graphene dispersion
In salt buffer, the partially fluorinated graphene solution of evenly dispersed nano-scale is obtained by ultrasonic treatment.In backward solution
Mitoxantrone is added and obtains partially fluorinated graphene-mitoxantrone after reaction and post-processing.The nanometer of this method preparation is micro-
Grain will not make a significant impact cell in the experimentation in later period, not influence the science of experimental result, experiment flow letter
Reaction condition and special reaction unit single, easy to operate, that do not need harshness.
The specific technical proposal of the invention is: it is a kind of with fluorinated graphene be the carrier loaded nanoparticle for having mitoxantrone
Preparation method, in terms of g and mL, comprising the following steps:
1) container is cooled to 0 DEG C in ice-water bath, the 20-25 mL concentrated sulfuric acid is added；Then 0.5-2 g crystalline graphite powder is added
With 0.2-1 g sodium nitrate；It is ultrasonically treated 20-30 min.
The present invention is cheap using crystalline flake graphite as raw material.
2) it is stirred to react, keeps reaction temperature to be lower than 10 DEG C, 2-4 g potassium permanganate is then weighed, in 25-30 min
It is slowly added in batches；Elementary reaction 1.5-2.5 h.
The present invention increases potassium manganate in batches can make reaction more mild, convenient for control temperature of reaction system, prevent anti-
Should be excessively fierce, generate unnecessary impurity.Simultaneously graphite-sulfuric acid single order can be generated under its oxidation by sulfuric acid intercalation
Intercalation object.
3) it is warming up to 35-40 DEG C, reacts 25-30 min；
4) 70-120 mL deionized water is measured, is slowly added to after ice-water bath is cooled to 0 DEG C；Then temperature adjustment is to 90-95
DEG C, continue to be stirred to react 25-30 min.
The present invention is by graphite oxide obtained in step 3), by being reacted with water, while water enter interlayer substitution it is therein
Acid obtains graphene oxide to removing.
5) 50-70 mL distilled water stopped reaction is added, adds the H that 20-30 mL volume fraction is 25-35%2O2, continue
It is stirred to react 15-20 min；
6) HCl solution that 30-50 mL volume fraction is 8-12% is added, stands 4-5 days.
Product is stood 4-5 days in step 6) by the present invention, is that the separation of the impurity such as the acid in lower sediment penetrates into supernatant
In liquid, to reduce centrifugation time.
7) supernatant of solution, Zai Qu lower layer viscous fluid centrifugal treating are first removed with dropper, until viscous fluid is in neutrality, it will
Viscous fluid in centrifuge tube pours into evaporating dish, is freeze-dried 24-48 h, obtains graphene oxide sheet；
8) graphene oxide sheet is ground into graphene oxide powder；
9) 0.5-1.5 g graphene oxide powder and 20-40 mL methylene chloride or 1,2- dichloroethanes, stirring is added in another extracting container
10-14 h keeps its evenly dispersed.
For the present invention with methylene chloride or 1 in step 9), 2- dichloroethanes is solvent, enables graphene oxide powder at it
In it is evenly dispersed.
10) 0.5-1 mL fluorization agent diethylaminosulfurtrifluoride is added dropwise, is then ultrasonically treated 4-6 h, stirring at room temperature
React 24-72 h.
The present invention using diethylaminosulfurtrifluoride as fluorization agent, have very strong fluorination, can at normal temperatures and pressures by
Oxygen-containing functional group in graphene oxide is partially converted into fluorine-containing functional group.It is prepared for hydrophilic partially fluorinated graphene, and
And can be stable be dispersed in water.A large amount of oxygen containing hydrophilic functional groups that oxidation fluorinated graphene sheet surfaces are possessed, this
Help to make it through hydrogen bond and biocompatibility is loaded and improved to drug.
11) after the termination reaction of 15-30 mL methanol is added, partially fluorinated graphite ene product is obtained by filtration, and with ethyl alcohol and go
Ionized water sufficiently washs, dry at 50-70 DEG C；
12) partially fluorinated graphene dispersion obtained by 0.05-0.1 g step 11) is delayed in the phosphate that 45-60 mL pH is 7.4
In fliud flushing, ultrasonic treatment obtains partially fluorinated graphene solution.
