CN102058562A - Method for preparing gamma-polyglutamic acid/chitosan nano capsules - Google Patents
Method for preparing gamma-polyglutamic acid/chitosan nano capsules Download PDFInfo
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- CN102058562A CN102058562A CN2011100276569A CN201110027656A CN102058562A CN 102058562 A CN102058562 A CN 102058562A CN 2011100276569 A CN2011100276569 A CN 2011100276569A CN 201110027656 A CN201110027656 A CN 201110027656A CN 102058562 A CN102058562 A CN 102058562A
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Abstract
The invention discloses gamma-polyglutamic acid/chitosan nano capsules and a preparation method thereof. The nano capsules are prepared by proportioning gamma-polyglutamic acid (gamma-PGA), chitosan (CS) and Mg<2+> which are used as raw materials according to a ratio that the gamma-PGA to the CS to the Mg<2+> is 1mg:90mg:90mol by utilizing a polyelectrolyte self-assembly principle. The preparation method comprises the following steps of: preparing a gamma-polyglutamic acid aqueous solution and a chitosan ethylic acid solution with different concentrations; in the presence of Mg<2+>, obtaining a nano capsule solution in a mode of dropping while stirring; and then drying to obtain the gamma-polyglutamic acid/chitosan nano capsules. In the invention, the prepared nano capsules have uniform particle size, and the grain size is in the nano scale; the adopted raw materials are natural high molecular materials having no toxicity and harm to human bodies and theenvironment; and the nano capsules have the advantages of simple preparation process and moderate condition, thus the nano capsules can be used as vectors applied to the medicine industry and can also be used for functional food and the embedding of essences.
Description
Technical field
The present invention relates to the application of gamma-polyglutamic acid-, specifically is to utilize gamma-polyglutamic acid-and the chitosan a kind of method for feedstock production γ-PGA/CS Nano capsule.
Background technology
(γ-Polyglutamic acid, γ-PGA) a kind ofly form gamma-glutamyl amine bond by D-or L-glutamic acid by alpha-amido and γ-carboxyl and close the anionic polymer that forms gamma-polyglutamic acid-.γ-PGA is a kind of polymer substance of water-soluble biodegradable, has characteristics such as edibility, avirulence, caking property, moisture retention, and its application is very extensive.In present research report, γ-PGA is used for added value than higher field of medicaments as pharmaceutical carrier, biological adhesive, secondly γ-PGA also can be used as flocculating agent, heavy metal chelant is used for the water treatment aspect, can also be used for food, health product and cosmetics as water-retaining agent and fruit, the antifreezing agent of vegetable, antistaling agent.Exist a large amount of activated free carboxies in γ-PGA molecular structure thereby be a kind of anionic polymer.
γ-PGA has dual mode usually as pharmaceutical carrier: a kind of is to utilize the modification to γ-PGA such as Polyethylene Glycol, L-phenylalanine, benzylamine and alcohol; Another kind of mode is directly to combine with medicines such as camptothecine, taxol, penicillamine and cisplatin, and the γ that makes in this way-PGA-medicinal composition all has certain improvement to water solublity, half-life, toxicity and the slow-releasing etc. of medicine.
Chitosan is the product behind the chitin deacetylase base, and its active group is the amino behind the deacetylation, owing to have a certain amount of amino in the molecular structure, CS is that a kind of weak base also is present unique natural cationic polymer.CS has excellent biological compatibility, safety and immunostimulatory activity, also have simultaneously blood fat reducing, cholesterol reducing, antibiotic, to increase physiologically active such as immunity be a kind of good natural biological medical material.
Having the microsphere of slow release or control-release function or the research of microcapsule is current focus, and it can be used for field of medicaments also can be used for food and essence and flavoring agent field.The method that is usually used in preparing microcapsule at present has emulsion process, spray drying method and complex coacervation etc.The technology of these methods is relatively complicated, and preparation condition is relatively harsher, owing to have plurality of raw materials in the reaction system, causes that easily certain side reaction brings by-product simultaneously.
