CN108816161A - A kind of preparation method being retained anti-oxidant starch base capsule - Google Patents
A kind of preparation method being retained anti-oxidant starch base capsule Download PDFInfo
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- CN108816161A CN108816161A CN201810593264.0A CN201810593264A CN108816161A CN 108816161 A CN108816161 A CN 108816161A CN 201810593264 A CN201810593264 A CN 201810593264A CN 108816161 A CN108816161 A CN 108816161A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
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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
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
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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
- C08J2351/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
- C08J2351/02—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to polysaccharides
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Abstract
The invention belongs to medical material preparation technical fields, and in particular to a kind of preparation method for being retained anti-oxidant starch base capsule.The present invention is raw material using corn flour,The water imbibitions group such as hydroxyl that the corn starch base after water suction exposes,The Hyarogen-bonding of composition is bigger,Water conservation after being conducive to water suction,The calcium chloride mixed in starch capsule is permeable in the spacial framework of grafting corn flour,The moisture-holding capacity of starch base capsule can be improved,So that starch base capsule keeps high-moisture,Water lock performance is improved,To make the flexibility of capsule be maintained,Soybean protein isolate is dispersed in loose porous sodium alginate gel,After oxidizing substance or illumination aoxidize soybean protein isolate,Breaks down into amino acids small molecule enters sodium alginate gel micropore,Decline wall material porosity,Improve oxygen barrier properties,Starch base capsule sorptivety lycopene extracting solution in the present invention,Oxidation reaction occurs for the filler for avoiding capsule,To reach oxidation resistant purpose.
Description
Technical field
The invention belongs to medical material preparation technical fields, and in particular to a kind of preparation for being retained anti-oxidant starch base capsule
Method.
Background technique
Capsule is widely used in medicine and food-processing industry as a kind of protectiveness lapping.According to capsule
Application demand can dissolve in water so that capsule material needs to possess certain water solubility and suitable mechanical strength
Content is discharged, while being able to maintain original form when by external force will not be damaged.
Gelatin is the traditional fabrication material of capsule, high mechanical strength, good toughness, while can be dissolved in 30 DEG C or more of water
In, it is so far still most widely used capsule material.But there are many disadvantages for gelatine capsule itself, such as：It is easy to cooperating microorganisms,
Frangible, ambient humidity is then easy to stick together with drug greatly, and the low then flexibility of ambient humidity is poor, frangible.In addition, gelatin point
Subchain contains a large amount of reactive groups, and reaction may be crosslinked with content drug.
So far, it is known that can be used for producing edible or medical capsule shells non-gelatin materials has：Hydroxypropyl methyl is fine
Tie up element, algal polysaccharides, pulullan polysaccharide, starch.Natural or modified starch is usually used in food or drug processing industry.By to day
The physics of right starch, chemical modification, make it have characteristic not available for ative starch, such as improve mobility, water solubility, film forming
Property, mechanical strength etc..From the aspect of the popularity in the prices of raw materials and source, starch is considered as that most potential capsule is former
Material, if the defect of plant capsule expensive raw material price and gelatine capsule can be made up using starch as capsule shells wall material.Starch
Capsule is as a kind of plant-derived products, and raw material sources are extensive, low in cost and safe and reliable, and working process simple flow is fast
The a variety of birth defects and risk disadvantage of gelatine capsule can be solved perfectly in victory, no animal endogenous pathogens and other sensitizers
End, is a kind of perfect substitute of gelatine capsule.
But starch hollow capsule launch is had not yet to see, main cause has：（1）Due to being easy to shape between starch molecule
At very strong hydrogen bond, starch film is brittle and frangible, it is difficult to intensity height, the Capsules of resistance to filling be made；（2）Starch capsule moisture retention
Can be bad, it is easy weathering dehydration and becomes fragile, cause capsule easily damaged when filling, it is difficult to required capsule be made, seriously affect
The popularization and application of starch capsule；（3）Since starch film forming is limited and mechanical performance is bad, viscosity or hardness are difficult to meet
The requirement of capsule is produced, while being easy the moisture absorption, capsule preservation condition is more demanding, and the shelf-life is not grown, therefore makes it in this neck
The successful application in domain is restricted.
Therefore, it is badly in need of providing that a kind of component is relatively easy, and performance of keeping humidity is good, starch base Capsules raw material at low cost
Composition and preparation method thereof.