The present invention obtains evenly dispersed nanometer in the phosphate buffer that pH is 7.4 using ultrasonic cell disruptor
The partially fluorinated graphene solution of size is brought conveniently for load mitoxantrone below.
13) taking 0.8-1 mL concentration is that the mitoxantrone of 2 mg/ mL is slowly dropped into partially fluorinated graphene solution；It keeps away
Light stirs 24-30 h, and centrifugation is collected particle, saved after the material freeze of lower layer is dry, is made negative by carrier of fluorinated graphene
It is loaded with the nanoparticle of mitoxantrone.
Preferably, stirring rate is 400-800 rpm in step 2,20-40 min is stirred.
Preferably, during standing, every 1-2 d removes supernatant in step 6), aliquots of deionized water is added.
Preferably, in step 7), centrifugal process specifically: supercentrifuge is used, respectively in 4000 rpm, 6000
10 min are centrifuged under rpm, 8000 rpm, 10000 rpm, 12000 rpm, remove supernatant in centrifuge tube after centrifugation every time and are added
Enter aliquots of deionized water.
Preferably, each reaction that step 9), step 10), step 11) carry out carries out at room temperature.
Preferably, in step 12), ultrasonic treatment specifically: utilize ultrasound under 630 W power of ultrasonic cell disruptor
Wave processing 2.5-3 h obtains the partially fluorinated graphene solution of evenly dispersed nano-scale.
The present invention is obtained in the phosphate buffer that pH is 7.4 in step 12) using ultrasonic cell disruptor
The partially fluorinated graphene solution of the nano-scale of even dispersion is brought conveniently for load mitoxantrone below.
Preferably, in step 13), centrifugation specifically: high-speed refrigerated centrifuge is used, 12000-16000 rpm's
It is centrifuged 7-15 min under revolving speed, collects particle.
It is compared with the prior art, the beneficial effects of the present invention are: the present invention passes through improvement first using crystalline flake graphite as raw material
Graphene oxide is prepared in hummers method and a series of post-processings, then passes through fluorization agent diethylaminosulfurtrifluoride
Fluorination converts fluoro-containing group for graphene oxide part oxygen-containing group, is prepared for hydrophilic partially fluorinated graphene,
And can be stable be dispersed in water.Fluorinated graphene preparation process is simple and convenient to operate, does not need harsh reaction simultaneously
Condition and special reaction unit.A large amount of oxygen containing hydrophilic functional groups that partially fluorinated graphene film layer surface is possessed, this has
Help to make it through hydrogen bond and biocompatibility is loaded and improved to drug.The partially fluorinated graphene dispersion that will then obtain
In the phosphate buffer that pH is 7.4, the partially fluorinated graphite of evenly dispersed nano-scale is obtained by ultrasonication
Alkene solution.Mitoxantrone is added in backward solution and obtains partially fluorinated graphene-mitoxantrone after reaction and post-processing.It should
The nanoparticle of method preparation will not make a significant impact cell in the experimentation in later period, not influence the section of experimental result
The property learned, experiment flow are simple and convenient to operate, do not need harsh reaction condition and special reaction unit.
Detailed description of the invention
Fig. 1 is the infrared spectrum comparison diagram of product and commercially available graphene oxide made from embodiment 1-3.
Specific embodiment
The present invention will be further described with reference to the examples below.