In sum, γ-PGA and chitosan be grouped together make Nano capsule and will have (1) extra small volume and can pass through the thinnest blood capillary, avoid macrophage to remove rapidly, so prolong its persistent period in blood greatly; (2) can penetration cell and interstice arrive target organ, as liver, spleen, lung, spinal cord and lymph; (3) can control its release by the temperature sensitivity of biodegradability, pH value, ion and material; (4) drug effect and reduce character such as toxic and side effects can be improved, medicine, polypeptide, protein, vaccine, nucleic acid, gene etc. can be used to carry.And do not see at present that having is grouped together γ-PGA and chitosan and make the report of Nano capsule.
Summary of the invention
One of purpose of the present invention is to provide a kind of gamma-polyglutamic acid-and chitosan nano capsule.
To two of the purpose of inventing, provide a kind of mode to carry out complex coacervation and make gamma-polyglutamic acid-and the capsular method of chitosan nano by the polyelectrolyte self assembly.
The object of the present invention is to provide a kind of gamma-polyglutamic acid-and chitosan of utilizing to carry out a kind of method that complex coacervation makes Nano capsule by the mode of polyelectrolyte self assembly.
Technical scheme of the present invention
A kind of γ-PGA/CS Nano capsule is with raw material gamma-polyglutamic acid-(γ-PGA) and chitosan (CS) and Mg
2+Proportioning press γ-PGA:CS:Mg
2+Be 1mg:1～90mg:2～90mol, utilize polyelectrolyte self assembly principle to make microcapsule, promptly at first prepare the gamma-polyglutamic acid-aqueous solution and the chitosan-acetic acid solution of variable concentrations, at finite concentration Mg
2+Ion exists down, obtains Nano capsule solution by the mode that stirs while dripping, and drying obtains gamma-polyglutamic acid-/chitosan nano capsule then.
The preparation method of a kind of γ-PGA/CS Nano capsule comprises the steps:
(1), the preparation of solution:
1., take by weighing γ-PGA solid and be dissolved in the ultra-pure water, obtaining mass concentration is γ-PGA aqueous solution of 0.05 mg/mL～5 mg/mL, regulating pH value is 6.0～8.0;
2., take by weighing the CS solid and be dissolved in 1% the acetum, obtaining mass concentration is the CS acetum of 0.1 mg/mL～10 mg/mL, regulating pH value is 3.0～6.0;
3., take by weighing MgSO
47H
2O is dissolved in step 2. in the gained solution, control Mg
2+Concentration be 0mol/L～2mol/mL, obtain Mg
2+The CS acetum;
(2), with in the step (1): 1. the γ of gained-PGA aqueous solution adds the 3. Mg of gained by the mode that stirs while dripping
2+The CS acetum in, rate of addition is 0.5mL/h～5mL/h, mixing speed is 50r/min～200r/min, final γ-PGA aqueous solution with contain Mg
2+The mixed liquor of CS acetum;
Gamma-polyglutamic acid-(γ-PGA) and chitosan (CS) and Mg wherein
2+Proportioning press γ-PGA:CS:Mg
2+Be 1mg:1～90mg:2～90mol;
(3), with the γ-PGA aqueous solution of step (2) gained with contain Mg
2+The mixed liquor of CS acetum be to continue stirring reaction 10min～120min under 50r/min～200r/min condition to obtain γ-PGA/CS Nano capsule solution at rotating speed;
(4), with the γ-PGA/CS Nano capsule solution centrifugal of step (3) gained, centrifugal condition is 1000r/min～3000r/min, centrifugation time is 5min～10min, and collecting supernatant is 0.01MPa in vacuum, and temperature is that 30 ℃ of following vacuum drying 48h promptly obtain γ-PGA/CS Nano capsule.
