CN102274193A - Method for preparing improved plant polyphenol compound carrying sustained-release microspheres - Google Patents
Method for preparing improved plant polyphenol compound carrying sustained-release microspheres Download PDFInfo
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- CN102274193A CN102274193A CN2011102549255A CN201110254925A CN102274193A CN 102274193 A CN102274193 A CN 102274193A CN 2011102549255 A CN2011102549255 A CN 2011102549255A CN 201110254925 A CN201110254925 A CN 201110254925A CN 102274193 A CN102274193 A CN 102274193A
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Abstract
The invention discloses a method for preparing improved plant polyphenol compound carrying sustained-release microspheres. The method comprises the following steps of: (1) mixing a plant polyphenol compound and water-soluble chitosan; (2) mixing the obtained mixture and aqueous solution of sodium alga acid; (3) adding the obtained mixed solution into gelatinizer solution or chitosan-containing gelatinizer solution in a form of small drops; and (4) recovering formed spherical objects, cleaning, drying and the like. When the method is used, the leakage and loss of the plant polyphenol compound in the preparation process can be reduced, the preparation process is simple and the condition is mild, so the activity of the plant polyphenol compound is easy to keep.
Description
Technical field
Year plant polyphenol compounds sustained-release micro-spheres that the present invention relates to the preparation method of a kind of improved year plant polyphenol compounds sustained-release micro-spheres and prepare thus belongs to microsphere preparation technology.
Background technology
The plant polyphenol compounds is the chemical substance with a plurality of phenolic hydroxyl groups that is present in the plant, can be distributed in epidermis, root, stem, leaf, flower and the fruit of plant.The plant polyphenol compounds has reproducibility, removes free radical ability and multiple physiologically active; for example can play effective protective effect, delay body aging, prevention and treatment cardiovascular and cerebrovascular disease, antiinflammatory, antitumor, antiulcer etc. lipid peroxidation and biomacromolecule damage that free radical brings out.
Alginate microsphere is simple because of its preparation process, does not need high temperature, adds organic solvent or other hazardous compound, has obtained extensive use in the fields such as immobilization of medicament slow release, cell and enzyme.The preparation process of medicine carrying alginate microsphere is normally mixed medicine earlier with sodium alginate aqueous solution, adopt methods such as needle injection method, gas shearing method or capillary tube crush method to join with the fine droplet form in the gellant solution (for example calcium chloride solution) of sodium alginate then, just can form the medicine carrying calcium alginate gel bead at once.The oral back of this medicine carrying microballoons medicine can slowly be discharged, and can reduce blood concentration " peak valley " effect and medicining times.If also contain chitosan in the calcium chloride solution, the gel micro-ball surface will form chitosan and calcium alginate polyelectrolyte film, both can improve the stability of gel micro-ball, also can further regulate the rate of release of contained medicine.Utilize this method can prepare the sustained-release micro-spheres that carries the plant polyphenol compounds equally, but in preparation process, the plant polyphenol compounds can be leaked in the gellant solution from gel micro-ball, cause damage, especially less or when being water solublity, it is bigger to reveal loss when the plant polyphenol kind compound molecular weight.
Summary of the invention
For solving the deficiency that exists in the above-mentioned technology, the purpose of this invention is to provide the preparation method of a kind of improved year plant polyphenol compounds sustained-release micro-spheres, can reduce the leakage loss of plant polyphenol compounds in the preparation process.
To achieve these goals, the technical solution used in the present invention is: the preparation method of a kind of improved year plant polyphenol compounds sustained-release micro-spheres is characterized in that this method may further comprise the steps:
Step 1: the plant polyphenol compounds is mixed with water-soluble chitosan;
Step 2: step 1 gained mixture is mixed with sodium alginate aqueous solution;
Step 3: step 2 gained mixed liquor is joined gellant solution with the fine droplet form or contain in the gellant solution of chitosan;
Step 4: reclaim the round that forms, cleaning, drying promptly get the sustained-release micro-spheres that carries the plant polyphenol compounds.
