CN109223726A - A kind of preparation method of Novel hollow capsule and obtained Novel hollow capsule - Google Patents
A kind of preparation method of Novel hollow capsule and obtained Novel hollow capsule Download PDFInfo
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- CN109223726A CN109223726A CN201811137073.XA CN201811137073A CN109223726A CN 109223726 A CN109223726 A CN 109223726A CN 201811137073 A CN201811137073 A CN 201811137073A CN 109223726 A CN109223726 A CN 109223726A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/4816—Wall or shell material
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
- A61K47/36—Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
Abstract
The invention discloses a kind of preparation method of Novel hollow capsule and obtained Novel hollow capsules, wherein, certain density chitosan is added dropwise in certain density high molecular weight polyelectrolyte mixed solution (sodium alginate, xanthan gum, carragheen wherein any two kinds of mixed solutions), hollow capsules can be formed under oscillation；The preparation method is simple, it is at low cost, be suitable for large-scale production, meanwhile, obtained hollow capsules are in Dagwood structure, have good compression strength, medicament slow release performance, absorption property.
Description
Technical field
The present invention relates to field of capsules, and in particular to the preparation of hollow capsules is particularly related to a kind of Novel hollow capsule
Preparation method and obtained Novel hollow capsule.
Background technique
Hollow capsules have been widely used for the industrial circles such as food, drug, cosmetics, bioengineering and organizational project,
With the continuous improvement to product structure and performance indicator requirement, in the prior art, the emulsion method and template legal system generallyd use
Standby technology, more or less encounters different problems or technical bottleneck.
For example, template in the prior art, use using particle as template, using layer-by-layer in template
Particle over-assemble polymer ultra-thin film, after removing removing template, structure and performance are controllable, easily assign various unique functions to obtain, and accord with
It closes end product and uses the microcapsules needed.
But since template material is generally CaCO3, gold, silicon or other inorganic material, template fabrication is complicated, at
This height is restricted by factors such as shape of template, sizes, can not carry out Flexible Production.
The problem of emulsion method and deficiency are mainly manifested in, first is that, due to preparation process to be added exhibiting high surface activating agent or
Inevitably, more or less residual toxic chemicals exist certain congenital for other chemical stabilizers, capsule product
Property it is insufficient.Second is that production cost is relatively high, complex treatment process.In addition, side reaction is to capsule property in synthesis process
It has a significant effect.
Summary of the invention
In order to overcome the above problem, present inventor has performed sharp studies, provide a kind of preparation side of Novel hollow capsule
Method, preparation cost is low, environmental friendly, and is suitable for large-scale production；Meanwhile obtained Novel hollow capsule is with unique
Sandwich structure, thereby completing the present invention.
One aspect of the present invention is to provide a kind of preparation method of Novel hollow capsule, is embodied in following side
Face:
(1) a kind of preparation method of Novel hollow capsule, wherein the described method comprises the following steps:
Chitosan, the first high molecular weight polyelectrolyte and the second high molecular weight polyelectrolyte are separately added into water by step 1
In, respectively obtain chitosan solution, the first solution and the second solution；
Step 2 mixes the first solution and the second solution, obtains mixed solution；
Step 3 chitosan solution is added dropwise in mixed solution, oscillation treatment, obtains the Novel hollow capsule.
(2) preparation method according to above-mentioned (1), wherein in step 1,
The molecular weight of the chitosan polyelectrolyte is 2000~10000Da, preferably 2000~6000Da.
(3) preparation method according to one of above-mentioned (1) to (2), wherein in step 1,
The molecular weight of the first high molecular weight polyelectrolyte and the second high molecular weight polyelectrolyte is separately
100000~800000Da, preferably 300000~700000Da, more preferably 400000~600000Da.
(4) preparation method according to one of above-mentioned (1) to (3), wherein in step 1, first high molecular weight
Polyelectrolyte and the second high molecular weight polyelectrolyte are different, and are separately selected from sodium alginate, xanthan gum or carragheen.