The another kind of preparation method of γ-PGA/CS Nano capsule comprises the steps:
(1), the preparation of solution:
1., take by weighing γ-PGA solid and be dissolved in the ultra-pure water, obtaining mass concentration is γ-PGA aqueous solution of 0.05mg/mL～5mg/mL, regulating pH value is 6.0～8.0;
2., take by weighing the CS solid and be dissolved in 1% the acetum, obtaining mass concentration is the CS acetum of 0.1mg/mL～10 mg/mL, regulating pH value is 3.0～6.0;
3. take by weighing MgSO
47H
2O is dissolved in step 1. in gained γ-PGA aqueous solution, control Mg
2+Concentration be 0mol/L～2mol/L, obtain containing Mg
2+γ-PGA aqueous solution;
(2), with in the step (1): 2. the CS aqueous acetic acid of gained adds the Mg that contains of 3. gained by the mode that stirs while dripping
2+γ-PGA aqueous solution in, rate of addition is 0.5mL/h～5mL/h, mixing speed is 50r/min～200r/min, finally must contain Mg
2+γ-PGA aqueous solution and the mixed liquor of CS acetum;
Gamma-polyglutamic acid-(γ-PGA) and chitosan (CS) and Mg wherein
2+Proportioning press γ-PGA:CS:Mg
2+Be 1mg:1～90mg:2～90mol;
(3), with the Mg that contains of step (2) gained
2+The γ-PGA aqueous solution and the mixed liquor of CS acetum be to continue stirring reaction 10 min～120 min under 50 r/min～200 r/min conditions to obtain γ-PGA/CS Nano capsule solution at rotating speed;
(4), with the γ-PGA/CS Nano capsule solution centrifugal of step (3) gained, centrifugal condition is 1000 r/min～3000 r/min, centrifugation time is 5 min～10 min, collecting supernatant is 0.01MPa in vacuum, and temperature is that 30 ℃ of following vacuum drying 48h promptly obtain γ-PGA/CS Nano capsule.
γ of the present invention-PGA/CS Nano capsule mean diameter is 150～220nm, and polydispersity coefficient is 0.13～0.16.Can be used for coating medicines such as erythromycin, nifedipine.
Beneficial effect of the present invention
γ of the present invention-PGA/CS Nano capsule mainly is to utilize the product γ-PGA of biofermentation and natural extract product C S to form Nano capsule for feedstock production, the two all is not have good biocompatibility and biodegradability through the natural product of modifying, nontoxic to human body and environment, its mean diameter is 150～220nm, polydispersity coefficient is 0.13～0.16, can be used as the carrier of medicines such as erythromycin, nifedipine, also can be used for the embedding of functional food and essence, promptly be specially adapted to food and field of medicaments.
In addition, the preparation method of Nano capsule of the present invention is to carry out at normal temperatures and pressures, and condition is relatively gentleer, is more conducive to extensive expansion and produces.Because the system of preparation Nano capsule is an aqueous solution, does not need other reagent, thereby reduced production cost simultaneously.
The specific embodiment
The reagent that the present invention is used:
Gamma-polyglutamic acid-: utilize bacillus subtilis to obtain containing the fermentation liquid of gamma-polyglutamic acid-, extract product in the fermentation liquid, the product that obtains after being further purified, its purity 〉=95% with isopropyl alcohol as precipitant again by fermenting and producing;
Chitosan: molecular weight is 150000, and deacetylation is 90%, biochemical reagents, the anodal bio tech ltd in Shanghai;
MgSO
47H
2O: analytical pure, sigma company produces;
The laser particle analyzer that the present invention is used: Nano-ZS nano particle size laser device, Britain Ma Erwen.
Embodiment 1
Precision takes by weighing γ-PGA solid 0.0250 g, is settled to 25 mL with ultra-pure water, and regulating pH value is 7.4, and obtaining concentration is γ-PGA aqueous solution of 1 mg/mL; Precision takes by weighing CS solid 0.0500 g, and the acetum with 1% is settled to 50 mL, and regulating pH value is 6.0, obtains mass concentration and is the CS acetum of 1 mg/mL; Precision takes by weighing 0.2465 g MgSO
47H
2O is dissolved in the 20 mL CS acetums, Mg
2+Concentration be 0.001 mol/L.With flow velocity is that 0.5 mL/h is added drop-wise to 20 mL with 4 mL γ-PGA aqueous solution and contains Mg
2+The CS acetum in, mixing speed is 100 r/min, then continues stirring reaction 30 min with identical mixing speed.The mixed liquor that obtains is centrifugal 8 min under 2000 r/min, and collecting supernatant is 0.01MPa in vacuum, and temperature is that 30 ℃ of following vacuum drying 48h obtain γ-PGA/CS Nano capsule.
Utilize laser particle analyzer to measure its mean diameter and be 175.0nm, polydispersity coefficient is 0.093.