Embodiment 1:
1) beaker is cooled to 0 DEG C in ice-water bath, magneton is added, 250 mL is added to the concentrated sulfuric acid that graduated cylinder measures 20 mL and burns
In cup；Then it weighs 0.5 crystalline graphite powder and beaker is added in 0.2 sodium nitrate；Then ultrasound is carried out, 20 min are continued；
2) beaker in step 1) is placed in magnetic agitation water-bath, 20 min is stirred under the revolving speed of 400 rpm, keep reaction
Temperature is lower than 10 DEG C, then weighs 2g potassium permanganate on an electronic balance, is slowly added in batches in 25min；The stage is anti-
Answer 1.5 h；
3) water bath temperature in step 2 is risen to 35 DEG C, reacts 25 min；
4) 70mL deionized water is measured slowly to be added in step 3) in beaker after ice-water bath is cooled to 0 DEG C；Then it adjusts
Step 3) water bath temperature is to after 90 DEG C or so, the reaction was continued under stirring auxiliary 25 min；
5) into step 4) beaker be added 50mL distilled water stopped reaction, add 25 mL volume fractions be 30% H2O2,
Continue to be stirred to react 15 min；
6) HCl solution that 40 mL volume fractions are 10% is measured with graduated cylinder, is then added into beaker in step 5).Product is existed
4 d are stood in beaker, every 1 d removes supernatant, and aliquots of deionized water is added；
7) supernatant in step 6) in beaker first is removed with dropper, Zai Qu lower layer viscous fluid uses supercentrifuge, exists respectively
10 min are centrifuged under 4000 rpm, 6000 rpm, 8000 rpm, 10000 rpm, 12000 rpm, remove centrifugation after centrifugation every time
Supernatant and aliquots of deionized water is added in pipe, until graphene oxide viscous fluid is in neutrality, the viscous fluid in centrifuge tube is poured into
In evaporating dish, 24 h of freeze-drying obtain graphene oxide sheet；
8) by graphene oxide sheet grind into powder in step 7)；
9) methylene chloride or 1 of graphene oxide and 20 mL in 0.5 g step 8), bis- chloroethene of 2- are added into 100 mL flasks
Alkane, and it is put into magneton；Stirring 10 h keeps its evenly dispersed；
10) into step 9) flask be added dropwise 0.5 mL fluorization agent diethylaminosulfurtrifluoride, be then ultrasonically treated 4 at room temperature
H is stirred to react 24 h；
11) after the termination reaction of 15 mL methanol is added in flask into step 10), partially fluorinated graphite ene product is obtained by filtration, is used in combination
Ethyl alcohol and deionized water are sufficiently washed, and are put into drying over night in 60 DEG C of baking ovens；
12) phosphate buffer for being first 7.4 in 45 mL pH by the partially fluorinated graphene dispersion in 0.05 g step 11)
In, the part of evenly dispersed nano-scale is obtained using 2.5 h of ultrasonication under 630 W power of ultrasonic cell disruptor
Fluorinated graphene solution.
13) take 0.8 mL mass concentration be 2 mg/ mL mitoxantrone be slowly dropped into fill it is partially fluorinated in step 12)
In the beaker of graphene solution；It is protected from light 24 h of stirring and is centrifuged 7 under the revolving speed of 12000 rpm using high-speed refrigerated centrifuge
Min collects particle, collects particle, saves, be made after substance (partially fluorinated graphene-mitoxantrone) freeze-drying of lower layer
With fluorinated graphene for the carrier loaded nanoparticle for having mitoxantrone.
