CN103585638A - Preparation method for sodium alginate and calcium carbonate hybrid particles - Google Patents
Preparation method for sodium alginate and calcium carbonate hybrid particles Download PDFInfo
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- CN103585638A CN103585638A CN201310590485.XA CN201310590485A CN103585638A CN 103585638 A CN103585638 A CN 103585638A CN 201310590485 A CN201310590485 A CN 201310590485A CN 103585638 A CN103585638 A CN 103585638A
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- sodium alginate
- solution
- calcium carbonate
- hybrid particles
- sodium
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- 239000000661 sodium alginate Substances 0.000 title claims abstract description 22
- 229940005550 sodium alginate Drugs 0.000 title claims abstract description 22
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 235000010413 sodium alginate Nutrition 0.000 title claims abstract description 18
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 title claims abstract description 16
- 229910000019 calcium carbonate Inorganic materials 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000002245 particle Substances 0.000 title claims abstract description 11
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 27
- 239000000243 solution Substances 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 17
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 14
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 14
- 239000011734 sodium Substances 0.000 claims abstract description 14
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 14
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 13
- 239000002904 solvent Substances 0.000 claims abstract description 8
- 239000011259 mixed solution Substances 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000012153 distilled water Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims 1
- 239000011575 calcium Substances 0.000 claims 1
- 229910052791 calcium Inorganic materials 0.000 claims 1
- 239000001110 calcium chloride Substances 0.000 claims 1
- 229910001628 calcium chloride Inorganic materials 0.000 claims 1
- 238000005660 chlorination reaction Methods 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000008187 granular material Substances 0.000 description 15
- 229960001193 diclofenac sodium Drugs 0.000 description 8
- JGMJQSFLQWGYMQ-UHFFFAOYSA-M sodium;2,6-dichloro-n-phenylaniline;acetate Chemical compound [Na+].CC([O-])=O.ClC1=CC=CC(Cl)=C1NC1=CC=CC=C1 JGMJQSFLQWGYMQ-UHFFFAOYSA-M 0.000 description 8
- 239000003814 drug Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- UEJWRQDKIBEMCR-UHFFFAOYSA-L calcium;sodium;carbonate Chemical compound [Na+].[Ca+2].[O-]C([O-])=O UEJWRQDKIBEMCR-UHFFFAOYSA-L 0.000 description 4
- 238000009388 chemical precipitation Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 239000004531 microgranule Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000005191 phase separation Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000001694 spray drying Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003937 drug carrier Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000003981 vehicle Substances 0.000 description 1
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Abstract
本发明涉及一种海藻酸钠-碳酸钙杂化颗粒的制备方法，包括：70-80℃条件下，将海藻酸钠加入溶剂中，得到海藻酸钠溶液；在室温条件下，分别配制碳酸钠、氯化钙溶液；将海藻酸钠溶液加入碳酸钠溶液中，搅拌，得到混合溶液；将氯化钙溶液迅速加入上述混合溶液中，搅拌，离心，干燥，即得。本发明所使用的原料廉价易得，具有良好的生物可降解性及生物相容性，具有应用及其做后续相关实验分析的潜力。
The invention relates to a preparation method of sodium alginate-calcium carbonate hybrid particles, comprising: adding sodium alginate into a solvent at 70-80°C to obtain a sodium alginate solution; and preparing sodium carbonate respectively at room temperature 1. Calcium chloride solution; add sodium alginate solution into sodium carbonate solution, stir to obtain a mixed solution; quickly add calcium chloride solution to the above mixed solution, stir, centrifuge, and dry to obtain. The raw materials used in the present invention are cheap and easy to obtain, have good biodegradability and biocompatibility, and have the potential of application and subsequent relevant experimental analysis.
Description
Technical field
The invention belongs to the preparation field of hydridization granular materials, particularly a kind of preparation method of sodium alginate-calcium carbonate hybrid granule.
Background technology
Biodegradable high-molecular refers to by the chemical action of the microorganism of nature or interpolation, and polymer substance is resolved into little minute compound, then enters natural cyclic process, and this method is succinctly effective, and the protection of environment is had to positive effect.Meanwhile, along with the development of new and high technology, biodegradated polymer materal has also met the demand of medical science and agricultural and other side, becomes the focus of Recent study.Degradable macromolecule is according to the difference of material source, and it is mainly divided into natural macromolecular material, synthesized polymer material and mix type macromolecular material.
