CN106829913A - A kind of preparation method of mesoporous carbosphere of bio-based and its application in 5 fluorouracil slow releases - Google Patents
A kind of preparation method of mesoporous carbosphere of bio-based and its application in 5 fluorouracil slow releases Download PDFInfo
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- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
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- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/33—Heterocyclic compounds
- A61K31/395—Heterocyclic compounds having nitrogen as a ring hetero atom, e.g. guanethidine or rifamycins
- A61K31/495—Heterocyclic compounds having nitrogen as a ring hetero atom, e.g. guanethidine or rifamycins having six-membered rings with two or more nitrogen atoms as the only ring heteroatoms, e.g. piperazine or tetrazines
- A61K31/505—Pyrimidines; Hydrogenated pyrimidines, e.g. trimethoprim
- A61K31/513—Pyrimidines; Hydrogenated pyrimidines, e.g. trimethoprim having oxo groups directly attached to the heterocyclic ring, e.g. cytosine
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- A61K9/0002—Galenical forms characterised by the drug release technique; Application systems commanded by energy
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Abstract
It is directly raw material with discarded oil-tea camellia husks the invention discloses one kind, the method that annealing and potassium hydroxide chemical activation technology preparation mesoporous carbon microsphere drug slow-released carrier are combined by hydrothermal carbonization.The structure of meso-hole structure makes prepared material have extra specific surface area（2081 m2/g）And to the superelevation adsorption capacity of the fluorouracil of cancer therapy drug 5（480.9 mg/g）.In SR test, the sustained release percentage of 5 fluorouracils is up to 67.4%.Because the raw material used in the preparation of mesoporous carbosphere is thick abandoned biomass, therefore compared with the conventional medicament slow-released carrier such as mesoporous silicon oxide, prepared material has stronger bio-compatibility.Used as a kind of slow releasing carrier of medication, the structure of the spherical microstructure of small size makes prepared material be expected to realize sustained release in biological cell.The use of simple preparation technology and low cost feedstock significantly reduces the cost of prepared bio-based mesoporous carbon microsphere drug slow-released carrier, therefore is adapted to large-scale production.
Description
Technical field
The invention belongs to abandoned biomass resource and slow releasing carrier of medication development field, bio-based mesoporous carbon is related generally to
The preparation method of microballoon and its application in cancer therapy drug 5 FU 5 fluorouracil sustained release.
Background technology
The exploitation of meso-porous carbon material is always important advanced subject in material science.In recent years, mesoporous carbon materials
Material has been widely used as adsorbent, energy storage material, catalyst carrier and medicinal slow release agent.At present, soft/hard template strategy is to be permitted
The method of the synthesising mesoporous carbon material that many scientists are widely recognized as.However, the use of high cost raw material and cumbersome operating procedure
The serious practical application for limiting the meso-porous carbon material prepared by soft/hard template strategy.
Biomass by hydro-thermal carbonization is a kind of low-cost environmental-protecting strategy for preparing carbon material.With spherical microstructure and fragrance
The carbon material of carbon skeleton can be by the hydrothermal carbonization mistake of some one-component biomass such as glucose, fructose, xylose, furfural, sucrose
Journey is easily obtained.Importantly, some scientists directly using thick abandoned biomass be raw material by hydrothermal carbonization technology into
Work(prepares the carbon material with potential using value.The cycling and reutilization of thick abandoned biomass not only reduces the life of carbon material
Produce cost and be conducive to environmental protection.However, due to the complicated component of thick abandoned biomass, directly using thick abandoned biomass
For raw material by the way that carbon material generally existing impurity prepared by hydrothermal carbonization technology is more, pattern difference the problems such as.
