CN106380636B - A kind of resistant starch carrier material of chitosan graft and its preparation method and application - Google Patents
A kind of resistant starch carrier material of chitosan graft and its preparation method and application Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L5/00—Compositions of polysaccharides or of their derivatives not provided for in groups C08L1/00 or C08L3/00
- C08L5/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
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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
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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
- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
- A61K9/5005—Wall or coating material
- A61K9/5021—Organic macromolecular compounds
- A61K9/5036—Polysaccharides, e.g. gums, alginate; Cyclodextrin
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
- C08J3/246—Intercrosslinking of at least two polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L3/00—Compositions of starch, amylose or amylopectin or of their derivatives or degradation products
- C08L3/04—Starch derivatives, e.g. crosslinked derivatives
- C08L3/06—Esters
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2303/00—Characterised by the use of starch, amylose or amylopectin or of their derivatives or degradation products
- C08J2303/04—Starch derivatives
- C08J2303/06—Esters
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
- C08J2305/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/16—Applications used for films
Abstract
A kind of resistant starch carrier material of chitosan graft of the present invention and its preparation method and application, comprising the following steps: choose the acetate resistant starch that degree of substitution is 0.1~3.0 and dissolve 20~40min in organic solvent at 40~60 DEG C；Chitosan is added under agitation；Then initiator, activator and crosslinking agent are sequentially added, cooling after reaction 15min~50min is mediated at 40 DEG C~80 DEG C, with the resistant starch carrier material of the as chitosan graft obtained after ethanol precipitation and drying.The present invention passes through the coating thickness of suitable control carrier material, and preparation of the function factor in upper digestive tract is no more than 30%, and the release rate in simulation colonic environment is up to 50% or more.The acetate resistant starch carrier material of chitosan graft realizes colon targeting controlled release characteristic of the function factor in the storage stability and human body alimentary canal environment in food liquid system.
Description
Technical field
The present invention designs natural polysaccharide material in the research and development in functional activity substance control release field, especially relates to
And the polysaccharide films coating composite carrier and polysaccharide films coating composite carrier of a kind of load function factor are in food
In preservation mechanism and its Transmission system in human body and the control of function factor is discharged.
Background technique
Function factor is the material base of functional food, by the target controlling and releasing Transmission system energy for designing food function factor
It solves the problems, such as the processing faced and physiologic barrier, prevents due to the period of processing and storing especially food liquid system and Human Physiology
Function factor caused by environment destroys, so that it is guaranteed that effective performance of food function.Carrier material is mentioned in function factor stability
High and biology transmission use aspects play an important role, and good biocompatibility, biodegradable possessed by natural polysaccharide, price
The advantages that cheap, is widely used in field of food and medicine as carrier material.
Currently, very extensive as the research of controlled release system carrier material for starch both at home and abroad.Saboktakin etc. exists
Nano particle is prepared for by the electrostatic interaction of CS and carboxymethyl starch under temperate condition, (Saboktakin M R,
Tabatabaie R M,Maharramov A,et al.Synthesis and in vitro evaluation of
carboxymethyl starch–chitosan nanoparticles as drug delivery system to the
colon[J].International Journal of Biological Macromolecules,2011,48(3):381-
385) nano particle in methanol solution assembles 5-ASA by suction-operated, and determines both polyelectrolyte
Zeta- current potential and granularity and the granule size for assembling micro-capsule obtain assembling micro-capsule in neutrality in simulation extracorporeal releasing experiment
Rate of release in solution is maximum, and h substance has been separated by electrophoresis out by SDS-PAGE, has demonstrated 5-ASA from nano particle
Release is based on ion exchange mechanism.Researcher thinks can disappearing for the realization assembling micro-capsule by adjusting the ratio of polyelectrolyte
Change road targeting delivery.Kailasapathy etc. is induced with calcium ion, prepares alginate-amylomaize microcapsules
(Kailasapathy K.Survival of free and encapsulated probiotic bacteria and
their effect on the sensory properties of yoghurt[J].Lwt-Food Science and
Technology, 2006,39 (10): 1221-1227.), lactobacillus acidophilus and bifidobacterium lactis are embedded, are added to
In Yoghourt.The rear acidification for being added to the Yoghourt of embedding strain is slower than the Yoghourt for directly adding strain, and the generation of exocellular polysaccharide is also compared
The Yoghourt for not adding embedding strain is more.The system research of the present inventor team hydroxypropyl and carboxymethyl etherification, crosslinking, esterification
Etc. chemical modifications to the digestic property of starch and the affecting laws of digestion resistibility.On this basis, the present inventor team utilizes
The characteristic of resistant starch develops New film coating piece, the bone for being suitable as functional activity component colon site Targeting delivery
Frame piece and film coating pellet Transmission system, and obtain and function ingredients target is reached based on the regulation of starch carrier material digestic property
The method transmitted to controlled release.Meanwhile the molecular specificity recognition mechanism based on sugar chain in glycoprotein, it successfully constructs anti-digestion and forms sediment
Powder oral colon-target adheres to carrier material and its solid-state controlled release micro pill Transmission system.