Summary of the invention
Present invention mainly solves the technical issues of, for being retained at present, anti-oxidant starch base capsule performance of keeping humidity is bad, hold
Easy-weathering dehydration becomes fragile, and causes capsule easily damaged when filling, and it is poor to be retained anti-oxidant starch base capsule antioxygenic property, and capsule is protected
When depositing, the oxidizable defect of capsule filling provides a kind of preparation method for being retained anti-oxidant starch base capsule.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that：
A kind of preparation method being retained anti-oxidant starch base capsule, it is characterised in that specifically preparation step is：
（1）It takes 40~50g corn flour to be placed in conical flask, 3~5g alpha-amylase and sodium dihydrogen phosphate-phosphorus is added into conical flask
Sour disodium hydrogen buffer, constant volume is 100~110mL, then 8~10mL liquor natrii hypochloritis is added into conical flask, by conical flask
It is placed in oscillator, heating water bath heating, oscillating reactions is added 10~12mL sodium hydroxide solution into conical flask and terminates instead
It answers, obtains starch enzymolysis liquid；
（2）Above-mentioned starch enzymolysis liquid is placed in baking oven, heat temperature raising, it is dry, enzymatic hydrolysis corn flour is obtained, 20~25g enzyme is weighed
Solution corn flour is added in the three-necked flask with thermometer and nitrogen conduit, and 100~110mL distillation is added into three-necked flask
Water, to three-necked flask heat temperature raising, 10~15mL calcium chloride solution and acrylic acid is added to three-necked flask in preheating, is protected in nitrogen
Under shield, continue heat temperature raising, initiation reaction obtains performed polymer product；
（3）Sodium hydroxide solution is added to above-mentioned performed polymer product, neutralizes liquid pH in above-mentioned three-necked flask, continues by above-mentioned anti-
Conditioned response is answered, graft product is obtained, graft product is put into drying box, is heated to 40~45 DEG C, dry 4~5h,
3~4h of forced air drying under the conditions of 120~130 DEG C obtains grafting corn flour；
（4）Above-mentioned grafting corn flour is placed in the water-bath with blender, 40~50mL distilled water is added into water-bath,
Heat temperature raising, start blender, stir 20~25min, to water-bath be added 20~25g calcium chloride, continue stirring 40~
45min obtains starch base coagulant liquid；
（5）Tomato is taken to be put into beater, mashing crushes, and obtains slurries, adjusts slurries pH with sodium hydroxide solution, is alkalized
Alkalization slurries are placed in a beaker by slurries, and heat temperature raising stirs 5~7h, obtain pyrolysis slurries, and slurry temperature to be pyrolyzed is down to
Pyrolysis slurries filtering is removed residue and obtains tomato extracting solution by room temperature；
（6）According to parts by weight, 20~25 parts of soybean protein isolate solution, 100~120 parts of starch base coagulant liquids are poured into reaction
In kettle, starts blender with the revolving speed of 400~450r/min and stir 15~20min, then 5~10 parts of alginic acids are added to reaction kettle
Sodium solution, heat temperature raising, whipping process add gelatin viscosity in water management reaction kettle, and glue in reaction kettle is sent into capsule manufacture and is set
Starch capsule shells are prepared in standby, starch capsule shells are put into tomato extracting solution after sorptivety to be put into vacuum oven and are done
It is dry, it obtains being retained anti-oxidant starch base capsule.
Step（1）The sodium dihydrogen phosphate-disodium hydrogen phosphate pH of cushioning fluid is 7, the quality point of liquor natrii hypochloritis
Number is 0.1%, and heating water bath warming temperature is 42~45 DEG C, and oscillation revolving speed is 135~140r/min, the oscillating reactions time for 3~
4 days, the mass fraction of sodium hydroxide solution was 40%.
Step（2）The heat temperature raising temperature is 60~70 DEG C, and drying time is 8~9h, and heat temperature raising temperature is 45
~50 DEG C, preheating time is 10~15min, and the mass fraction of calcium chloride solution is 0.5%, and the additional amount of acrylic acid is that enzymatic hydrolysis is beautiful
Rice flour quality 17~20%, heat temperature raising temperature are 55~60 DEG C, and the initiation time is 30~35min.
Step（3）The mass fraction of the sodium hydroxide solution be 25%, neutralize three-necked flask in liquid pH be 6.5~
7.0, continue by the above-mentioned reaction condition reaction time to be 3~4h.