The source of wherein said plant polyphenol compounds without limits, for example can be from Fructus Vitis viniferae, Fructus Kaki, Fructus Mali pumilae, blue berry, Fructus Pruni pseudocerasi, Fructus Pruni salicinae, Fructus Crataegi, Citrus, Pericarpium Citri tangerinae, beans, Semen arachidis hypogaeae, Rhizoma Steudnerae Henryanae, Semen Ginkgo, Radix Et Rhizoma Rhei, Cortex Cinnamomi, Folium Camelliae sinensis, Folium eucalypti globueli (Eucalyptus globulus Labill.), Folium Bambusae and Cortex Pini etc., can be a kind of chemical compound, also can be different compound compositions.
Water-soluble chitosan described in the step 1 be meant can be water-soluble chitosan.
Chitosan described in the step 3 typically refers to the solubility in acid chitosan, that is: water insoluble but be dissolved in the chitosan of acid solutions such as acetic acid, formic acid, hydrochloric acid or citric acid, also can be water-soluble chitosan.
Described gellant is meant the material that can make sodium alginate gelization, for example the salt of polyvalent cations such as calcium chloride, strontium chloride, barium chloride.
The sustained-release micro-spheres that carries the plant polyphenol compounds according to the inventive method preparation also is provided.
The sustained-release micro-spheres that carries the plant polyphenol compounds according to the inventive method preparation, it is characterized in that this microspherulite diameter is less than 3mm, be single nuclear structure, its material is made up of plant polyphenol compounds and water-soluble chitosan and alginate: perhaps be hud typed structure, its nuclear material is made up of plant polyphenol compounds and water-soluble chitosan and alginate, and its shell material is chitosan and alginate polyelectrolyte film.
Advantage of the present invention and good effect are:
The present invention utilizes water-soluble chitosan to adsorb mutually with the plant polyphenol compounds, can produce the character of electrostatic interaction again with sodium alginate, earlier the plant polyphenol compounds is mixed with water-soluble chitosan, and then prepare gel micro-ball with splashing in the gellant solution after sodium alginate aqueous solution is mixed, so just can stop effectively that the plant polyphenol compounds is leaked in the gellant solution in the preparation process from gel micro-ball, reduce loss.And because use is water-soluble chitosan, its molecular weight can not form large-sized insoluble matter with plant polyphenol compounds and sodium alginate far below the solubility in acid chitosan, influences the preparation of sustained-release micro-spheres.The inventive method preparation process is simple, and mild condition does not need high temperature, adds organic solvent or other hazardous compound, is beneficial to the activity that keeps the plant polyphenol compounds.
The specific embodiment
The present invention is further described in conjunction with the embodiments, and purpose is to help the reader to understand spirit of the present invention better, but not as the qualification to the scope of the present invention.
Carry the sustained-release micro-spheres of plant polyphenol compounds according to following step preparation:
Step 1: the plant polyphenol compounds is mixed with water-soluble chitosan.
Water-soluble chitosan can be available from commercially available water-soluble chitosan product, and also can adopt the solubility in acid chitosan is raw material, gets through enzymic degradation.Can be earlier that water-soluble chitosan is soluble in water, and then the plant polyphenol compounds of adding solid powdery, mixing fast; Also can directly the powdery, water-soluble chitosan be mixed mutually with pulverous plant polyphenol compounds.The weight ratio of water-soluble chitosan and plant polyphenol compounds is chosen as 1: 1～and 1: 1000, be preferably 1: 20～1: 400.
Step 2: step 1 gained mixture is mixed with sodium alginate aqueous solution.
The final concentration of sodium alginate can be 0.5～10% (w/v) in the gained mixed liquor, is preferably 1.5～6% (w/v); The final concentration of plant polyphenol compounds can be 0.05～15% (w/v), is preferably 0.5～6% (w/v).The pH value of mixed liquor is generally 4.5～7.5, is preferably 5～6.
Step 3: step 2 gained mixed liquor is joined gellant solution with the fine droplet form or contain in the gellant solution of chitosan.
