CN110522949A - A kind of load native copper/rhizome of davallia compound brushite preparation method - Google Patents

A kind of load native copper/rhizome of davallia compound brushite preparation method Download PDF

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CN110522949A
CN110522949A CN201911006486.9A CN201911006486A CN110522949A CN 110522949 A CN110522949 A CN 110522949A CN 201911006486 A CN201911006486 A CN 201911006486A CN 110522949 A CN110522949 A CN 110522949A
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davallia
rhizome
brushite
compound
powder
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CN110522949B (en
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赵三团
裴正军
李光大
张开丽
商文超
李朋斌
翟江波
景爱华
李景华
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Henan University of Science and Technology
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Abstract

A kind of load native copper/rhizome of davallia compound brushite preparation method, the specific method is as follows: weighing beta-calcium phosphate powder and a water calcium phosphate powder according to molar ratio 1.1:1, grind to obtain mixed powder A1, the calcium alginate microsphere that load has 3wt% Rhizoma Drynariae extract is added, grind to obtain mixed powder A2,1:2 weighs vinegar pyritum ignited and tri-distilled water in proportion, and it is 11:1 that mild fire, which is endured to ratio, and filter to get filtrate B；Liquor B is added in mixed powder A2 for 2.5:1 in proportion, tune mixes to obtain uniform lotion, which is inserted in mold, composite material is taken out to obtain after solidification.The present invention compares growth factor-loaded equal drugs, and price is less expensive, raw materials used simple and easy to get, efficacy stability is suitble to large-scale production, and brushite synthetic environment is utilized as acidity, and calcium alginate microsphere non-bloating feature in acid condition, keep the material system of complex microsphere more stable.