In addition, also having extensive research to the controlled release system based on chitosan both at home and abroad.Li Jing etc. is with water soluble chitosan
Basic material has studied a kind of tumour cell targeting technology (Li Jing that novel receptor-ligand (GLUT1-glucose) mediates
The building of nano-carrier system based on chitosan and its cancer target Journal of Sex Research [D] Chinese Marine University, 2012) select Ah
Mycin prepares DOX-FWSC nanoparticle and DOX-FGSC nanoparticle as model drug, average grain diameter be respectively 136.6nm and
153.1nm, dose are respectively 12.53% and 20.1%；Encapsulation rate is respectively 40.37% and 64.8%.It is tired both in 118h
Product drug release amount is respectively 92% and 85%, as a result illustrates that two kinds of prepared drug-carrying nanometer particles all have preferably slow controlled release properties
It carries.Khunawattanakul etc. is prepared for nanometer thin by the electrostatic interaction assembling between chitosan and zeopan
Film (Khunawattanakul W, Puttipipatkhachorn S, Rades T, et al.Novel chitosan-
magnesium aluminum silicate nanocomposite film coatings for modified-release
Tablets [J] .International Journal of Pharmaceutics, 2011,407 (1-2): 132-41) experiment
Confirm that assembling micro-capsule reduces degradation of the chitosan in gastric juice, and compared with individual chitosan film, drug release
Rate decreases, and adjusts the rate of release of drug, by the mass ratio between control chitosan and zeopan with reality
Existing alimentary canal targeting delivery.
In order to ensure effective performance of food function factor effect, it is necessary to take into account the period of processing and storing and human physiological environment
Caused function factor destroys, and the carrier material of research institute's exploitation at present fails to take into account the matching of the two.Currently, passing through
Chitosan and resistant starch grafting prepare the research work of function factor controlled release carrier material and its controlled release Transmission system in state
It does not report inside.
Summary of the invention
The deficiency of release carrier material preparation, one of the technical problem to be solved in the present invention are controlled for the existing capability factor
It is that chitosan-acetate resistant starch copolymer is obtained by the method for grafting.It is big by the molecular weight for regulating and controlling chitosan
The small degree of substitution with acetate starch, to be used to more preferable generation graft reaction.Meanwhile reasonable crosslinking agent and its dosage are selected,
A kind of nontoxic, of low pollution, thin film coating material conveniently, controllably are obtained under reasonable reaction condition.
The second technical problem to be solved by the present invention is a kind of resistant starch carrier material conduct of chitosan graft
The application of drug and food function factor control release carrier material.
The purpose of the present invention is achieved through the following technical solutions:
A kind of resistant starch carrier material of chitosan graft and preparation method thereof, which is characterized in that including following step
It is rapid:
It chooses the acetate resistant starch that degree of substitution is 0.1~3.0 and dissolves 20 in organic solvent at 40~60 DEG C
~40min；It is 2.0 × 10 that molecular weight is added under agitation4G/mol~4.0 × 105The chitosan of g/mol；Then successively
Initiator, activator and crosslinking agent is added, cooling after reaction 15min~50min is mediated at 40 DEG C~80 DEG C, uses ethanol precipitation
And the resistant starch carrier material of the as chitosan graft obtained after drying.
The mass ratio of the chitosan and acetate resistant starch is 1:1.
The organic solvent is dimethyl sulfoxide.
The mass ratio of the acetate resistant starch and organic solvent is 1:20~2:3.
The initiator is potassium peroxydisulfate and anhydrous sodium sulfite, and activator is ammonium ceric nitrate, crosslinking agent N, N '-methylene
Base bisacrylamide.