Can adopt needle injection method, high-pressure spray gun spurt method, gas shearing method, capillary tube crush method or other method that mixed liquor is added with the fine droplet form.The concentration of gellant can be selected by test for can make sodium alginate form concentration complete, blocky gel micro-ball in the gellant solution.For example, when gellant was calcium chloride, concentration can be 0.5～10% (w/v), was preferably 1～6% (w/v).When containing chitosan in the gellant solution, the concentration of chitosan can be 0.01～2% (w/v), is preferably 0.1～1% (w/v).The pH value of gellant solution can be 4.5～6.5, is preferably 5～6.
Step 4: reclaim the round that forms, cleaning, drying promptly get the sustained-release micro-spheres that carries the plant polyphenol compounds.
Can adopt filtration or centrifugation method to separate the gel micro-ball that forms from gellant solution, drying means can adopt vacuum lyophilization, vacuum drying, spray drying or other drying means.
The microsphere that carries the plant polyphenol compounds for preparing according to the method described above, its particle diameter are usually less than 3mm, and the plant polyphenol compounds in the microsphere of oral back can slowly be discharged.When not containing chitosan in the gellant solution, the microsphere of formation is single nuclear structure, is made up of plant polyphenol compounds and water-soluble chitosan and alginate; When containing chitosan in the gellant solution, the microsphere of preparing is hud typed structure, and the nuclear material is made up of plant polyphenol compounds and water-soluble chitosan and alginate, and the shell material is the polyelectrolyte film that chitosan and alginate form.
In following embodiment 1～embodiment 5, the plant polyphenol compounds is an example with grape pip procyanidin extract (Oligomeric Proanthocyanidins content 〉=85%, total phenol content 〉=95%) all, and the gellant of sodium alginate all is example with calcium chloride.
Embodiment 1: conventional method preparation (in the gellant solution not chitosan-containing)
Get 1 gram grape pip procyanidin extract, be dissolved in the 10mL water, join then in 30mL, 4% the sodium alginate aqueous solution, abundant mixing, with No. 6 syringe needles mixed liquor is splashed in 3% the calcium chloride solution, gentle agitation 30min, isolated by filtration gained round, and the total phenol content of detection of leaks aldehydes matter in the calcium chloride solution.
Embodiment 2: conventional method preparation (containing chitosan in the gellant solution)
With the chitosan solution of 0.5% acetic acid preparation 1%, mix with 6% calcium chloride solution equal-volume then, make chitosan-calcium chloride solution.Get 1 gram grape pip procyanidin extract, be dissolved in the 10mL water, join then in 30mL, 4% the sodium alginate aqueous solution, abundant mixing, mixed liquor is splashed in above-mentioned chitosan-calcium chloride solution gentle agitation 30min, isolated by filtration gained round with No. 6 syringe needles.After testing, be leaked to that the total phenol content of aldehydes matter is about 48% of embodiment 1 in chitosan-calcium chloride solution.
Embodiment 3: improved method preparation (in the gellant solution not chitosan-containing)
Get 1 gram grape pip procyanidin extract, join in 10mL, 0.1% the commercially available water-soluble chitosan solution, quick mixing, and then join in 30mL, 4% the sodium alginate aqueous solution, other step is with embodiment 1, isolated by filtration gained round is washed back 50 ℃ of dryings, promptly gets the sustained-release micro-spheres that carries procyanidin.The about 1mm of the mean diameter of this sustained-release micro-spheres is single nuclear structure, and its material is made up of grape pip procyanidin extract and water-soluble chitosan and calcium alginate.After testing, be leaked to that the total phenol content of aldehydes matter is about 20% of embodiment 1 in the calcium chloride solution.
Embodiment 4: improved method preparation (containing chitosan in the gellant solution)
With the chitosan solution of 0.5% acetic acid preparation 1%, mix with 6% calcium chloride solution equal-volume then, make chitosan-calcium chloride solution.Get 1 gram grape pip procyanidin extract, join in 10mL, 0.1% the commercially available water-soluble chitosan solution, quick mixing, and then join in 30mL, 4% the sodium alginate aqueous solution, fully mixing splashes into mixed liquor in above-mentioned chitosan-calcium chloride solution with No. 6 syringe needles, gentle agitation 30min, isolated by filtration gained round is washed back 50 ℃ of dryings, promptly gets the sustained-release micro-spheres that carries procyanidin.This sustained-release micro-spheres is hud typed structure, and the nuclear material is made up of grape pip procyanidin extract and water-soluble chitosan and calcium alginate, and the shell material is chitosan and calcium alginate polyelectrolyte film.After testing, be leaked to that the total phenol content of aldehydes matter is about 18% of embodiment 2 in chitosan-calcium chloride solution.Above-mentioned microsphere was handled in simulated gastric fluid 1 hour, and the release rate of aldehydes matter is about 10%, and microsphere is placed in the simulated intestinal fluid once more, 12 hours cumulative release rate of aldehydes matter about 85%.