Embodiment 2
Precision takes by weighing γ-PGA solid 0.0250 g, is settled to 25 mL with ultra-pure water, and regulating pH value is 7.4, and obtaining concentration is γ-PGA aqueous solution of 1 mg/mL; Precision takes by weighing CS solid 0.0500 g, and the acetum with 1% is settled to 50 mL, and regulating pH value is 6.0, obtains mass concentration and is the CS acetum of 1 mg/mL; Precision takes by weighing 0.4930 g MgSO
47H
2O is dissolved in the 20 mL CS acetums, Mg
2+Concentration be 0.002 mol/L.With flow velocity is that 1.0 mL/h are added drop-wise to 10 mL with 10 mL γ-PGA aqueous solution and contain Mg
2+The CS acetum in, mixing speed is 100 r/min, then continues stirring reaction 30 min with identical mixing speed.The mixed liquor that obtains is centrifugal 8 min under 2000 r/min, and collecting supernatant is 0.01MPa in vacuum, and temperature is that 30 ℃ of following vacuum drying 48h obtain γ-PGA/CS Nano capsule.
Utilize laser particle analyzer to measure its mean diameter and be 158.5nm, polydispersity coefficient is 0.132.
Embodiment 3
Precision takes by weighing γ-PGA solid 0.0100 g, is settled to 50 mL with ultra-pure water, and regulating pH value is 7.4, and obtaining concentration is γ-PGA aqueous solution of 0.2 mg/mL; Precision takes by weighing CS solid 0.1000 g, and the acetum with 1% is settled to 50 mL, and regulating pH value is 3.0, obtains mass concentration and is the CS acetum of 2 mg/mL; Precision takes by weighing 0.2465 g MgSO
47H
2O is dissolved in the 20 mL CS acetums, Mg
2+Concentration be 0.001 mol/L.With flow velocity is that 0.5 mL/h is added drop-wise to 10 mL with 2 mL γ-PGA aqueous solution and contains Mg
2+The CS acetum in, mixing speed is 100 r/min, then continues stirring reaction 60 min with identical mixing speed.The mixed liquor that obtains is centrifugal 8 min under 2000 r/min, and collecting supernatant is 0.01MPa in vacuum, and temperature is that 30 ℃ of following vacuum drying 48h obtain γ-PGA/CS Nano capsule.
Utilize laser particle analyzer to measure its mean diameter and be 215.4nm, polydispersity coefficient is 0.139.
Embodiment 4
Precision takes by weighing γ-PGA solid 0.0050 g, is settled to 50 mL with ultra-pure water, and regulating pH value is 7.4, and obtaining concentration is γ-PGA aqueous solution of 0.1 mg/mL; Precision takes by weighing CS solid 0.0500 g, and the acetum with 1% is settled to 50 mL, and regulating pH value is 6.0, and obtaining mass concentration is the CS acetum of 1 mg/mL; Precision takes by weighing 0.2465 g MgSO
47H
2O is dissolved in the 20 mL CS acetums, Mg
2+Concentration be 0.001 mol/L.With flow velocity is that 0.5 mL/h is added drop-wise to 18 mL with 2 mL γ-PGA aqueous solution and contains Mg
2+The CS acetum in, mixing speed is 100 r/min, then continues stirring reaction 60 min with identical mixing speed.The mixed liquor that obtains is centrifugal 8 min under 2000 r/min, and collecting supernatant is 0.01MPa in vacuum, and temperature is that 30 ℃ of following vacuum drying 48h obtain γ-PGA/CS Nano capsule.
Utilize laser particle analyzer to measure its mean diameter and be 170.5nm, polydispersity coefficient is 0.163.
Embodiment 5
Precision takes by weighing CS solid 0.1000 g, and the acetum with 1% is settled to 200 mL, and regulating pH value is 6.0, and obtaining mass concentration is the CS acetum of 0.5 mg/mL; Precision takes by weighing γ-PGA solid 0.0250 g, is settled to 50 mL with ultra-pure water, and regulating pH value is 7.0, and obtaining concentration is γ-PGA aqueous solution of 0.5mg/mL; Precision takes by weighing 0.2465 g MgSO
47H
2O is dissolved in 10 mL γ-PGA aqueous solution, Mg
2+Concentration be 0.002 mol/mL.With flow velocity is that 1 mL/h is added to 20 mL with 5 mLCS drips of solution and contains Mg
2+γ-PGA aqueous solution in, mixing speed is 120 r/min, then continues stirring reaction 30 min with identical mixing speed.The mixed liquor that obtains is centrifugal 7 min under 2000 r/min, and collecting supernatant is 0.01MPa in vacuum, and temperature is that 30 ℃ of following vacuum drying 48h obtain γ-PGA/CS Nano capsule.