(5) preparation method according to one of above-mentioned (1) to (4), wherein in step 1,
The mass percent concentration of the chitosan solution be 5~60%, preferably 10~40%, more preferably 20~
40%, such as 30~40%；And/or
The mass percent concentration of first solution is 0.5~2%, such as 1%；And/or
The mass percent concentration of second solution is 0.1~1%, such as 0.5%；
(6) preparation method according to one of above-mentioned (1) to (5), wherein in step 2,
By volume (0.5~2): 1 mixes the first solution with the second solution, obtains mixed solution；
(7) preparation method according to one of above-mentioned (1) to (6), wherein in step 3,
1:(10~500 by volume) chitosan solution is added in mixed solution, preferred 1:(10~200), more preferably
1:(30~100), such as 1:50；And/or
The oscillation treatment carries out 1~for 24 hours, preferably 2~8h of progress, more preferably 4~6h of progress.
Another aspect of the present invention provides a kind of Novel hollow capsule, is embodied in the following aspects:
(8) a kind of hollow capsules are obtained preferably by preparation method described in one of above-mentioned (1) to (7), more preferably described
The diameter of hollow capsules is 500 μm~10cm.
(9) hollow capsules according to above-mentioned (8), wherein the cyst wall of the hollow capsules is Dagwood structure,
Adjacent layer structure is different, and every alternating floor structure is identical.
Detailed description of the invention
Fig. 1 shows one of chitosan obtained by embodiment 1 (sodium alginate/xanthan gum) capsule electron micrograph
(cross section of capsule-wall is mainly shown)；
Fig. 2 is the two (masters of chitosan (sodium alginate/xanthan gum) capsule electron micrograph obtained by embodiment 1
The cross section of the adjacent layer of capsule-wall is shown).
Specific embodiment
Below by embodiment and experimental example, the present invention is described in more detail.Illustrated by these, spy of the invention
Point and advantage will become more apparent from clear.
The present invention provides a kind of preparation method of hollow capsules with sandwich unique texture, and the method includes following
Step:
Chitosan, the first high molecular weight polyelectrolyte and the second high molecular weight polyelectrolyte are separately added into water by step 1
In, respectively obtain chitosan solution, the first solution and the second solution；
Step 2 mixes the first solution and the second solution, obtains mixed solution；
Step 3, the chitosan solution for obtaining step 1 are added dropwise in the mixed solution that step 2 obtains, and then vibrate,
Obtain the Novel hollow capsule.
Wherein, using between chitosan and two kinds of high molecular weight polyelectrolyte (being respectively provided with opposite positive and negative charge)
Electrostatic interaction forms complexing film so that three is complexed；Since the diffusion rate of two kinds of high molecular weight polyelectrolyte is different, with shell
The rate that glycan combines is different, and formation complexing film is first reacted with one of which, continues diffusion with another and forms new complexing
Film.Under the driving effect of osmotic pressure, solution spontaneously constantly repeats the process that above-mentioned complexing-diffusion-is complexed again, i.e., controllably
The capsule of the different cyst wall numbers of plies of sandwich special construction is made.
A kind of preferred embodiment according to the present invention, in step 1, the molecular weight of the chitosan is 2000~
10000Da。
In further preferred embodiment, in step 1, the molecular weight of the chitosan is 2000~6000Da.
Wherein, if the number-average molecular weight of chitosan is less than 2000Da, it is anti-that complexing occurs with high molecular weight polyelectrolyte
At once, it since the binding site of chitosan and high molecular weight polyelectrolyte is few, tangles not enough, is not enough to that film forming is supported especially to have
There is the film of certain curvature, will finally form complex precipitate particle.Meanwhile if the number-average molecular weight of the chitosan is greater than
When 10000Da, chitosan occurs Electrostatic complexation with high molecular weight polyelectrolyte and reacts the complexing layer close structure to be formed, chitosan
It cannot pass through, diffusion process is prevented, and cannot finally form hollow structure.
A kind of preferred embodiment according to the present invention, in step 1, the first high molecular weight polyelectrolyte and second
The molecular weight of high molecular weight polyelectrolyte is separately 100000~800000Da.
In further preferred embodiment, in step 1, the first high molecular weight polyelectrolyte and the second high score
The molecular weight of son amount polyelectrolyte is separately 300000~700000Da.