Compared with soft/hard template strategy, potassium hydroxide chemical activation is one kind low cost and the letter for preparing porous carbon materials
Single strategy.However, micro-pore carbon material can only be prepared by potassium hydroxide chemical activation strategy.Absorption, energy storage, catalysis with
And during medicament slow release, because microcellular structure increased the resistance to mass tranfer between carbon material and target molecule, therefore by hydrogen
The practical application of porous carbon materials prepared by potassium oxide chemical activation strategy is severely limited.
The content of the invention
It is an object of the invention to provide a kind of preparation method of the mesoporous carbosphere of bio-based, and prepared bio-based is situated between
Hole carbosphere is applied to the sustained release of cancer therapy drug 5 FU 5 fluorouracil.
The present invention is such to work with implementation, a kind of preparation method of the mesoporous carbosphere of bio-based, it is characterised in that
The method comprises the following steps：
（1）A certain amount of discarded oil-tea camellia husks powder and phloroglucin are added into deionized water respectively, it is fully swelling after will be outstanding
Turbid liquid carries out hydro-thermal reaction in being transferred to polytetrafluoroethyllining lining stainless steel hydrothermal reaction kettle；
（2）With water as solvent, through surname extraction and microwave and ultrasonic wave synergic extraction step after, be obtained fragrance carbosphere；
（3）Under an argon atmosphere, prepared fragrant carbosphere is made annealing treatment, annealing carbosphere is obtained；
（4）Prepared annealing carbosphere is placed in 3h is stirred vigorously in potassium hydroxide aqueous solution, be subsequently placed in general in 60 DEG C of baking ovens
Moisture in suspension is evaporated；
（5）Under an argon atmosphere, by the mixture calcining of anneal carbosphere and potassium hydroxide, wash with water to neutrality and micropore is obtained
Carbosphere；
（6）Prepared micropore carbosphere is continued to press step（4）With（5）Processed, mesoporous carbosphere is finally obtained；
（7）Proved by field emission scanning electron microscope, transmission electron microscope and nitrogen porosity analysis and characterization, via
It is above-mentioned（1）~（6）Discarded oil-tea camellia husks successfully can be converted into mesoporous carbosphere by step.
Step（1）The raw material for being used is waste gas oil-tea camellia husks powder, phloroglucin, oil-tea camellia husks powder, deionized water
Mass ratio be 1：4：150, the compactedness of hydrothermal reaction kettle is 60%, and hydrothermal temperature is 230 DEG C, and the hydro-thermal reaction time is
24h, hydro-thermal reaction heating rate is 1 DEG C/min.
Step（3）In annealing temperature be 650 DEG C, annealing time is 2h, and heating rate is 5 DEG C/min.
Step（4）Middle annealing carbosphere, potassium hydroxide, the mass ratio of deionized water are 1：2：20.
Step（5）In calcining heat be 850 DEG C, calcination time is 2h, and heating rate is 5 DEG C/min.
Used as a kind of slow releasing carrier of medication, the prepared mesoporous carbosphere of bio-based of the present invention can be applied to cancer therapy drug 5- fluorine
The sustained release of uracil, operating procedure is as follows：
（1）A certain amount of mesoporous carbosphere and the finite concentration 5 FU 5 fluorouracil aqueous solution are mixed, at room temperature acutely after concussion 24h,
The mesoporous carbosphere of adsorption saturation is collected by filtration and 12h is vacuum dried at 60 DEG C.
（2）The mesoporous carbosphere of adsorption saturation is transferred in beaker, to beaker under the conditions of flow velocity is 0.5 mL/min
In slowly add water.Because adsorbate has concentration difference between solvent and adsorbent, therefore 5 FU 5 fluorouracil can be from adsorption saturation
Mesoporous carbosphere in be sustained out.
（3）The absorption to 5 FU 5 fluorouracil and slow release effect with the mesoporous carbosphere of high-efficient liquid phase chromatogram technique monitoring.
To make load of the mesoporous carbosphere to 5 FU 5 fluorouracil reach extreme value, step（1）Intermediary hole carbosphere and 5- fluorine are urinated
Mass fraction of the pyrimidine in water phase should be 800 mg/L.