Biodegradable medical macromolecular materials as for diagnosing, the material for the treatment of and neomorph, be widely used in recent years medicine and control the fields such as release vehicle, its research occupies very important position in fields such as biotechnology, life sciences and medical science.
Microgranule is the granule of 1 to 1000 micron of diameter.Preparing the most popular method of biodegradable microgranule is chemical precipitation method, phase separation method, spray drying method and solvent evaporated method.Wherein phase separation method, spray drying method and solvent evaporated method conventionally have adding of organic solvent in implementation procedure, may cause pollution in various degree to environment, and operation relative complex, and the response time is slightly long.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation method of sodium alginate-calcium carbonate hybrid granule, raw material used in the present invention is cheap and easy to get, there is good biodegradability and biocompatibility, there is application and do the potentiality that follow-up related experiment is analyzed.
The preparation method of a kind of sodium alginate-calcium carbonate hybrid granule of the present invention, comprising:
(1) under 70-80 ℃ of condition, sodium alginate is added in distilled water, obtain sodium alginate soln;
(2) at ambient temperature, prepare respectively sodium carbonate, calcium chloride solution;
(3) sodium alginate soln is added in sodium carbonate liquor, stir, obtain mixed solution;
(4) calcium chloride solution is added rapidly in above-mentioned mixed solution, stir, centrifugal, dry, obtain sodium alginate-calcium carbonate hybrid granule, wherein sodium alginate soln, sodium carbonate liquor, the volume ratio of calcium chloride solution is 1:1:1.
In described step (1), the concentration of sodium alginate soln is 0.5-1g/L.
In described step (2), the concentration of sodium carbonate liquor is 0.05-0.1mol/L, and the concentration of calcium chloride solution is 0.05-0.1mol/L, and the solvent of solution is distilled water.
In described step (3), stir speed (S.S.) is 110-120r/min, and mixing time is 5-10min.
In described step (4), stir speed (S.S.) is 110-120r/min, and mixing time is 0.5-1h.
In described step (4), centrifugation rate is 8000-10000r/min, and centrifugation time is 5-30min.
In described step (4), baking temperature is 45-55 ℃.
What in described step (4), make has good application prospect containing carboxyl family macromolecule micron particle in the fields such as biomedical and biological engineering, is suitable for as pharmaceutical carrier, can be used for the preparation of wound dressing.
Chemical precipitation method be take water conventionally as solvent, belongs to environmentally friendly, and easy and simple to handle, and the response time is short.This patent adopts chemical precipitation method, and whole process all be take distilled water as solvent, has synthesized calcium carbonate-sodium alginate hydridization granule of 5 microns of left and right of diameter, and preparation method is cheap, and is green process.
beneficial effect
(1) whole preparation process of the present invention solvent used is distilled water, and the adding of organic solvent-free, environmentally safe, belongs to environmentally friendly production process;
(2) raw material used in the present invention is cheap and easy to get, has good biodegradability and biocompatibility, has application and does the potentiality that follow-up related experiment is analyzed.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the resulting calcium carbonate-sodium alginate of embodiment 1 hydridization granule;
Fig. 2 is the scanning electron microscope of the resulting calcium carbonate-sodium alginate of embodiment 2 hydridization granule;
Fig. 3 is the infrared spectrogram of the resulting calcium carbonate-sodium alginate of embodiment 1 hydridization granule;
Fig. 4 is that the resulting load of embodiment 2 has diclofenac sodium medicine, and the medicine of diclofenac sodium is controlled to release graphics.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.In addition should be understood that those skilled in the art can make various changes or modifications the present invention after having read the content of the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1
Under (1) 70 ℃ of condition, 5g sodium alginate is dissolved in 1000mL distilled water, obtains 0.5g/L sodium alginate soln;
(2) take in the volumetric flask that 10.6g natrium carbonicum calcinatum adds 1L, add distilled water, be mixed with the sodium carbonate liquor of 0.1mol/L;
(3) take in the volumetric flask that 11.1g anhydrous calcium chloride adds 1L, add distilled water, be mixed with the calcium chloride solution of 0.1mol/L;
(4) get sodium alginate soln 20mL described in (1), join in 100ml beaker, get sodium carbonate liquor described in same volume (2) simultaneously and add in beaker, under the rotating speed of 110r/min, stir ten minutes;
(5) get 20ml(3) described in calcium chloride solution, pour into rapidly described in (4) in mixed liquor, under same rotational speed, stir one hour;
(6) final resulting mixed liquor is put into centrifuge, under the rotating speed of 8000r/min centrifugal ten minutes, gained granule is put into 50 ℃ of thermostatic drying chambers dry.