In embodiment still more preferably, in step 2, the first high molecular weight polyelectrolyte and second high
The molecular weight of molecular weight polyelectrolyte is separately 400000~600000Da.
Wherein, if with chitosan complex reaction institute occurs for the molecular weight of complex polyelectrolyte particle more than after above range
The polyelectrolyte membrane of formation will be excessively fine and close, this, which would potentially result in chitosan, cannot pass through polyelectrolyte membrane, to hinder
The further diffusion of chitosan not can be carried out the process that complexing-diffusion-is complexed again, finally, one layer of compact texture will be can only obtain
Film.
A kind of preferred embodiment according to the present invention, in step 1, in the chitosan solution, the matter of chitosan
Measuring percent concentration is 5~60%.
In further preferred embodiment, in step 1, in the chitosan solution, the quality hundred of chitosan
Dividing specific concentration is 10~40%.
In embodiment still more preferably, in step 1, in the chitosan solution, the quality of chitosan
Percent concentration is 20~40%, such as 30~40%.
A kind of preferred embodiment according to the present invention, in step 1, the mass percent concentration of first solution is
0.5~2%, such as 1%；The mass percent concentration of second solution is 0.1~1%, such as 0.5%.
Wherein, chitosan is controlled at higher concentrations (5~60%), and the control of high molecular weight polyelectrolyte is relatively low dense
Under degree, in this way, the two is since ion concentration difference forms osmotic pressure, chitosan expands to high molecular weight polyelectrolyte under osmotic pressure
It dissipates, is then combined using electrostatic interaction, form film.
A kind of preferred embodiment according to the present invention, in step 2, by volume (0.5~2): 1 by the first solution with
The mixing of second solution, such as 1:1, obtain mixed solution.
A kind of preferred embodiment according to the present invention, in step 3,1:(10~500 by volume) chitosan is molten
Liquid is added in mixed solution.
In further preferred embodiment, in step 3,1:(10~200 by volume) chitosan solution is added
Enter in mixed solution.
In embodiment still more preferably, in step 3,1:(30~100 by volume) by chitosan solution
It is added in mixed solution, such as 1:50.
A kind of preferred embodiment according to the present invention, in step 3, the oscillation carries out 1~for 24 hours.
In further preferred embodiment, in step 3, the oscillation carries out 2~8h.
In embodiment still more preferably, in step 3, the oscillation carries out 4~6h.
Wherein, the purpose of oscillation is to advantageously promote molecule diffusion, prevents capsule adherent.
Second aspect of the present invention provides a kind of Novel hollow capsule, obtains preferably by above-mentioned preparation method.
A kind of preferred embodiment according to the present invention, Novel hollow capsule be hollow structure, a diameter of 500 μm~
10cm。
In further preferred embodiment, the cyst wall of the Novel hollow capsule is three multilayer Mingzhi's structures, adjacent
Layer structure is different, and every alternating floor structure is identical.
Beneficial effect possessed by the present invention includes:
(1) preparation method of the present invention is simple, and the preparation of capsule, and preparation process can be completed under room temperature, normal pressure
In carried out under room temperature, normal pressure, technological parameter is easily controllable, production efficiency with higher；
(2) capsule with Dagwood structure can be made using preparation method of the present invention.
(3) raw material that the present invention uses is nontoxic for natural polysaccharide, and every layer of obtained capsule is closed ball
Body, therefore, obtained capsule product are particularly suitable as pharmaceutical carrier；
(4) preparation method obtains through the invention capsule compression strength with higher, good absorption property,
Suitable for the sewage treatment containing chemical components such as finish, organic solvent or organic dyestuff.
Embodiment
The present invention is further described below by way of specific embodiment.But these embodiments are only exemplary, not
Any restrictions are constituted to protection scope of the present invention.