Step（4）The heating water bath warming temperature is 40~45 DEG C, and speed of agitator is 90~100r/min.
Step（5）The mashing grinding time is 20~30min, and the mass fraction of sodium hydroxide solution is 30%, is adjusted
Slurry pH value is 7.5~9.0, and heat temperature raising temperature is 50~60 DEG C.
Step（6）The mass fraction of the soybean protein isolate solution is 3%, and the mass fraction of sodium alginate soln is
5%, heat temperature raising temperature be 50~55 DEG C, control reaction kettle in gelatin viscosity be 200~300mPas, the sorptivety time be 2~
3h, the set temperature of vacuum oven are 45~50 DEG C.
The beneficial effects of the invention are as follows：
（1）After the present invention digests corn flour, more active sites and acrylic monomers graft copolymerization are exposed, in corn flour
After the amylopectin grafted propylene acid of the overwhelming majority, the three-dimensional netted space structure of diverging is presented, thus starch base capsule possesses
Fabulous water-swelling property, the starch base capsule fill volume expanded after water suction is also improved, in addition, corn starch base is sudden and violent
The water imbibitions group such as hydroxyl of exposing, the Hyarogen-bonding of composition is bigger, the water conservation after being conducive to water suction, after avoiding water suction excessive
Leakage, the calcium chloride that the present invention mixes in starch capsule is permeable in the spacial framework of grafting corn flour, can be improved
The moisture-holding capacity of starch base capsule arrives Water Molecular Adsorption since corn flour grafted propylene acid rear surface has a large amount of hydrophilic radicals
In gel structure, calcium chloride can be in water suction undersaturated condition always in this way, and the water absorbing properties of calcium chloride are stronger, starch
Base rubber capsule always exists water penetration pressure to the external world, so that starch base capsule keeps high-moisture, water lock performance is improved, to make
The flexibility of capsule is maintained；
（2）Using soybean protein isolate, enzymatic starch, sodium alginate as the wall material of capsule, soybean in starch base capsule in the present invention
Protein isolate is dispersed in loose porous sodium alginate gel, after oxidizing substance or illumination aoxidize soybean protein isolate, point
Solution enters sodium alginate gel micropore at amino acid small molecule, declines wall material porosity, improves oxygen barrier properties, and can subtract
Few light injects capsule, and when human body takes in capsule, there are the sodium that oxidisability high volence metal ion can replace sodium alginate in human body
Ion forming complex avoids it from further invading capsule to reach antioxidant effect, and starch base capsule passes through in the present invention
Sorptivety lycopene extracting solution, since lycopene is how unsaturated hydrocarbon, reproducibility is extremely strong, therefore passes through wall material
Oxidation occurs for the oxidizing substance meeting preferential oxidation lycopene entered behind anti-oxidant defence line, the filler for avoiding capsule instead
It answers, to reach oxidation resistant purpose.
Specific embodiment
40~50g corn flour is taken to be placed in conical flask, it is 7 that 3~5g alpha-amylase is added into conical flask and adds pH value
Sodium dihydrogen phosphate-disodium hydrogen phosphate buffer, constant volume is 100~110mL, then 8~10mL mass point is added into conical flask
The liquor natrii hypochloritis that number is 0.1%, conical flask is placed in oscillator, and heating water bath is warming up to 42~45 DEG C, with 135~
After oscillating reactions 3~4 days, the hydrogen-oxygen that 10~12mL mass fraction is 40% is added into conical flask for the speed oscillation of 140r/min
Change sodium solution and terminate reaction, obtains starch enzymolysis liquid；
Above-mentioned starch enzymolysis liquid is placed in baking oven, is heated to 60~70 DEG C, dry 8~9h obtains enzymatic hydrolysis corn flour, claims
It takes 20~25g enzymatic hydrolysis corn flour to be added in the three-necked flask with thermometer and nitrogen conduit, 100 is added into three-necked flask
~110mL distilled water is heated to 45~50 DEG C to three-necked flask, preheats 10~15min, 10 are added to three-necked flask~
The acrylic acid of calcium chloride solution and enzymatic hydrolysis corn flour quality 17~20% that 15mL mass fraction is 0.5%, under nitrogen protection, after