Embodiment 2:
1) beaker is cooled to 0 DEG C in ice-water bath, magneton is added, 250 mL is added to the concentrated sulfuric acid that graduated cylinder measures 23 mL and burns
In cup；Then it weighs 0.1 g crystalline graphite powder and beaker is added in 0.5 g sodium nitrate；Then ultrasound is carried out, 5min is continued；
2) beaker in step 1) is placed in magnetic agitation water-bath, 30 min is stirred under the revolving speed of 600 rpm, keep reaction
Temperature is lower than 10 DEG C, then weighs 3 g potassium permanganate on an electronic balance, is slowly added in batches in 28 min；The stage
React 2 h；
3) water bath temperature in step 2 is risen to 38 DEG C, reacts 30 min；
4) 100 mL deionized waters are measured slowly to be added in step 3) in beaker after ice-water bath is cooled to 0 DEG C；Then it adjusts
Step 3) water bath temperature is saved to after 93 DEG C or so, the reaction was continued under stirring auxiliary 27 min；
5) into step 4) beaker be added 60 mL distilled water stopped reaction, add 25 mL volume fractions be 30% H2O2,
Continue to be stirred to react 18 min；
6) HCl solution that 40 mL volume fractions are 10% is measured with graduated cylinder, is then added into beaker in step 5).Product is existed
4.5 d are stood in beaker, every 1.5 d removes supernatant, and aliquots of deionized water is added；
7) supernatant in step 6) in beaker first is removed with dropper, Zai Qu lower layer viscous fluid uses supercentrifuge, exists respectively
10 min are centrifuged under 4000 rpm, 6000 rpm, 8000 rpm, 10000 rpm, 12000 rpm, remove centrifugation after centrifugation every time
Supernatant and aliquots of deionized water is added in pipe, until graphene oxide viscous fluid is in neutrality, the viscous fluid in centrifuge tube is poured into
In evaporating dish, 36 h of freeze-drying obtain graphene oxide sheet；
8) by graphene oxide sheet grind into powder in step 7)；
9) it is added the methylene chloride or 1 of graphene oxide and 30 mL in 1 g step 8) into 100 mL flasks, 2- dichloroethanes,
And it is put into magneton；Stirring 12 h keeps its evenly dispersed；
10) into step 9) flask be added dropwise 0.8 mL fluorization agent diethylaminosulfurtrifluoride, be then ultrasonically treated 5 at room temperature
H is stirred to react 36 h；
11) after the termination reaction of 25 mL methanol is added in flask into step 10), partially fluorinated graphite ene product is obtained by filtration, is used in combination
Ethyl alcohol and deionized water are sufficiently washed, and are put into drying over night in 60 DEG C of baking ovens；
12) the partially fluorinated graphene dispersion in 0.05-0.1 g step 11) is delayed in the phosphate that 50 mL pH are 7.4 first
In fliud flushing, the portion of evenly dispersed nano-scale is obtained using 3 h of ultrasonication under 630 W power of ultrasonic cell disruptor
Divide fluorinated graphene solution.
13) it takes 1 mL mass concentration to be slowly dropped into for the mitoxantrone of 2 mg/ mL and fills partially fluorinated stone in step 12)
In the beaker of black alkene solution；It is protected from light 24 h of stirring and is centrifuged 10 under the revolving speed of 14000 rpm using high-speed refrigerated centrifuge
Min collects particle, collects particle, saves, be made after substance (partially fluorinated graphene-mitoxantrone) freeze-drying of lower layer
With fluorinated graphene for the carrier loaded nanoparticle for having mitoxantrone.
Embodiment 3:
1) beaker is cooled to 0 DEG C in ice-water bath, magneton is added, 250 mL is added to the concentrated sulfuric acid that graduated cylinder measures 25 mL and burns
In cup；Then 2 g crystalline graphite powders are weighed and beaker is added in 1 g sodium nitrate；Then ultrasound is carried out, 30 min are continued；
2) beaker in step 1) is placed in magnetic agitation water-bath, 40 min is stirred under the revolving speed of 800 rpm, keep reaction
Temperature is lower than 10 DEG C, then weighs 4 g potassium permanganate on an electronic balance, is slowly added in batches in 30 min；The stage
React 2.5 h；
3) water bath temperature in step 2 is risen to 40 DEG C, reacts 30 min；