Embodiment 1
40:1:0.5 in mass ratio weighs the chitosan that molecular weight is 2000Da, the seaweed that molecular weight is 300,000 Da respectively
Sour sodium and molecular weight are 300,000 Da xanthan gum, spare；
Taken chitosan is added into deionized water dissolving, obtains the chitosan solution that mass percent concentration is 40%；
Taken sodium alginate is added in deionized water and is dissolved, the sodium alginate that mass percent concentration is 1% is configured to
Solution；
Taken xanthan gum is added in deionized water and is dissolved, the xanthan peptization that mass percent concentration is 0.5% is configured to
Liquid；
Sodium alginate soln is added in xanthan gum solution in the ratio of 1:1, is stirred, mixed solution is obtained；
Above-mentioned chitosan solution is immersed in mixed solution by 1:50 dropwise by volume under oscillation, and sustained oscillation is for 24 hours
Afterwards, capsule is obtained.
Electron microscopy is carried out to obtained capsule, as a result as shown in Fig. 1~2, it is known that, obtained capsule is hollow
Structure, and cyst wall is Dagwood structure, one layer is tight structure, and one layer is open structure.
Embodiment 2
The process of embodiment 1 is repeated, difference is, the mass percent concentration of chitosan solution is 20%.
Electron microscopy is carried out to obtained hollow capsules, learns that capsule-wall has Dagwood structure.
Embodiment 3
Repeat the process of embodiment 1, difference is: (1) mass percent concentration of chitosan solution is 30%, (2) sea
The mass percent concentration of solution of sodium alginate is 2%, and the mass percent concentration of (3) xanthan gum solution is 1%.
Electron microscopy is carried out to obtained hollow capsules, learns that capsule-wall has Dagwood structure.
Embodiment 4
The process of embodiment 1 is repeated, difference is, (1) xanthan gum solution is added in sodium alginate soln by 2:1 by volume
In, obtain mixed solution；(2) chitosan solution is added in mixed solution 1:30 by volume.
Electron microscopy is carried out to obtained hollow capsules, learns that capsule-wall has Dagwood structure.
Embodiment 5
The process of embodiment 1 is repeated, difference is, the molecular weight of (1) described chitosan is 6000Da, (2) described seaweed
The molecular weight of sour sodium is 700,000 Da, and the molecular weight of (3) described xanthan gum is 600,000 Da.
Electron microscopy is carried out to obtained hollow capsules, learns that capsule-wall has Dagwood structure.
Embodiment 6
40:1:1 in mass ratio weighs the chitosan that molecular weight is 2000Da, the alginic acid that molecular weight is 300,000 Da respectively
Sodium and molecular weight are 300,000 Da carragheens, spare；
Taken chitosan is added into deionized water dissolving, obtains the chitosan solution that mass percent concentration is 40%；
Taken sodium alginate is added in deionized water and is dissolved, the sodium alginate that mass percent concentration is 1% is configured to
Solution；
Taken carragheen is added in deionized water and is dissolved, the xanthan gum solution that mass percent concentration is 1% is configured to；
Sodium alginate soln is added in carrageenan solutions in the ratio of 1:1, is stirred, mixed solution is obtained；
Above-mentioned chitosan solution is immersed in mixed solution by 1:50 dropwise by volume under oscillation, and sustained oscillation is for 24 hours
Afterwards, capsule is obtained.
Electron microscopy is carried out to obtained capsule, it is known that, obtained capsule is hollow structure, and cyst wall is multilayer
Sandwich structure, one layer is tight structure, and one layer is open structure.
Embodiment 7
40:1:0.5 in mass ratio weighs the chitosan that molecular weight is 2000Da, the OK a karaoke club that molecular weight is 300,000 Da respectively
Glue and molecular weight are 300,000 Da xanthan gum, spare；
Taken chitosan is added into deionized water dissolving, obtains the chitosan solution that mass percent concentration is 40%；
Taken carragheen is added in deionized water and is dissolved, the carrageenan solutions that mass percent concentration is 1% are configured to；
Taken xanthan gum is added in deionized water and is dissolved, the xanthan peptization that mass percent concentration is 0.5% is configured to
Liquid；
Carrageenan solutions are added in xanthan gum solution in the ratio of 1:1, are stirred, mixed solution is obtained；
Above-mentioned chitosan solution is immersed in mixed solution by 1:50 dropwise by volume under oscillation, and sustained oscillation is for 24 hours
Afterwards, capsule is obtained.