The mass ratio of the potassium peroxydisulfate, anhydrous sodium sulfite, ammonium ceric nitrate and N, N '-methylene-bisacrylamide are 1:
0.02:0.1:(0.01~0.028).
The time interval that the initiator, activator and crosslinking agent are added is 2~5min.
The resistant starch carrier material of the chitosan graft of above method preparation.
Food system function factor pellet is oral to disappear the resistant starch carrier material of the chitosan graft preparing
Change the application in road controlled release membranes coated systems.Concrete application is the resistant starch carrier material using chitosan graft to function
Particle, pellet or the tablet of the energy factor are coated, and oral digestion road controlled release membranes coated systems are obtained, by the film coating system
It unites for the control release to function factor.
Chitosan has different pH value responsiveness, it can be made one by characteristics such as the molecular structures of adjusting chitosan
Cannot be dissolved under the pH environment of fixed food system and under the low in acidity environment of human stomach water absorption and swelling and dissolve characteristic.It is anti-
Digestible starch, which has, is not degraded by gastric acid in human body upper digestive tract and various digestive ferments, but can be by microbial degradation in colon
Characteristic.The present invention can take into account function by the polysaccharide composite carrier material that resistant starch and chitosan graft are formed to filter out
The factor targets the function factor controlled release occlusion vehicle material that control discharges in storage stability and human body alimentary canal in food system
Material and its controlled release Transmission system.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) according to demand of both target controlling and releasing characteristic in the storage stability of function factor and human body alimentary canal, from
The angle of function factor storage stability and biological utilisation validity is taken into account, designs and is suitble to function factor control in food liquid system
The polysaccharide carrier material and its controlled release Transmission system for making release, improve the bioavilability of function factor.
(2) the pH response performance of the colon targeting controlled release characteristic of acetate resistant starch and chitosan is combined,
The acetate resistant starch for filtering out the chitosan graft of function factor control release in suitable food liquid system is compound more
Sugared film coating carrier material, and by regulating and controlling it in the filming performance on pellet surface, construct suitable food liquid system
Polysaccharide films coating micro-pill Transmission system with pH responsiveness and colon targeting controlled release characteristic.
(3) coating thickness of suitable control carrier material, preparation of the function factor in upper digestive tract are no more than
30%, and the release rate in simulation colonic environment is up to 50% or more.With the acetate resistant starch film packet of single layer
Clothing pellet (identical acetate starch coating weight gain) is compared, the acetate resistant starch film coating micro-pill of chitosan graft
It is special to realize colon targeting controlled release of the function factor in the storage stability and human body alimentary canal environment in food liquid system
Property.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail, but embodiment of the present invention is not limited in
This.
Embodiment 1
Prepare acetate resistant starch (the specific preparation method reference: Journal of that 5g degree of substitution is 0.1
Agricultural and food chemistry, 2011,59 (10): 5738-5745) at 40 DEG C in 95g dimethyl sulfoxide
Middle dissolution 20min.Being transferred in kneading reactor later and 5g molecular weight is added while stirring is 2.0 × 104The chitosan of g/mol,
5g potassium peroxydisulfate and 0.1g anhydrous sodium sulfite are added after 2min, then every 2min sequentially add 0.5g ammonium ceric nitrate and
0.05gN, N '-methylene-bisacrylamide.Cooling terminate is reacted after then reacting 15min at 40 DEG C, is done with after ethanol precipitation
It is dry.
The acetate resistant starch for the chitosan graft being prepared is configured to acetone to 4% coating solution, is being flowed
Change the 5-ASA pellet surface in bed at 40 DEG C by its even application in partial size for 0.5-0.7mm, the vinegar of chitosan graft is made
Acid esters resistant starch film coating micro-pill.The pellet is stored and releasing in the in-vitro simulated digestive tract environment of people in Yoghourt system
It puts performance and chitosan film coating, the comparison of acetate resistant starch film coating micro-pill release performance is as shown in table 1.By
Table data comparison is it is found that the coating obtained of the acetate resistant starch control slow releasing carrier material of resulting chitosan graft is micro-
Ball has less leakage rate in Yoghourt system, and adds up release rate in colonic fluid and dramatically increase.