Utilize laser particle analyzer to measure its mean diameter and be 200.6nm, polydispersity coefficient is 0.145.
Above said content only is the basic explanation of the present invention under conceiving, and according to any equivalent transformation that technical scheme of the present invention is done, all should belong to protection scope of the present invention.
Claims (8)
1. γ-PGA/CS Nano capsule is characterized in that raw material gamma-polyglutamic acid-(γ-PGA) and chitosan (CS) and Mg
2+Proportioning press γ-PGA:CS:Mg
2+Be 1mg:1～90mg:2～90mol, utilize polyelectrolyte self assembly principle to make capsule;
Promptly at first prepare the gamma-polyglutamic acid-aqueous solution and the chitosan-acetic acid solution of variable concentrations, at finite concentration Mg
2+Ion exists down, obtains Nano capsule solution by the mode that stirs while dripping, and drying obtains gamma-polyglutamic acid-/chitosan nano capsule then.
2. the preparation method of a kind of γ as claimed in claim 1-PGA/CS Nano capsule is characterized in that specifically comprising the steps:
(1), the preparation of solution:
1., take by weighing γ-PGA solid and be dissolved in the ultra-pure water, obtaining mass concentration is γ-PGA aqueous solution of 0.05mg/mL～5mg/mL, regulating pH value is 6.0～8.0;
2., take by weighing the CS solid and be dissolved in 1% the acetum, obtaining mass concentration is the CS acetum of 0.1mg/mL～10mg/mL, regulating pH value is 3.0～6.0;
3., take by weighing MgSO
47H
2O is dissolved in step 2. in the gained CS acetum, control Mg
2+Concentration be 0mol/L～2mol/L, obtain containing Mg
2+The CS acetum;
(2), with in the step (1): 1. the γ of gained-PGA aqueous solution adds the 3. Mg of gained by the mode that stirs while dripping
2+The CS acetum in, rate of addition is 0.5mL/h～5mL/h, mixing speed is 50r/min～200r/min, final γ-PGA aqueous solution with contain Mg
2+The mixed liquor of CS acetum;
Gamma-polyglutamic acid-(γ-PGA) and chitosan (CS) and Mg wherein
2+Proportioning press γ-PGA:CS:Mg
2+Be 1mg:1～90mg:2～90mol;
(3), the mixed liquor with step (2) gained is to continue stirring reaction 10min～120min under 50r/min～200r/min condition to obtain γ-PGA/CS Nano capsule solution at rotating speed;
(4), with the γ-PGA/CS Nano capsule solution centrifugal of step (3) gained, centrifugal condition is 1000r/min～3000r/min, centrifugation time is 5min～10min, and collecting supernatant is 0.01MPa in vacuum, and temperature is that 30 ℃ of following vacuum drying 48h promptly obtain γ-PGA/CS Nano capsule.
3. the preparation method of a kind of γ as claimed in claim 2-PGA/CS Nano capsule is characterized in that:
In the step (1): γ 1.-PGA aqueous solution mass concentration is 1mg/mL, and pH value is 7.4;
2. CS acetum mass concentration is 1mg/mL, and regulating pH value is 6.0;
3. contain Mg
2+The CS acetum in Mg
2+Concentration be 1mol/L;
In the step (2): in step (1): 1. the γ of gained-PGA aqueous solution adds the 3. Mg of gained by the mode that stirs while dripping
2+The CS acetum in, rate of addition is 0.5mL/h, mixing speed is 100r/min, final γ-PGA aqueous solution with contain Mg
2+The mixed liquor of CS acetum;
Gamma-polyglutamic acid-(γ-PGA) and chitosan (CS) and Mg wherein
2+Proportioning press γ-PGA:CS:Mg
2+Be 1mg:5mg:5mol;
In the step (3): is to continue stirring reaction 30min under the 100r/min condition to obtain γ-PGA/CS Nano capsule solution with the mixed liquor of step (2) gained at rotating speed;
In the step (4): with the γ-PGA/CS Nano capsule solution centrifugal of step (3) gained, centrifugal condition is 2000r/min, centrifugation time is 8min, and collecting supernatant is 0.01MPa in vacuum, and temperature is that 30 ℃ of following vacuum drying 48h promptly obtain γ-PGA/CS Nano capsule.