Embodiment 2
(1) take 0.1g diclofenac sodium drug powder and add in the volumetric flask of 100ml, add distilled water, be mixed with the diclofenac sodium water solution of 1mg/ml;
(2) get sodium alginate soln 10mL described in embodiment 1, join in 100ml beaker, get sodium carbonate liquor described in same volume embodiment 1 simultaneously and add in beaker, under the rotating speed of 110r/min, stir ten minutes;
(3) get calcium chloride solution 10ml described in embodiment 1, join in 50ml beaker, get 10ml diclofenac sodium solution phase simultaneously and should join in the beaker that calcium chloride solution is housed, under the rotating speed of 110r/min, stir ten minutes, make it mix homogeneously;
(4) mixed liquor in beaker described in (3) is poured into rapidly in the beaker in (2), under the rotating speed of 110r/min, stir one hour;
(5) final resulting mixed liquor is put into centrifuge, under the rotating speed of 8000r/min centrifugal ten minutes, gained granule is put into 50 ℃ of thermostatic drying chambers dry, weigh the quality of dried powder, and get the centrifugal supernatant obtaining, with ultraviolet spectrophotometer, survey its absorbance, obtain the quality of free diclofenac sodium in solution, thereby calculate the quality of granule packaging medicine.
(6) the hydridization granule 12.2mg that includes 0.423mg diclofenac sodium medicine being put into pH value is to carry out external slow release experiment in 6.8 PBS buffer, obtains the external accumulative total release rate (data are as following table) of diclofenac sodium.
Claims (7)
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105854026A (en) * | 2016-04-06 | 2016-08-17 | 温州生物材料与工程研究所 | Basic protein entrapment vector, preparation method of entrapment vector and entrapment method |
| CN106420631A (en) * | 2016-11-17 | 2017-02-22 | 青岛悦海医药科技有限公司 | Preparation method of micro-pore sodium alginate-starch composite particles |
| CN108392672A (en) * | 2018-03-23 | 2018-08-14 | 曹朗翘 | Pseudo-ginseng seaweed gel dressing and preparation method thereof |
| KR20210088934A (en) * | 2020-01-07 | 2021-07-15 | 주식회사 테라시온 바이오메디칼 | Micro-beads and Method for producing thereof, Hemostatic dressings including the same |
| CN118580550A (en) * | 2024-05-20 | 2024-09-03 | 青岛农业大学 | A method for improving the anti-swelling performance and mechanical properties of seaweed-based biodegradable straws |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102286155A (en) * | 2011-05-30 | 2011-12-21 | 武汉大学 | Preparation method of sodium alginate-calcium carbonate hybridized micron particles |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102286155A (en) * | 2011-05-30 | 2011-12-21 | 武汉大学 | Preparation method of sodium alginate-calcium carbonate hybridized micron particles |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105854026A (en) * | 2016-04-06 | 2016-08-17 | 温州生物材料与工程研究所 | Basic protein entrapment vector, preparation method of entrapment vector and entrapment method |
| CN106420631A (en) * | 2016-11-17 | 2017-02-22 | 青岛悦海医药科技有限公司 | Preparation method of micro-pore sodium alginate-starch composite particles |
| CN106420631B (en) * | 2016-11-17 | 2019-03-22 | 青岛悦海医药科技有限公司 | A kind of preparation method of micropore sodium alginate-starch composite particles |
| CN108392672A (en) * | 2018-03-23 | 2018-08-14 | 曹朗翘 | Pseudo-ginseng seaweed gel dressing and preparation method thereof |
| KR20210088934A (en) * | 2020-01-07 | 2021-07-15 | 주식회사 테라시온 바이오메디칼 | Micro-beads and Method for producing thereof, Hemostatic dressings including the same |
| KR102302405B1 (en) | 2020-01-07 | 2021-09-16 | 주식회사 테라시온 바이오메디칼 | Micro-beads and Method for producing thereof, Hemostatic dressings including the same |
| CN118580550A (en) * | 2024-05-20 | 2024-09-03 | 青岛农业大学 | A method for improving the anti-swelling performance and mechanical properties of seaweed-based biodegradable straws |
| CN118580550B (en) * | 2024-05-20 | 2024-12-06 | 青岛农业大学 | Method for improving swelling resistance and mechanical property of seaweed-based degradable straw |
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