Electron microscopy is carried out to obtained capsule, it is known that, obtained capsule is hollow structure, and cyst wall is multilayer
Sandwich structure, one layer is tight structure, and one layer is open structure.
Comparative example
Comparative example 1
The process of embodiment 1 is repeated, difference is: the mass percent concentration of sodium alginate soln and xanthan gum solution is equal
It is very low, only 0.1%.
As a result, it has been found that will form precipitating when sodium alginate and very low xanthan gum mixed solution concentration.Due to chitosan
Binding site between sodium alginate and sodium alginate and xanthan gum mixed solution is insufficient, only forms precipitating, is not enough to support
Film especially forms the film of certain curvature.
Comparative example 2
The process of embodiment 1 is repeated, difference is: chitosan solution being directly added into mixed solution and is stirred, and
It is not to be added dropwise.
It was found that the hollow capsules cannot be formed at all, but the whole state in similar " sticky ".
Preferred embodiment and exemplary example is combined to describe the invention in detail above.But need to state
It is that these specific embodiments are only not constitute any limit to protection scope of the present invention to illustrative explanations of the invention
System.Without departing from spirit of that invention and protection scope, the technology of the present invention content and embodiments thereof can be carried out
Various improvement, equivalencing or modification, these fall within the protection scope of the present invention.Protection scope of the present invention is with appended power
Subject to benefit requires.
Claims (9)
1. a kind of preparation method of Novel hollow capsule, which is characterized in that the described method comprises the following steps:
Chitosan, the first high molecular weight polyelectrolyte and the second high molecular weight polyelectrolyte are separately added into water by step 1, point
Chitosan solution, the first solution and the second solution are not obtained；
Step 2 mixes the first solution and the second solution, obtains mixed solution；
Step 3, the chitosan solution for obtaining step 1 are added dropwise in the mixed solution that step 2 obtains, and then vibrate, obtain
The Novel hollow capsule.
2. preparation method according to claim 1, which is characterized in that in step 1,
The molecular weight of the chitosan is 2000~10000Da, preferably 2000~6000Da.
3. preparation method according to claim 1 or 2, which is characterized in that in step 1, first high-molecular-weight poly
The molecular weight of electrolyte and the second high molecular weight polyelectrolyte is separately 100000~800000Da, preferably 300000
~700000Da, more preferably 400000~600000Da.
4. according to claim 1 to preparation method described in one of 3, which is characterized in that in step 1, first macromolecule
It measures polyelectrolyte and the second high molecular weight polyelectrolyte is different, and be separately selected from sodium alginate, xanthan gum or carragheen.
5. according to claim 1 to preparation method described in one of 4, which is characterized in that in step 1,
The mass percent concentration of the chitosan solution is 5~60%, preferably 10~40%, more preferably 20~40%,
Such as 30~40%；And/or
The mass percent concentration of first solution is 0.5~2%, such as 1%；And/or
The mass percent concentration of second solution is 0.1~1%, such as 0.5%.
6. preparation method according to one of claims 1 to 5, which is characterized in that in step 2, by volume (0.5~
2): 1 mixes the first solution with the second solution, obtains mixed solution.
7. preparation method according to one of claims 1 to 6, which is characterized in that in step 3,
1:(10~500 by volume) chitosan solution is added in mixed solution, preferred 1:(10~200), more preferable 1:(30
, such as 1:50~100)；And/or
The oscillation treatment carries out 1~for 24 hours, preferably 2~8h of progress, more preferably 4~6h of progress.
8. a kind of Novel hollow capsule, obtains preferably by preparation method described in one of claim 1 to 7, more preferably described
The diameter of hollow capsules is 500 μm~10cm.
9. Novel hollow capsule according to claim 8, wherein the cyst wall of the hollow capsules is Dagwood structure,
Adjacent layer structure is different, and every alternating floor structure is identical.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114306273A (en) * | 2022-01-11 | 2022-04-12 | 新昌辽远科技有限公司 | Multilayer hollow capsule and preparation method thereof |
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