The advantage of the invention is that：Under the structure-directing effect of phloroglucin, successfully will be useless by hydrothermal carbonization technology
Abandon oil-tea camellia husks and be converted into the perfect fragrance carbosphere of pattern, then potassium hydroxide chemistry is living by annealing and twice
Prepared fragrant carbosphere is successfully converted into mesoporous carbosphere by change process；The successful structure of meso-hole structure, makes prepared material
With extra specific surface area（2081 m2/g）And to the superelevation adsorption capacity of 5 FU 5 fluorouracil（480.9 mg/g）；Due to
Used thick waste biomass materials in the preparation of mesoporous carbosphere, thus with the conventional medicament slow-released carrier such as mesoporous silicon oxide
Compare, prepared material has stronger bio-compatibility；As a kind of slow releasing carrier of medication, the spherical microstructure of small size
Structure makes prepared material be expected to realize sustained release in biological cell；The use of simple manufacturing process and low cost feedstock, makes institute
The cost for preparing bio-based mesoporous carbon microsphere drug slow-released carrier is significantly reduced, therefore is adapted to large-scale production.
Brief description of the drawings
Fig. 1 is the Flied emission scanning electron microscopy of the mesoporous carbosphere of bio-based prepared by the method in embodiment 1
Mirror（A and b）And transmission electron microscope（c）Photo.It can be seen that from FIG. 1 a that the prepared mesoporous carbosphere of bio-based has had
Beautiful spherical microstructure.As can be seen that by annealing and potassium hydroxide chemical activating process twice from Fig. 1 b and 1c
Succeeded in carbosphere surface construction meso-hole structure.
Fig. 2 is the nitrogen adsorption-desorption isotherm of the mesoporous carbosphere of bio-based prepared by the method in embodiment 1
And pore size distribution curve.There is the IV type thermoisopleths that H2 is detained ring to show, annealing and twice potassium hydroxide chemistry in Fig. 2 a
After activation, meso-hole structure successfully builds on carbosphere surface.As can be seen that the mesoporous carbosphere tool of prepared bio-based from Fig. 2 b
There is homogeneous hole size, most probable pore size is 3.6 nm.
Fig. 3 is absorption and extended release kinetics curve of the mesoporous carbosphere of prepared bio-based to 5 FU 5 fluorouracil.From Fig. 3 a
In as can be seen that because with meso-hole structure and extra specific surface area, the prepared mesoporous carbosphere of bio-based is urinated 5- fluorine in water
The absorption of pyrimidine is with high capacity and the speed being exceedingly fast.The slow process that adds water from Fig. 3 b as can be seen that in beaker
In, because adsorbate has concentration difference between solvent and adsorbent, 5 FU 5 fluorouracil can be from the mesoporous carbosphere of adsorption saturation
Out, sustained release percentage is up to 67.4% for middle sustained release.
Specific embodiment
Embodiment 1
The discarded oil-tea camellia husks for reclaiming are washed and at 60 DEG C 12h is dried, is then placed in being crushed in disintegrating machine, cross 200
Closed preservation after mesh sieve.1.6g oil-tea camellia husks powder and 0.4g phloroglucins are added into 60ml deionized waters respectively, then
With 500W ultrasonic cleaner ultrasonic disperses 1h.After 6h is stirred at room temperature, it is poly- the four of 100ml that suspension is transferred into volume
In PVF inner liner stainless steel hydrothermal reaction kettle, the hydro-thermal reaction 24h at 230 DEG C, the heating rate of hydro-thermal reaction for 1 DEG C/
min.After reaction terminates, with water as solvent, fragrance carbosphere is obtained through surname extraction and microwave and ultrasonic wave synergic extraction step.