Description

A kind of load native copper/rhizome of davallia compound brushite preparation method
Technical field
The invention belongs to biomedical materials fields, and in particular to a kind of load native copper/rhizome of davallia compound brushite Preparation method.
Background technique
Native copper has a long history as the drug that synthetism is cured the wound in China.It is counted according to " Chinese medicinal formulae voluminous dictionary ", In 117 first prescriptions of two word of successive dynasties using names synthetism, 43 head are accounted for using native copper person, up to 36.8%.Research thinks that native copper is Ferrous mineral pyrite, iron content is abundant, is conducive to the formation of collagen in union early stage poroma, to the calcium of middle and advanced stage poroma Change also has facilitation.It can make a variety of enzymes also containing various trace elements necessary to the human bodies such as copper, zinc, manganese in native copper simultaneously Increased activity, promote collagenous fibres formed, calcium phosphorus precipitation, promote the formation of poroma.
The rhizome of davallia is that another taste often uses Chinese medicine synthetism good medicine.Modern pharmacy is studies have shown that Rhizoma Drynariae extract can promote The expression of bone growth factor significantly increases the proliferation of osteoblast, calcification and New bone formation conducive to bone, increases poroma thickness, Improve healing of fracture.Meanwhile Process of Total Flavonoids in Drynaria Fortunei acute toxicity testing shows diet, work after mouse, rat oral gavage administration Dynamic, state of mind shackles body chain variation without exception, clinical application good security can be used with longer-term.The rhizome of davallia and nature Copper is decocted as traditional orthopaedics synthetism good medicine, the two usually compatible use together even across high temperature, and drug effect is still able to maintain surely It is fixed.
Brushite is calcium phosphate dibasic dihydrate, is clinically common a kind of calcium phosphate bone repair materials, chemical group Divide, good biocompatibility close with skeleton inorganic component, degradation property is excellent.Since brushite is synthesizing often by phosphorus Hydrochlorate solid phase powder reconciles with aqueous solution liquid phase, therefore this kind of synthos are highly suitable as the load system of drug, Drug controlled release.In order to further increase the Bone Defect Repari performance of brushite, it is raw that all kinds of activity are often loaded on brushite Object molecule, such as bone morphogenetic protein and insulin-like growth factor.But the most price of these active biomolecules is very high It is expensive, at the same half-life short, it is easily free, height is required to composite material preparation process, and the material shelf-life is shorter, increases material Cost of manufacture also aggravates the financial burden of patient in clinical use.
Summary of the invention
In view of the above technical problems, the brushite being had excellent performance using Bone Defect Repari selects Chinese medicine othopedics clinically as matrix Two taste synthetism good medicine ----native copper and the rhizomes of davallia being often used, according to the feature of native copper, the rhizome of davallia and brushite respectively, Two taste Chinese medicines and brushite are compound, it is made and carries native copper/rhizome of davallia compound brushite.
The technical scheme is that a kind of load native copper/rhizome of davallia compound brushite preparation method, specific method It is as follows:
Step 1: weighing beta-calcium phosphate powder according to the ratio of molar ratio 1.1:1 and a water calcium phosphate powder is put into mortar, grind Grind to obtain mixed powder A1；
Step 2: the calcium alginate microsphere that load has 3wt% Rhizoma Drynariae extract is added in mixed powder A1, mixing is ground to obtain Powder A2；
Step 3: 1:2 weighs vinegar pyritum ignited and tri-distilled water in proportion, wherein vinegar pyritum ignited is calculated in gram, and tri-distilled water is with milli It rises and calculates, after boiling, it is 11: 1 that mild fire, which is endured to ratio, and liquor B is obtained by filtration；
Step 4: the proportionally ratio of 2.5:1, liquor B is added in mixed powder A2, wherein mixed powder A2 is in gram It calculates, liquor B is calculated with milliliter, mixes 20s using stainless steel knife tune, obtain uniform lotion, which is inserted in mold, to lotion It is taken out after solidification, the composite material of regular shape can be obtained.
It advanced optimizes, milling time is 15min in the step 1, and milling time is 5min in step 2.
It advanced optimizes, the diameter of calcium alginate microsphere is 300-800 μm in the step 2.
It advanced optimizes, the additional amount of calcium alginate microsphere is 1 wt% of powder gross mass in the step 2.
It advanced optimizes, in the step 2, calcium alginate microsphere specific is the preparation method comprises the following steps: choose Rhizoma Drynariae extract It is ground to powder, is added in 1.5-2.5wt% sodium alginate soln, extracts using syringe after mixing evenly and is added dropwise to 2-6 wt%CaCl2In solution, forms microballoon and stand crosslinking, which is immersed in citric acid solution after deionized water is washed, then Pre-freeze, freezing after secondary washing.
It advanced optimizes, the citric acid solution is the 0.5M citric acid solution containing 1 wt% chitosan.
The beneficial effects of the present invention are:
One, for the brushite being had excellent performance using Bone Defect Repari as matrix, the two taste synthetisms for selecting Chinese medicine othopedics to be clinically often used are good Medicine ----native copper and the rhizome of davallia, two taste Chinese medicines and brushite are compound, and rhizome of davallia drug therein is by the way of microballoon Load selects for Rhizoma Drynariae extract to be carried on diameter on 300-800 μm of calcium alginate microsphere, wherein 95% or more is distributed At 300-800 μm, 75% or more is distributed in 300-600 μm, is prepared under environment using calcium alginate microsphere in the acidity of brushite More stable, solid and non-swelling feature maintains the release of stablizing of Rhizoma Drynariae extract, meanwhile, it is imitated using the occupy-place of microballoon It answers, forms hole of corresponding size after its degradation, it is viscous to facilitate cell for 300-800 μm of bionic tone tissue of porous anatomical structure Echo growth；Native copper medicament selection is loaded by way of being brewed into certain concentration medical fluid, will be loaded with the alginic acid of the rhizome of davallia Calcium microballoon and beta-calcium phosphate and two kinds of phosphate of calcium dihydrogen phosphate are compound, are prepared into the composite phosphate raw material for carrying the rhizome of davallia, will The medical fluid that native copper is brewed into debita spissitudo does solidify liquid, and composite phosphate raw material and native copper medical fluid are reconciled, solid to it After change, native copper/rhizome of davallia compound brushite is made；
Two, native copper and the rhizome of davallia are cheap as traditional Chinese medicine, are combined on brushite, compared to growth factor-loaded etc. Drug, price are less expensive；Raw materials used simple and easy to get, efficacy stability is suitble to large-scale production, and brushite synthesis ring is utilized Border is acidity, and calcium alginate microsphere non-bloating feature in acid condition, keeps the material system of complex microsphere more stable.
Detailed description of the invention
Fig. 1 is the cross-section diagram of embodiment 1
Fig. 2 is the cross-section diagram of embodiment 2
Fig. 3 is the cross-section diagram of embodiment 3
Fig. 4 is the pure material cross-section diagram that microballoon is not added
Fig. 5 is the MTT vegetative map of embodiment 1-3.
Specific embodiment
A specific embodiment of the invention are as follows:
Embodiment 1
A kind of load native copper/rhizome of davallia compound brushite preparation method, includes the following steps:
Step 1: according to the ratio of molar ratio 1.1:1 weigh sieving 200 mesh beta-calcium phosphate powder and a water calcium phosphate powder put Enter in mortar, grinds 15min, obtain mixed powder A1；
Step 2: preparing 1.5wt% sodium alginate soln, 2wt%CaCl2Solution and 0.5M citric acid containing 1 wt% chitosan are molten Liquid chooses Rhizoma Drynariae extract and is ground to powder, be added in sodium alginate soln, extracted and dripped using syringe after mixing evenly CaCl is added2In solution, forms microballoon and stand crosslinking 4h, which is immersed in citric acid solution after deionized water is washed In, pre-freeze for 24 hours, must have been loaded with freeze drier freeze-drying 6h at being -80 DEG C in temperature after being washed with deionized again The calcium alginate microsphere for accounting for 1 wt% of powder A1 gross mass is added in powder A1 for the calcium alginate microsphere of 3wt% Rhizoma Drynariae extract, The diameter of the calcium alginate microsphere is distributed in 300-800 μm for 95% or more, and 75% or more is distributed in 300-600 μm, grinds 5min Obtain mixed powder A2；
Step 3: 1:2 weighs vinegar pyritum ignited and tri-distilled water in proportion, wherein vinegar pyritum ignited is calculated in gram, and tri-distilled water is with milli It rises and calculates, after boiling, it is 11:1 that mild fire, which is endured to vinegar pyritum ignited and tri-distilled water ratio, and liquor B is obtained by filtration；
Step 4: the proportionally ratio of 2.5:1, liquor B is added in mixed powder A2, wherein mixed powder A2 is in gram It calculates, liquor B is calculated with milliliter, then mixes 20s using stainless steel knife tune, obtain uniform lotion, lotion is inserted in mold, to cream It is taken out after body solidification, the i.e. composite material of regular shape can be obtained.
Embodiment 2
A kind of load native copper/rhizome of davallia compound brushite preparation method, includes the following steps:
Step 1: according to the ratio of molar ratio 1.1:1 weigh sieving 200 mesh beta-calcium phosphate powder and a water calcium phosphate powder put Enter in mortar, grinds 15min, obtain mixed powder A1；
Step 2: preparing 2wt% sodium alginate soln, 4wt%CaCl2Solution and 0.5M citric acid solution containing 1 wt% chitosan, It chooses Rhizoma Drynariae extract and is ground to powder, be added in sodium alginate soln, extract and be added dropwise using syringe after mixing evenly Enter CaCl2In solution, forms microballoon and stand crosslinking 4h, which is immersed in citric acid solution after deionized water is washed, Pre-freeze for 24 hours, must load 3wt% with freeze drier freeze-drying 6h at being -80 DEG C in temperature after being washed with deionized again The calcium alginate microsphere for accounting for 1 wt% of powder A1 gross mass is added in the calcium alginate microsphere of Rhizoma Drynariae extract in powder A1, should The diameter of calcium alginate microsphere is distributed in 300-800 μm for 95% or more, and 75% or more is distributed in 300-600 μm, and grinding 5min is obtained Mixed powder A2；
Step 3: 1:2 weighs vinegar pyritum ignited and tri-distilled water in proportion, wherein vinegar pyritum ignited is calculated in gram, and tri-distilled water is with milli It rises and calculates, after boiling, it is 11g:1ml that mild fire, which is endured to solid-to-liquid ratio, and liquor B is obtained by filtration；
Step 4: the proportionally ratio of 2.5:1, liquor B is added in mixed powder A2, wherein mixed powder A2 is in gram It calculates, liquor B is calculated with milliliter, then mixes 20s using stainless steel knife tune, obtain uniform lotion, lotion is inserted in mold, to cream It is taken out after body solidification, the i.e. composite material of regular shape can be obtained.
Embodiment 3
A kind of load native copper/rhizome of davallia compound brushite preparation method, includes the following steps:
Step 1: according to the ratio of molar ratio 1.1:1 weigh sieving 200 mesh beta-calcium phosphate powder and a water calcium phosphate powder put Enter in mortar, grinds 15min, obtain mixed powder A1；
Step 2: preparing 2.5wt% sodium alginate soln, 6 wt%CaCl2Solution and 0.5M citric acid containing 1 wt% chitosan are molten Liquid chooses Rhizoma Drynariae extract and is ground to powder, be added in sodium alginate soln, extracted and dripped using syringe after mixing evenly CaCl is added2In solution, forms microballoon and stand crosslinking 4h, which is immersed in citric acid solution after deionized water is washed In, pre-freeze for 24 hours, must have been loaded with freeze drier freeze-drying 6h at being -80 DEG C in temperature after being washed with deionized again The calcium alginate microsphere of 3wt% Rhizoma Drynariae extract, in powder A1 be added account for 1 wt% of powder A1 gross mass calcium alginate it is micro- The diameter of ball, the calcium alginate microsphere is distributed in 300-800 μm for 95% or more, and 75% or more is distributed in 300-600 μm, grinding 5min obtains mixed powder A2；
Step 3: 1:2 weighs vinegar pyritum ignited and tri-distilled water in proportion, wherein vinegar pyritum ignited is calculated in gram, and tri-distilled water is with milli It rises and calculates, after boiling, it is 11g:1ml that mild fire, which is endured to solid-to-liquid ratio, and filtering obtains liquor B；
Step 4: the proportionally ratio of 2.5:1, liquor B is added in mixed powder A2, wherein mixed powder A2 is in gram It calculates, liquor B is calculated with milliliter, then mixes 20s using stainless steel knife tune, obtain uniform lotion, lotion is inserted in mold, to cream It is taken out after body solidification, the i.e. composite material of regular shape can be obtained.
Drug bearing microsphere obtained by embodiment 1-3 is subjected to Shape measure and cytotoxicity detection, wherein Shape measure is logical It crosses and is taken pictures using digital camera, observe the cross-section morphology of material, Fig. 1 is 1 section of case study on implementation, and display microballoon dispersion is embedded into In epiglaubite matrix, simultaneously because separately removing, can also observe the hole that microballoon occupy-place leaves；Fig. 2 is 2 section of embodiment, Show that many microballoon dispersions are embedded into brushite matrix, simultaneously because separately removing, can also observe that microballoon occupy-place is stayed Under hole；Fig. 3 is 3 section of embodiment, shows that a large amount of microballoon dispersions are embedded into brushite matrix, simultaneously because separately stripping From can also observe the hole that microballoon occupy-place leaves, Fig. 4 is the blank control group that microballoon is not added, it is seen that material is fine and close；Cell Toxicity detection detects MTT method by using the cytotoxicity in national standard GB/T 16886.5-2017, uses the leaching liquor of material Cytotoxicity is detected, the use of cell is Human osteoblast-like cell MG63, cell Initial seeding density is 3000 thin in 96 orifice plates Born of the same parents/hole, testing result are as shown in Figure 5, it is seen that and the absorbance value OD of embodiment 1-3 is above the blank control group that microballoon is not added, Show material no cytotoxicity, while showing there is certain stimulation to the growth of cell.
Main feature of the invention, application method, basic principle and advantages of the present invention has been shown and described above.This Industry technology personnel are it should be appreciated that the present invention is not limited to the above embodiments, described in above-described embodiment and invention book only It is invention the principle of the present invention, without departing from the spirit and scope of the present invention, the present invention can also have according to the actual situation Various changes and modifications, these changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention It is defined by the appending claims and its equivalent thereof.