4. the preparation method of a kind of γ as claimed in claim 2-PGA/CS Nano capsule is characterized in that in the step (1): γ 1.-PGA aqueous solution mass concentration is 1mg/mL, and pH value is 7.4;
2. CS acetum mass concentration is 1mg/mL, and regulating pH value is 6.0;
3. contain Mg
2+The CS acetum in Mg
2+Concentration be 2mol/L;
(2), with in the step (1): 1. the γ of gained-PGA aqueous solution adds the 3. Mg of gained by the mode that stirs while dripping
2+The CS acetum in, rate of addition is 1.0mL/h, mixing speed is 100r/min, final γ-PGA aqueous solution with contain Mg
2+The mixed liquor of CS acetum;
Gamma-polyglutamic acid-(γ-PGA) and chitosan (CS) and Mg wherein
2+Proportioning press γ-PGA:CS:Mg
2+Be 1mg:1mg:2mol;
(3), the mixed liquor with step (2) gained is to continue stirring reaction 30min under the 100r/min condition to obtain γ-PGA/CS Nano capsule solution at rotating speed;
(4), with the γ-PGA/CS Nano capsule solution centrifugal of step (3) gained, centrifugal condition is 2000r/min, centrifugation time is 8min, and collecting supernatant is 0.01MPa in vacuum, and temperature is that 30 ℃ of following vacuum drying 48h promptly obtain γ-PGA/CS Nano capsule.
5. the preparation method of a kind of γ as claimed in claim 2-PGA/CS Nano capsule is characterized in that:
In the step (1): γ 1.-PGA aqueous solution mass concentration is 0.2mg/mL, and pH value is 7.4;
2. CS acetum mass concentration is 2mg/mL, and regulating pH value is 3.0;
3. contain Mg
2+The CS acetum in Mg
2+Concentration be 1mol/L;
In the step (2): in step (1): 1. the γ of gained-PGA aqueous solution adds the 3. Mg of gained by the mode that stirs while dripping
2+The CS acetum in, rate of addition is 0.5mL/h, mixing speed is 100r/min, final γ-PGA aqueous solution with contain Mg
2+The mixed liquor of CS acetum;
Gamma-polyglutamic acid-(γ-PGA) and chitosan (CS) and Mg wherein
2+Proportioning press γ-PGA:CS:Mg
2+Be 1mg:50mg:25mol;
In the step (3): is to continue stirring reaction 60min under the 100r/min condition to obtain γ-PGA/CS Nano capsule solution with the mixed liquor of step (2) gained at rotating speed;
In the step (4): with the γ-PGA/CS Nano capsule solution centrifugal of step (3) gained, centrifugal condition is 2000r/min, centrifugation time is 8min, and collecting supernatant is 0.01MPa in vacuum, and temperature is that 30 ℃ of following vacuum drying 48h promptly obtain γ-PGA/CS Nano capsule.
6. the preparation method of a kind of γ as claimed in claim 2-PGA/CS Nano capsule is characterized in that:
In the step (1): γ 1.-PGA aqueous solution mass concentration is 0.1mg/mL, and pH value is 7.4;
2. CS solution quality concentration is 1mg/mL, and regulating pH value is 6.0;
3. contain Mg
2+The CS acetum in Mg
2+Concentration be 1mol/L;
In the step (2): in step (1): 1. the γ of gained-PGA aqueous solution is by stirring while dripping
The mode of mixing adds the 3. Mg of gained
2+The CS acetum in, rate of addition is 0.5mL/h, mixing speed is 100r/min, final γ-PGA aqueous solution with contain Mg
2+The mixed liquor of CS acetum;
Gamma-polyglutamic acid-(γ-PGA) and chitosan (CS) and Mg wherein
2+Proportioning press γ-PGA:CS:Mg
2+Be 1mg:90mg:90mol;
In the step (3): is to continue under the 100r/min condition the mixed liquor of step (2) gained at rotating speed
Continuous stirring reaction 60min obtains γ-PGA/CS Nano capsule solution;
In the step (4): with the γ-PGA/CS Nano capsule solution centrifugal of step (3) gained, centrifugal condition is 2000r/min, centrifugation time is 8min, and collecting supernatant is 0.01MPa in vacuum, and temperature is that 30 ℃ of following vacuum drying 48h promptly obtain γ-PGA/CS Nano capsule.