Embodiment 5: use homemade water-soluble chitosan
The chitosan solution of the acetic acid preparation 5% with 2% is regulated pH5～6, adds cellulase, 50 ℃ of reactions, and the question response fluid viscosity greatly reduces after-filtration, concentrated, lyophilization, and dry thing is clayed into power, and gets homemade water-soluble chitosan.Get 1 gram grape pip procyanidin extract, join in 10mL, 0.2% the self-control water-soluble chitosan solution, mixing fast, other step is with embodiment 4.After testing, be leaked in the preparation process that the total phenol content of aldehydes matter is about 80% of embodiment 4 in chitosan-calcium chloride solution.
Claims (3)
1. the preparation method of an improved year plant polyphenol compounds sustained-release micro-spheres is characterized in that this method may further comprise the steps
Step 1: the plant polyphenol compounds is mixed with water-soluble chitosan;
Step 2: step 1 gained mixture is mixed with sodium alginate aqueous solution;
Step 3: step 2 gained mixed liquor is joined gellant solution with the fine droplet form or contain in the gellant solution of chitosan;
Step 4: reclaim the round that forms, cleaning, drying promptly get the sustained-release micro-spheres that carries the plant polyphenol compounds.
2. the sustained-release micro-spheres that carries the plant polyphenol compounds of method preparation according to claim 1.
3. the sustained-release micro-spheres of described year plant polyphenol compounds of claim 2 is characterized in that this microspherulite diameter less than 3mm, is single nuclear structure, and its material is made up of plant polyphenol compounds and water-soluble chitosan and alginate; Perhaps be hud typed structure, its nuclear material is made up of plant polyphenol compounds and water-soluble chitosan and alginate, and its shell material is chitosan and alginate polyelectrolyte film.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104095186A (en) * | 2014-07-21 | 2014-10-15 | 天津市林业果树研究所 | Preparation method for probiotic sustained release agent containing plant extracts |
| CN115486510A (en) * | 2022-10-22 | 2022-12-20 | 南通奥凯生物技术开发有限公司 | High-purity feed additive containing sodium diacetate and preparation method thereof |
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| CN1383819A (en) * | 2002-05-17 | 2002-12-11 | 天津市园艺工程研究所 | Protocyanidin slow release capsule |
| WO2003075861A1 (en) * | 2002-03-12 | 2003-09-18 | Cognis Iberia, S.L. | Antioxidative preparations |
| CN1486700A (en) * | 2002-09-30 | 2004-04-07 | 王洪栋 | Proanthocyanidin compound and its prepn |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2003075861A1 (en) * | 2002-03-12 | 2003-09-18 | Cognis Iberia, S.L. | Antioxidative preparations |
| CN1383819A (en) * | 2002-05-17 | 2002-12-11 | 天津市园艺工程研究所 | Protocyanidin slow release capsule |
| CN1486700A (en) * | 2002-09-30 | 2004-04-07 | 王洪栋 | Proanthocyanidin compound and its prepn |
Non-Patent Citations (2)
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| 张峻等: "壳聚糖-海藻酸钠微胶囊对葡萄多酚控制释放的研究", 《食品科学》, vol. 25, no. 5, 31 December 2004 (2004-12-31), pages 102 - 104 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104095186A (en) * | 2014-07-21 | 2014-10-15 | 天津市林业果树研究所 | Preparation method for probiotic sustained release agent containing plant extracts |
| CN115486510A (en) * | 2022-10-22 | 2022-12-20 | 南通奥凯生物技术开发有限公司 | High-purity feed additive containing sodium diacetate and preparation method thereof |
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Application publication date: 20111214 |