Claims (6)

1. a kind of load native copper/rhizome of davallia compound brushite bone renovating material preparation method, which is characterized in that specific method It is as follows:
Step 1: weighing beta-calcium phosphate powder according to the ratio of molar ratio 1.1:1 and a water calcium phosphate powder is put into mortar, grind Grind to obtain mixed powder A1；
Step 2: the calcium alginate microsphere that load has 3wt% Rhizoma Drynariae extract is added in mixed powder A1, mixing is ground to obtain Powder A2；
Step 3: 1:2 weighs vinegar pyritum ignited and tri-distilled water in proportion, wherein vinegar pyritum ignited is calculated in gram, and tri-distilled water is with milli It rises and calculates, after boiling, it is 11:1 that mild fire, which is endured to ratio, and liquor B is obtained by filtration；
Step 4: the proportionally ratio of 2.5:1, liquor B is added in mixed powder A2, wherein mixed powder A2 is with milligram It calculates, liquor B is calculated with milliliter, mixes 20s using stainless steel knife tune, obtain uniform lotion, which is inserted in mold, to cream It is taken out after body solidification, the composite material of regular shape can be obtained.
2. a kind of load native copper/rhizome of davallia compound brushite bone renovating material preparation method according to claim 1, It is characterized in that, milling time is 15min in the step 1, milling time is 5min in step 2.
3. a kind of load native copper/rhizome of davallia compound brushite bone renovating material preparation method according to claim 1, It is characterized in that, the diameter of calcium alginate microsphere is 300-800 μm in the step 2.
4. a kind of load native copper/rhizome of davallia compound brushite bone renovating material preparation method according to claim 1, It is characterized in that, the additional amount of calcium alginate microsphere is 1 wt% of powder gross mass in the step 2.
5. a kind of load native copper/rhizome of davallia compound brushite bone renovating material preparation method according to claim 1, It is characterized in that, in the step 2, calcium alginate microsphere it is specific the preparation method comprises the following steps: choosing Rhizoma Drynariae extract is ground to powder End is added in 1.5-2.5wt% sodium alginate soln, is extracted using syringe after mixing evenly and is added dropwise to 2-6 wt%CaCl2 It in solution, forms microballoon and stands crosslinking, which is immersed in citric acid solution after deionized water is washed, after washing again Pre-freeze, freezing.
6. a kind of load native copper/rhizome of davallia compound brushite bone renovating material preparation method according to claim 5, It is characterized in that, the citric acid solution is the 0.5M citric acid solution containing 1 wt% chitosan.
CN201911006486.9A 2019-10-22 2019-10-22 Preparation method of compound brushite carrying native copper/rhizoma drynariae Active CN110522949B (en)

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