7. the preparation method of a kind of γ as claimed in claim 1-PGA/CS Nano capsule is characterized in that specifically comprising the steps:
1., take by weighing γ-PGA solid and be dissolved in the ultra-pure water, obtaining mass concentration is γ-PGA aqueous solution of 0.05 mg/mL～5 mg/mL, regulating pH value is 6.0～8.0;
2., take by weighing the CS solid and be dissolved in 1% the acetum, obtaining mass concentration is the CS acetum of 0.1 mg/mL～10 mg/mL, regulating pH value is 3.0～6.0;
3. take by weighing MgSO
47H
2O is dissolved in step 1. in gained γ-PGA aqueous solution, control Mg
2+Concentration be 0 mol/L～2mol/L, obtain containing Mg
2+γ-PGA aqueous solution;
(2), with in the step (1): 2. the CS acetum of gained adds the Mg that contains of 3. gained by the mode that stirs while dripping
2+γ-PGA aqueous solution in, rate of addition is 0.5mL/h～5mL/h, mixing speed is 50r/min～200r/min, finally must contain Mg
2+γ-PGA aqueous solution and the mixed liquor of CS acetum;
Gamma-polyglutamic acid-(γ-PGA) and chitosan (CS) and Mg wherein
2+Proportioning press γ-PGA:CS:Mg
2+Be 1mg:1～90mg:2～90mol;
(3), with the Mg that contains of step (2) gained
2+The γ-PGA aqueous solution and the mixed liquor of CS acetum be to continue stirring reaction 10min～120min under 50r/min～200r/min condition to obtain γ-PGA/CS Nano capsule solution at rotating speed;
(4), with the γ-PGA/CS Nano capsule solution centrifugal of step (3) gained, centrifugal condition is 1000r/min～3000r/min, centrifugation time is 5min～10min, and collecting supernatant is 0.01MPa in vacuum, and temperature is that 30 ℃ of following vacuum drying 48h promptly obtain γ-PGA/CS Nano capsule.
8. the preparation method of a kind of γ as claimed in claim 7-PGA/CS Nano capsule is characterized in that:
In the step (1): γ 1.-PGA aqueous solution mass concentration is 0.5mg/mL, and pH value is 7.0;
2. CS acetum mass concentration is 0.5mg/mL, and pH value is 6.0;
3. contain Mg
2+γ-PGA aqueous solution in Mg
2+Concentration be 2mol/L;
In the step (2): in step (1): 2. the CS acetum of gained adds the Mg that contains of 3. gained by the mode that stirs while dripping
2+γ-PGA aqueous solution in, rate of addition is 0.5mL/h～5mL/h, mixing speed is 50r/min～200r/min, finally must contain Mg
2+γ-PGA aqueous solution and the mixed liquor of CS acetum;
Gamma-polyglutamic acid-(γ-PGA) and chitosan (CS) and Mg wherein
2+Proportioning press γ-PGA:CS:Mg
2+Be 1mg:4mg:16mol;
In the step (3): is to continue stirring reaction 30min under the 120r/min condition to obtain γ-PGA/CS Nano capsule solution with the mixed liquor of step (2) gained at rotating speed;
In the step (4): with the γ-PGA/CS Nano capsule solution centrifugal of step (3) gained, centrifugal condition is 2000r/min, centrifugation time is 7min, and collecting supernatant is 0.01MPa in vacuum, and temperature is that 30 ℃ of following vacuum drying 48h promptly obtain γ-PGA/CS Nano capsule.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102977594A (en) * | 2012-12-13 | 2013-03-20 | 上海应用技术学院 | Gamma-polyglutamic acid/gelatin nanocapsules and preparation method thereof |
| CN103834036A (en) * | 2013-12-27 | 2014-06-04 | 长沙理工大学 | Chitosan and poly benzyl glutamate graft copolymer and preparation method thereof |
| CN106137780A (en) * | 2016-08-24 | 2016-11-23 | 广州睿森生物科技有限公司 | A kind of microcapsule containing dimethyl phthalate, mosquito-repellent water and preparation method thereof |
| CN109125290A (en) * | 2018-08-28 | 2019-01-04 | 江南大学 | A kind of pH and reduction double-response type drug-loading nanoparticles |