4) 120 mL deionized waters are measured slowly to be added in step 3) in beaker after ice-water bath is cooled to 0 DEG C；Then it adjusts
Step 3) water bath temperature is saved to after 95 DEG C or so, the reaction was continued under stirring auxiliary 30 min；
5) into step 4) beaker be added 70 mL distilled water stopped reaction, add 30 mL volume fractions be 30% H2O2,
Continue to be stirred to react 20 min；
6) HCl solution that 40 mL volume fractions are 10% is measured with graduated cylinder, is then added into beaker in step 5).Product is existed
5 d are stood in beaker, every 2 d removes supernatant, and aliquots of deionized water is added；
7) supernatant in step 6) in beaker first is removed with dropper, Zai Qu lower layer viscous fluid uses supercentrifuge, exists respectively
10 min are centrifuged under 4000 rpm, 6000 rpm, 8000 rpm, 10000 rpm, 12000 rpm, remove centrifugation after centrifugation every time
Supernatant and aliquots of deionized water is added in pipe, until graphene oxide viscous fluid is in neutrality, the viscous fluid in centrifuge tube is poured into
In evaporating dish, 48 h of freeze-drying obtain graphene oxide sheet；
8) by graphene oxide sheet grind into powder in step 7)；
9) methylene chloride or 1 of graphene oxide and 40 mL in 1.5 g step 8), bis- chloroethene of 2- are added into 100 mL flasks
Alkane, and it is put into magneton；Stirring 14 h keeps its evenly dispersed；
10) into step 9) flask be added dropwise 1 mL fluorization agent diethylaminosulfurtrifluoride, be then ultrasonically treated 6 at room temperature
H is stirred to react 72 h；
11) after the termination reaction of 30 mL methanol is added in flask into step 10), partially fluorinated graphite ene product is obtained by filtration, is used in combination
Ethyl alcohol and deionized water are sufficiently washed, and are put into drying over night in 60 DEG C of baking ovens；
12) phosphate buffer for being first 7.4 in 60 mL pH by the partially fluorinated graphene dispersion in 0.1 g step 11)
In, the part fluorine of evenly dispersed nano-scale is obtained using 3 h of ultrasonication under 630 W power of ultrasonic cell disruptor
Graphite alkene solution.
13) it takes 1 mL mass concentration to be slowly dropped into for the mitoxantrone of 2 mg/ mL and fills partially fluorinated stone in step 12)
In the beaker of black alkene solution；It is protected from light 30 h of stirring and is centrifuged 15 under the revolving speed of 16000 rpm using high-speed refrigerated centrifuge
Min collects particle, collects particle, saves, be made after substance (partially fluorinated graphene-mitoxantrone) freeze-drying of lower layer
With fluorinated graphene for the carrier loaded nanoparticle for having mitoxantrone.It will
Infrared detection:
Infrared detection, fluorination are carried out to fluorinated graphene (recording fluorinated graphene 1-3 respectively) obtained during embodiment 1-3
The structure of graphene and graphene oxide is by ftir analysis result as shown in Figure 1, by the analysis result
It can be seen that occurring three absorption peaks in raw material graphene oxide, they are respectively with 3430 cm−1And 1730 cm−1With 1630
cm−1Centered on, 3430 cm can be determined by analysis−1The absorption peak at place is the stretching vibration of carboxyl and hydroxyl O-H.1730
cm−1The absorption peak at place can be determined that as the stretching vibration of C=O in carboxyl and ketone group.1630 cm−1The absorption peak at place is also C=C
Stretching vibration.This is the result shows that be successful by the conversion of graphene to graphene oxide.
The infrared spectrum of fluorinated graphene and graphene oxide is compared it can be found that they are in 1221 cm−1Occurs one
New absorption peak, it is possible to determine that be the eigen vibration of C-F, while these three samples still have with 3430 cm−1And 1730 cm−1With 1630 cm−1Centered on absorption peak, this illustrates in fluorinated graphene or there are these oxygen-containing groups such as this O-H, C=O
, this also indicates that not all oxygen-containing functional group has been converted to fluorine-containing functional group.