Table 1
Embodiment 2
Prepare acetate resistant starch (the specific preparation method reference: Journal of that 5g degree of substitution is 0.1
Agricultural and food chemistry, 2011,59 (10): 5738-5745) it is sub- in 7.5g dimethyl at 40 DEG C
40min is dissolved in sulfone.Then being transferred in kneading reactor and 5g molecular weight is added while stirring is 4.0 × 105The shell of g/mol is poly-
5g potassium peroxydisulfate and 0.1g anhydrous sodium sulfite are added after 2min, then sequentially adds 0.5g ammonium ceric nitrate every 2min for sugar, and
0.07gN, N '-methylene-bisacrylamide.Cooling terminate is reacted after then reacting 20min at 80 DEG C, with drying after ethanol precipitation.
The acetate resistant starch for the chitosan graft being prepared is configured to acetone to 4% coating solution, is being flowed
Change the 5-ASA pellet surface in bed at 40 DEG C by its even application in partial size for 0.5-0.7mm, the vinegar of chitosan graft is made
Acid esters resistant starch film coating micro-pill.The pellet is stored and releasing in the in-vitro simulated digestive tract environment of people in Yoghourt system
It puts performance and chitosan film coating, the comparison of acetate resistant starch film coating micro-pill release performance is as shown in table 2.By
Table data comparison is it is found that the coating obtained of the acetate resistant starch control slow releasing carrier material of resulting chitosan graft is micro-
Ball has less leakage rate in Yoghourt system, and the release rate in gastric juice and intestinal fluid is relative to Chitosan Coating pellet
It significantly reduces, but is higher than the release rate of acetate resistant starch coating micro-pill, and add up release rate in colonic fluid and dramatically increase.
Table 2
Embodiment 3
Prepare acetate resistant starch (the specific preparation method reference: Journal of that 5g degree of substitution is 1.9
Agricultural and food chemistry, 2011,59 (10): 5738-5745) at 60 DEG C in 30g dimethyl sulfoxide
Dissolve 20min.Then being transferred in kneading reactor and 5g molecular weight is added while stirring is 2.0 × 104The chitosan of g/mol, 5min
5g potassium peroxydisulfate and 0.1g anhydrous sodium sulfite are added afterwards, then sequentially adds 0.5g ammonium ceric nitrate and 0.05gN, N '-every 5min
Methylene-bisacrylamide.Cooling terminate is reacted after then reacting 50min at 60 DEG C, with drying after ethanol precipitation.
The acetate resistant starch for the chitosan graft being prepared is configured to acetone to 4% coating solution, is being flowed
Change the 5-ASA pellet surface in bed at 40 DEG C by its even application in partial size for 0.5-0.7mm, the vinegar of chitosan graft is made
Acid esters resistant starch film coating micro-pill.The pellet is stored and releasing in the in-vitro simulated digestive tract environment of people in Yoghourt system
It puts performance and chitosan film coating, the comparison of acetate resistant starch film coating micro-pill release performance is as shown in table 3.By
Table data comparison is it is found that the coating obtained of the acetate resistant starch control slow releasing carrier material of resulting chitosan graft is micro-
Ball has less leakage rate in Yoghourt system, and adds up release rate in colonic fluid and dramatically increase.In gastric juice and intestinal fluid
Significant decrease of the release rate relative to Chitosan Coating pellet, but be higher than the release rate of acetate resistant starch coating micro-pill.
Table 3
Embodiment 4
Prepare acetate resistant starch (the specific preparation method reference: Journal of that 5g degree of substitution is 1.9
Agricultural and food chemistry, 2011,59 (10): 5738-5745) at 60 DEG C in 60g dimethyl sulfoxide
Middle dissolution 40min.Then being transferred in kneading reactor and 5g molecular weight is added while stirring is 4.0 × 105The chitosan of g/mol,
5g potassium peroxydisulfate and 0.1g anhydrous sodium sulfite are added after 5min, then every 5min sequentially add 0.5g ammonium ceric nitrate and
0.14gN, N '-methylene-bisacrylamide.Cooling terminate is reacted after then reacting 50min at 60 DEG C, is done with after ethanol precipitation
It is dry.
The acetate resistant starch for the chitosan graft being prepared is configured to acetone to 4% coating solution, is being flowed
Change the 5-ASA pellet surface in bed at 40 DEG C by its even application in partial size for 0.5-0.7mm, the vinegar of chitosan graft is made
Acid esters resistant starch film coating micro-pill.The pellet is stored and releasing in the in-vitro simulated digestive tract environment of people in Yoghourt system
It puts performance and chitosan film coating, the comparison of acetate resistant starch film coating micro-pill release performance is as shown in table 4.By
Table data comparison is it is found that the coating obtained of the acetate resistant starch control slow releasing carrier material of resulting chitosan graft is micro-
Ball has less leakage rate in Yoghourt system, adds up release rate in gastric juice and intestinal fluid and is minimized, and colon
Add up release rate in liquid to dramatically increase.