Under argon gas atmosphere, prepared fragrant carbosphere is carried out into annealing 2h under the conditions of 650 DEG C of heating rates are 5 DEG C/min, made
Must be annealed carbosphere.Annealing carbosphere and 0.6g potassium hydroxide will be placed in 6mL water prepared by 0.3g, will be hanged after being stirred vigorously 3h
Turbid liquid is placed in 60 DEG C of baking ovens and is evaporated moisture.Under an argon atmosphere, by the mixture of anneal carbosphere and potassium hydroxide 850
DEG C heating rate is to calcine 2h under the conditions of 5 DEG C/min, washes with water to neutrality and micropore carbosphere is obtained.Prepared microporous carbon is micro-
Ball continues to be processed by above-mentioned potassium hydroxide chemical activation step, and it is mesoporous that micropore is expanded in activation process, is finally obtained
Mesoporous carbosphere.By field emission scanning electron microscope, transmission electron microscope and nitrogen analysis of porosity to characterize
Prepare the pattern and meso-hole structure of material.Result shows that prepared material has perfect spherical microstructure and size uniformity
Meso-hole structure（Fig. 1 and Fig. 2）.
Embodiment 2
The mesoporous carbosphere of bio-based prepared by 40mg and the 5 FU 5 fluorouracil aqueous solution that 50mL concentration is 800 mg/L are mixed.Room
After the lower acutely concussion 24h of temperature, the mesoporous carbosphere of adsorption saturation is collected by filtration and 12h is vacuum dried at 60 DEG C.Absorption is full
The mesoporous carbosphere of sum is transferred in beaker, is slowly added water under the conditions of flow velocity is 0.5 mL/min to beaker, urinates 5- fluorine
Pyrimidine is sustained out from the mesoporous carbosphere of adsorption saturation.Phonetic is urinated to 5- fluorine with the mesoporous carbosphere of high-efficient liquid phase chromatogram technique monitoring
The absorption of pyridine and slow release effect.Result shows, due to meso-hole structure and extra specific surface area, prepared bio-based mesoporous carbon
Microballoon is to the absorption of 5 FU 5 fluorouracil in water with high capacity and the speed being exceedingly fast（Fig. 3 a）.Slowly added water in beaker
During, because adsorbate has concentration difference between solvent and adsorbent, 5 FU 5 fluorouracil can be from the mesoporous carbon of adsorption saturation
It is sustained out in microballoon, sustained release percentage is up to 67.4%（Fig. 3 b）.
Claims (7)
1. the preparation method of the mesoporous carbosphere of a kind of bio-based, it is characterised in that the method comprises the following steps；
（1）A certain amount of discarded oil-tea camellia husks powder and phloroglucin are added into deionized water respectively, it is fully swelling after will be outstanding
Turbid liquid carries out hydro-thermal reaction in being transferred to polytetrafluoroethyllining lining stainless steel hydrothermal reaction kettle；
（2）With water as solvent, through surname extraction and microwave and ultrasonic wave synergic extraction step after, be obtained fragrance carbosphere；
（3）Under an argon atmosphere, prepared fragrant carbosphere is made annealing treatment, annealing carbosphere is obtained；
（4）Prepared annealing carbosphere is placed in 3h is stirred vigorously in potassium hydroxide aqueous solution, be subsequently placed in general in 60 DEG C of baking ovens
Moisture in suspension is evaporated；
（5）Under an argon atmosphere, by the mixture calcining of anneal carbosphere and potassium hydroxide, wash with water to neutrality and micropore is obtained
Carbosphere；
（6）Prepared micropore carbosphere is continued to press step（4）With（5）Processed, mesoporous carbosphere is finally obtained；
（7）Proved by field emission scanning electron microscope, transmission electron microscope and nitrogen porosity analysis and characterization, via
It is above-mentioned（1）~（6）Discarded oil-tea camellia husks successfully can be converted into mesoporous carbosphere by step.