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 (7)
1. a kind of take fluorinated graphene as the preparation method of the carrier loaded nanoparticle for having mitoxantrone, special in terms of g and mL
Sign be the following steps are included:
1) container is cooled to 0 DEG C in ice-water bath, the 20-25 mL concentrated sulfuric acid is added；Then 0.5-2 g crystalline graphite powder is added
With 0.2-1 g sodium nitrate；It is ultrasonically treated 20-30 min；
2) it is stirred to react, keeps reaction temperature to be lower than 10 DEG C, then weigh 2-4 g potassium permanganate, in 25-30 min in batches
It is secondary to be slowly added to；Elementary reaction 1.5-2.5 h；
3) it is warming up to 35-40 DEG C, reacts 25-30 min；
4) 70-120 mL deionized water is measured, is slowly added to after ice-water bath is cooled to 0 DEG C；Then temperature adjustment is to 90-95
DEG C, continue to be stirred to react 25-30 min；
5) 50-70 mL distilled water stopped reaction is added, adds the H that 20-30 mL volume fraction is 25-35%2O2, continue to stir
React 15-20 min；
6) HCl solution that 30-50 mL volume fraction is 8-12% is added, stands 4-5 days；
7) supernatant of solution is first removed with dropper, Zai Qu lower layer viscous fluid centrifugal treating will be centrifuged until viscous fluid is in neutrality
Viscous fluid in pipe pours into evaporating dish, is freeze-dried 24-48 h, obtains graphene oxide sheet；
8) graphene oxide sheet is ground into graphene oxide powder；
9) 0.5-1.5 g graphene oxide powder and 20-40 mL methylene chloride or 1,2- dichloroethanes, stirring is added in another extracting container
10-14 h keeps its evenly dispersed；
10) 0.5-1 mL fluorization agent diethylaminosulfurtrifluoride is added dropwise, is then ultrasonically treated 4-6 h at room temperature, is stirred to react
24-72 h；
11) it is added after 15-30 mL methanol terminates reaction, is obtained by filtration partially fluorinated graphite ene product, and with ethyl alcohol and deionization
Water sufficiently washs, dry at 50-70 DEG C；
12) partially fluorinated graphene dispersion obtained by 0.05-0.1 g step 11) is delayed in the phosphate that 45-60 mL pH is 7.4
In fliud flushing, ultrasonic treatment obtains partially fluorinated graphene solution；
13) taking 0.8-1 mL concentration is that the mitoxantrone of 2 mg/ mL is slowly dropped into partially fluorinated graphene solution；It is protected from light and stirs
24-30 h is mixed, is centrifuged, particle is collected, is saved after the material freeze of lower layer is dry, being made has with fluorinated graphene to be carrier loaded
The nanoparticle of mitoxantrone.
2. it is as described in claim 1 it is a kind of with fluorinated graphene be the carrier loaded nanoparticle for having mitoxantrone preparation side
Method, which is characterized in that in step 2, stirring rate is 400-800 rpm, stirs 20-40 min.
3. it is as described in claim 1 it is a kind of with fluorinated graphene be the carrier loaded nanoparticle for having mitoxantrone preparation side
Method, which is characterized in that in step 6), during standing, every 1-2 d removes supernatant, and aliquots of deionized water is added.
4. it is as described in claim 1 it is a kind of with fluorinated graphene be the carrier loaded nanoparticle for having mitoxantrone preparation side
Method, which is characterized in that in step 7), centrifugal process specifically: supercentrifuge is used, respectively in 4000 rpm, 6000 rpm,
10 min are centrifuged under 8000 rpm, 10000 rpm, 12000 rpm, remove supernatant in centrifuge tube after centrifugation every time and be added etc.
Measure deionized water.
5. it is as described in claim 1 it is a kind of with fluorinated graphene be the carrier loaded nanoparticle for having mitoxantrone preparation side
Method, which is characterized in that each reaction that step 9), step 10), step 11) carry out carries out at room temperature.
6. it is as described in claim 1 it is a kind of with fluorinated graphene be the carrier loaded nanoparticle for having mitoxantrone preparation side
Method, which is characterized in that in step 12), ultrasonic treatment specifically: utilize ultrasonic wave under 630 W power of ultrasonic cell disruptor
Processing 2.5-3 h obtains the partially fluorinated graphene solution of evenly dispersed nano-scale.
7. it is as described in claim 1 it is a kind of with fluorinated graphene be the carrier loaded nanoparticle for having mitoxantrone preparation side
Method, which is characterized in that in step 13), centrifugation specifically: high-speed refrigerated centrifuge is used, in the revolving speed of 12000-16000 rpm
Lower centrifugation 7-15 min collects particle.
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