| CN109350606A (en) * | 2018-09-26 | 2019-02-19 | 青岛大学 | A kind of preparation method of polyelectrolyte hollow capsules and obtained hollow capsules |
| CN112064145A (en) * | 2020-09-21 | 2020-12-11 | 曲阜师范大学 | Preparation method of poly-gamma-glutamic acid/chitosan/nano-copper antibacterial composite fiber |
| CN112335887A (en) * | 2020-11-27 | 2021-02-09 | 曲阜师范大学 | Dietary silicon supplement and preparation process thereof |
| CN112425784A (en) * | 2020-11-27 | 2021-03-02 | 曲阜师范大学 | Preparation method of functional food for balancing intestinal flora and intestinal immunity |
| CN113730590A (en) * | 2021-09-07 | 2021-12-03 | 曲阜师范大学 | A microcapsule decoction piece for preventing and improving Alzheimer disease and dementia, and its preparation method |
| CN113768893A (en) * | 2021-09-17 | 2021-12-10 | 曲阜师范大学 | Microcapsule decoction pieces for embedding components for preventing and improving cardiovascular diseases and preparation method thereof |
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| CN102977594A (en) * | 2012-12-13 | 2013-03-20 | 上海应用技术学院 | Gamma-polyglutamic acid/gelatin nanocapsules and preparation method thereof |
| CN103834036A (en) * | 2013-12-27 | 2014-06-04 | 长沙理工大学 | Chitosan and poly benzyl glutamate graft copolymer and preparation method thereof |
| CN103834036B (en) * | 2013-12-27 | 2016-04-13 | 长沙理工大学 | Chitosan and poly benzyl glutamate graft copolymer and preparation method thereof |
| CN106137780A (en) * | 2016-08-24 | 2016-11-23 | 广州睿森生物科技有限公司 | A kind of microcapsule containing dimethyl phthalate, mosquito-repellent water and preparation method thereof |
| CN106137780B (en) * | 2016-08-24 | 2019-02-01 | 广州睿森生物科技有限公司 | A kind of microcapsules containing dimethyl phthalate, mosquito-repellent water and preparation method thereof |
| CN109125290A (en) * | 2018-08-28 | 2019-01-04 | 江南大学 | A kind of pH and reduction double-response type drug-loading nanoparticles |
| CN109125290B (en) * | 2018-08-28 | 2020-10-09 | 江南大学 | PH and reduction dual-response drug-loaded nanoparticle |
| CN109350606B (en) * | 2018-09-26 | 2021-08-13 | 青岛大学 | Preparation method of polyelectrolyte hollow capsule and hollow capsule obtained by preparation method |
| CN109350606A (en) * | 2018-09-26 | 2019-02-19 | 青岛大学 | A kind of preparation method of polyelectrolyte hollow capsules and obtained hollow capsules |
| CN112064145A (en) * | 2020-09-21 | 2020-12-11 | 曲阜师范大学 | Preparation method of poly-gamma-glutamic acid/chitosan/nano-copper antibacterial composite fiber |
| CN112425784A (en) * | 2020-11-27 | 2021-03-02 | 曲阜师范大学 | Preparation method of functional food for balancing intestinal flora and intestinal immunity |
| CN112335887A (en) * | 2020-11-27 | 2021-02-09 | 曲阜师范大学 | Dietary silicon supplement and preparation process thereof |
| FR3116719A1 (en) * | 2020-11-27 | 2022-06-03 | Qufu Normal University | Silicon-Based Food Supplement and Process for Its Preparation |
| CN112425784B (en) * | 2020-11-27 | 2023-02-03 | 曲阜师范大学 | Preparation method of functional food for balancing intestinal flora and intestinal immunity |
| CN113730590A (en) * | 2021-09-07 | 2021-12-03 | 曲阜师范大学 | A microcapsule decoction piece for preventing and improving Alzheimer disease and dementia, and its preparation method |
| CN113768893A (en) * | 2021-09-17 | 2021-12-10 | 曲阜师范大学 | Microcapsule decoction pieces for embedding components for preventing and improving cardiovascular diseases and preparation method thereof |
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