Table 4
Embodiment 5
Prepare acetate resistant starch (the specific preparation method reference: Journal of that 5g degree of substitution is 3
Agricultural and food chemistry, 2011,59 (10): 5738-5745) at 50 DEG C in 85g dimethyl sulfoxide
Middle dissolution 20min.Then being transferred in kneading reactor and 5g molecular weight is added while stirring is 2.0 × 104The chitosan of g/mol,
5g potassium peroxydisulfate and 0.1g anhydrous sodium sulfite are added after 3min, then every 3min sequentially add 0.5g ammonium ceric nitrate and
0.1gN, N '-methylene-bisacrylamide.Cooling terminate is reacted after then reacting 50min at 40 DEG C, is done with after ethanol precipitation
It is dry.
The acetate resistant starch for the chitosan graft being prepared is configured to acetone to 4% coating solution, is being flowed
Change the 5-ASA pellet surface in bed at 40 DEG C by its even application in partial size for 0.5-0.7mm, the vinegar of chitosan graft is made
Acid esters resistant starch film coating micro-pill.The pellet is stored and releasing in the in-vitro simulated digestive tract environment of people in Yoghourt system
It puts performance and chitosan film coating, the comparison of acetate resistant starch film coating micro-pill release performance is as shown in table 5.By
Table data comparison is it is found that the coating obtained of the acetate resistant starch control slow releasing carrier material of resulting chitosan graft is micro-
Ball has less leakage rate in Yoghourt system, and adds up release rate in colonic fluid and dramatically increase.
Table 5
Embodiment 6
Prepare acetate resistant starch (the specific preparation method reference: Journal of that 5g degree of substitution is 3
Agricultural and food chemistry, 2011,59 (10): 5738-5745) at 50 DEG C in 10g dimethyl sulfoxide
Middle dissolution 40min.Then being transferred in kneading reactor and 5g molecular weight is added while stirring is 4.0 × 105The chitosan of g/mol,
5g potassium peroxydisulfate and 0.1g anhydrous sodium sulfite are added after 3min, then every 3min sequentially add 0.5g ammonium ceric nitrate and
0.14gN, N '-methylene-bisacrylamide.Cooling terminate is reacted after then reacting 15min at 80 DEG C, is done with after ethanol precipitation
It is dry.
The acetate resistant starch for the chitosan graft being prepared is configured to acetone to 4% coating solution, is being flowed
Change the 5-ASA pellet surface in bed at 40 DEG C by its even application in partial size for 0.5-0.7mm, the vinegar of chitosan graft is made
Acid esters resistant starch film coating micro-pill.The pellet is stored and releasing in the in-vitro simulated digestive tract environment of people in Yoghourt system
It puts performance and chitosan film coating, the comparison of acetate resistant starch film coating micro-pill release performance is as shown in table 6.By
Table data comparison is it is found that the coating obtained of the acetate resistant starch control slow releasing carrier material of resulting chitosan graft is micro-
Ball has less leakage rate in Yoghourt system and gastric juice, intestinal fluid.
Table 6
Embodiment 7
Prepare acetate resistant starch (the specific preparation method reference: Journal of that 5g degree of substitution is 1.9
Agricultural and food chemistry, 2011,59 (10): 5738-5745) at 60 DEG C in 60g dimethyl sulfoxide
Middle dissolution 30min.Then being transferred in kneading reactor and 5g molecular weight is added while stirring is 1.5 × 105The chitosan of g/mol,
5g potassium peroxydisulfate and 0.1g anhydrous sodium sulfite are added after 3min, then every 3min sequentially add 0.5g ammonium ceric nitrate and
0.07gN, N '-methylene-bisacrylamide.Cooling terminate is reacted after then reacting 40min at 50 DEG C, is done with after ethanol precipitation
It is dry.