2. the preparation method of the mesoporous carbosphere of a kind of bio-based described in claim 1, it is characterised in that：Step（1）Made
Raw material is waste gas oil-tea camellia husks powder, and phloroglucin, oil-tea camellia husks powder, the mass ratio of deionized water are 1：4：150, water
The compactedness of thermal response kettle is 60%, and hydrothermal temperature is 230 DEG C, and the hydro-thermal reaction time is 24h, hydro-thermal reaction heating rate
It is 1 DEG C/min.
3. the preparation method of the mesoporous carbosphere of a kind of bio-based described in claim 1, it is characterised in that：Step（3）In
Annealing temperature is 650 DEG C, and annealing time is 2h, and heating rate is 5 DEG C/min.
4. the preparation method of the mesoporous carbosphere of a kind of bio-based described in claim 1, it is characterised in that：Step（4）In move back
Fiery carbosphere, potassium hydroxide, the mass ratio of deionized water are 1：2：20.
5. the preparation method of the mesoporous carbosphere of a kind of bio-based described in claim 1, it is characterised in that：Step（5）In
Calcining heat is 850 DEG C, and calcination time is 2h, and heating rate is 5 DEG C/min.
6. the mesoporous carbosphere of bio-based described in a kind of claim 1 is applied to the release method of 5 FU 5 fluorouracil, its feature
It is to comprise the following steps：
（1）A certain amount of mesoporous carbosphere and the finite concentration 5 FU 5 fluorouracil aqueous solution are mixed, at room temperature acutely after concussion 24h,
The mesoporous carbosphere of adsorption saturation is collected by filtration and 12h is vacuum dried at 60 DEG C；
（2）The mesoporous carbosphere of adsorption saturation is transferred in beaker, is delayed under the conditions of flow velocity is 0.5 mL/min to beaker
Slowly add water, because adsorbate has concentration difference between solvent and adsorbent, therefore 5 FU 5 fluorouracil can be from Jie of adsorption saturation
It is sustained out in the carbosphere of hole；
（3）The absorption to 5 FU 5 fluorouracil and slow release effect with the mesoporous carbosphere of high-efficient liquid phase chromatogram technique monitoring.
7. the mesoporous carbosphere of bio-based described in claim 6 is applied to the release method of 5 FU 5 fluorouracil, it is characterised in that：
To make load of the mesoporous carbosphere to 5 FU 5 fluorouracil reach extreme value, step（1）Intermediary hole carbosphere and 5 FU 5 fluorouracil are in water
Mass fraction in phase should be 800 mg/L.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| TWI639437B (en) * | 2017-08-17 | 2018-11-01 | 逢甲大學 | Medicine for treating or preventing gastric cancer |
| CN114853008A (en) * | 2022-04-28 | 2022-08-05 | 广西大学 | Preparation and application of camellia husk modified activated carbon adsorption decolorant |
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| CN103990133A (en) * | 2014-05-07 | 2014-08-20 | 沈阳药科大学 | Mesoporous carbon nanoparticle system with targeting site-specific drug release and application thereof |
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| CN103663450A (en) * | 2013-12-19 | 2014-03-26 | 中国科学院过程工程研究所 | Carbon microspheres with high specific surface area and preparation method for carbon microspheres with high specific surface area |
| CN103990133A (en) * | 2014-05-07 | 2014-08-20 | 沈阳药科大学 | Mesoporous carbon nanoparticle system with targeting site-specific drug release and application thereof |
| CN105883805A (en) * | 2016-04-20 | 2016-08-24 | 南昌航空大学 | Preparation method of camellia seed shell based carbon microspheres with high specific surface area |
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| TWI639437B (en) * | 2017-08-17 | 2018-11-01 | 逢甲大學 | Medicine for treating or preventing gastric cancer |
| CN114853008A (en) * | 2022-04-28 | 2022-08-05 | 广西大学 | Preparation and application of camellia husk modified activated carbon adsorption decolorant |
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