The acetate resistant starch for the chitosan graft being prepared is configured to acetone to 4% coating solution, is being flowed
Change the 5-ASA pellet surface in bed at 40 DEG C by its even application in partial size for 0.5-0.7mm, the vinegar of chitosan graft is made
Acid esters resistant starch film coating micro-pill.The pellet is stored and releasing in the in-vitro simulated digestive tract environment of people in Yoghourt system
It puts performance and chitosan film coating, the comparison of acetate resistant starch film coating micro-pill release performance is as shown in table 7.By
Table data comparison is it is found that the coating obtained of the acetate resistant starch control slow releasing carrier material of resulting chitosan graft is micro-
Ball, has less leakage rate in Yoghourt system, and gastric juice compares Chitosan Coating pellet with the preparation in intestinal fluid
It significantly reduces, and adds up release rate in colonic fluid and dramatically increased relative to acetate resistant starch coating micro-pill.
Table 7
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (11)
1. a kind of preparation method of the resistant starch carrier material of chitosan graft, which comprises the following steps:
It chooses the acetate resistant starch that degree of substitution is 0.1 ~ 3.0 and dissolves 20 ~ 40min in organic solvent at 40 ~ 60 DEG C；
It is 2.0 × 10 that molecular weight is added under agitation4g/mol ~4.0×105The chitosan of g/mol；Then initiation is sequentially added
Agent, activator and crosslinking agent are mediated cooling after reaction 15min ~ 50min at 40 DEG C ~ 80 DEG C, are obtained with after ethanol precipitation and drying
What is arrived is the resistant starch carrier material of chitosan graft.
2. the preparation method according to claim 1, which is characterized in that the chitosan and acetate resistant starch
Mass ratio is 1:1.
3. preparation method according to claim 2, which is characterized in that the organic solvent is dimethyl sulfoxide.
4. preparation method according to claim 3, which is characterized in that the acetate resistant starch and organic solvent
Mass ratio is 1:20 ~ 2:3.
5. preparation method according to claim 1 or 2 or 3 or 4, which is characterized in that the initiator be potassium peroxydisulfate and
Anhydrous sodium sulfite, activator are ammonium ceric nitrate, crosslinking agent N, N '-methylene-bisacrylamide.
6. preparation method according to claim 5, which is characterized in that the potassium peroxydisulfate, anhydrous sodium sulfite, cerous nitrate
Ammonium and N, the mass ratio of N '-methylene-bisacrylamide are 1:0.02:0.1:(0.01 ~ 0.028).
7. preparation method according to claim 6, which is characterized in that the initiator, activator and crosslinking agent were added
Time interval is 2 ~ 5 min.
8. the resistant starch carrier material of the chitosan graft of claim 1 ~ 7 any one the method preparation.
9. the resistant starch carrier material of chitosan graft according to any one of claims 8 is preparing food system function factor pellet
Application in oral digestion road controlled release membranes coated systems.
10. application according to claim 9, which is characterized in that utilize the resistant starch carrier material of chitosan graft
The pellet of function factor is coated, oral digestion road controlled release membranes coated systems is obtained, which is used for
Control release to function factor.
11. the resistant starch carrier material of chitosan graft according to any one of claims 8 is preparing food system function factor mouth
Take the application in alimentary canal controlled release membranes coated systems, which is characterized in that utilize the resistant starch carrier material of chitosan graft
Material is coated the particle or tablet of function factor, oral digestion road controlled release membranes coated systems is obtained, by the film coating
System is used for the control to function factor and discharges.
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| GB9412394D0 (en) * | 1994-06-21 | 1994-08-10 | Danbiosyst Uk | Colonic drug delivery composition |
| CN1219072C (en) * | 2003-12-12 | 2005-09-14 | 华南理工大学 | Digestion tolerant starch and its preparation method and uses |
| GB0607534D0 (en) * | 2006-04-13 | 2006-05-24 | Univ London Pharmacy | Colonic drug delivery formulation |
| CN101366946B (en) * | 2008-09-05 | 2010-06-02 | 华南理工大学 | Starch based segmented intestine targeting specific adhesion material, preparation and application thereof |
| CN101653609B (en) * | 2009-08-28 | 2011-07-06 | 华南理工大学 | Octenyl succinate starch with colon targeting controlled release function and preparation method thereof |
| EP2446877A1 (en) * | 2010-10-29 | 2012-05-02 | Roquette Frères | Modified starch derivative-based matrix for colon targeting |
| CN102250286B (en) * | 2011-05-30 | 2013-07-24 | 广西大学 | Preparation method of denatured starch special for preservative material |
| CN103992489A (en) * | 2014-03-14 | 2014-08-20 | 周忠凯 | Novel green processing method for increasing resistant starch content through crosslinking of starch and chitosan |
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2016
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