It is continuous to be heated to 55~60 DEG C, cause 30~35min, obtains performed polymer product；Quality point is added to above-mentioned performed polymer product
The sodium hydroxide solution that number is 25%, neutralizing liquid pH in above-mentioned three-necked flask is 6.5~7.0, is continued anti-by above-mentioned reaction condition
3~4h is answered, graft product is obtained, graft product is put into drying box, is heated to 40~45 DEG C, dry 4~5h, then at
3~4h of forced air drying under the conditions of 120~130 DEG C obtains grafting corn flour；Above-mentioned grafting corn flour is placed in blender
In water-bath, 40~50mL distilled water is added into water-bath, is heated to 40~45 DEG C, starts blender, with 90~
The revolving speed of 100r/min stirs 20~25min, and 20~25g calcium chloride is added to water-bath, continues 40~45min of stirring, obtains
Starch base coagulant liquid；Tomato is taken to be put into beater, mashing crushes 20~30min, obtains slurries, is 30% with mass fraction
It is 7.5~9.0 that sodium hydroxide solution, which adjusts slurry pH value, obtains alkalization slurries, alkalization slurries is placed in a beaker, heat temperature raising
To 50~60 DEG C, 5~7h is stirred, obtains pyrolysis slurries, slurry temperature to be pyrolyzed is down to room temperature, and pyrolysis slurries filtering removes
Residue obtains tomato extracting solution；According to parts by weight, by 20~25 parts of mass fractions be 3% soybean protein isolate solution, 100
~120 parts of starch base coagulant liquids pour into reaction kettle, start blender with the revolving speed of 400~450r/min and stir 15~20min,
The sodium alginate soln that 5~10 parts of mass fractions are 5% is added to reaction kettle again, is heated to 50~55 DEG C, whipping process adds
Gelatin viscosity is 200~300mPas in water management reaction kettle, and glue in reaction kettle is sent into capsule production equipment and is prepared into
To starch capsule shells, it is 45~50 DEG C that starch capsule shells, which are put into, and are put into set temperature in tomato extracting solution after 2~3h of sorptivety
It is dry in vacuum oven, it obtains being retained anti-oxidant starch base capsule.
It takes 40g corn flour to be placed in conical flask, 3g alpha-amylase is added into conical flask and adds the di(2-ethylhexyl)phosphate that pH value is 7
Hydrogen sodium-disodium hydrogen phosphate buffer, constant volume 100mL, then the sodium hypochlorite that 8mL mass fraction is 0.1% is added into conical flask
Conical flask is placed in oscillator by solution, and heating water bath is warming up to 42 DEG C, with the speed oscillation of 135r/min, oscillating reactions 3 days
Afterwards, the sodium hydroxide solution that 10mL mass fraction is 40% is added into conical flask and terminates reaction, obtains starch enzymolysis liquid；It will be upper
It states starch enzymolysis liquid to be placed in baking oven, is heated to 60 DEG C, dry 8h obtains enzymatic hydrolysis corn flour, weighs 20g enzymatic hydrolysis corn flour
It is added in the three-necked flask with thermometer and nitrogen conduit, 100mL distilled water is added into three-necked flask, to three-necked flask
45 DEG C are heated to, 10min is preheated, the calcium chloride solution and digest beautiful that 10mL mass fraction is 0.5% is added to three-necked flask
The acrylic acid of rice flour quality 17% continues to be heated to 55 DEG C, causes 30min, obtain performed polymer product under nitrogen protection；
The sodium hydroxide solution that mass fraction is 25% is added to above-mentioned performed polymer product, neutralizing liquid pH in above-mentioned three-necked flask is
6.5, continue to react 3h by above-mentioned reaction condition, obtains graft product, graft product is put into drying box, be heated to 40
DEG C, dry 4h, the forced air drying 3h under the conditions of 120 DEG C obtain grafting corn flour；Above-mentioned grafting corn flour is placed in have and is stirred
It mixes in the water-bath of device, 40mL distilled water is added into water-bath, be heated to 40 DEG C, start blender, with 90r/min's
Revolving speed stirs 20min, and 20g calcium chloride is added to water-bath, continues to stir 40min, obtains starch base coagulant liquid；Tomato is taken to be put into
In beater, mashing crushes 20min, obtains slurries, and the sodium hydroxide solution for being 30% with mass fraction adjusts slurry pH value and is
7.5, alkalization slurries are obtained, alkalization slurries are placed in a beaker, are heated to 50 DEG C, stir 5h, pyrolysis slurries are obtained, to heat
Solution slurry temperature is down to room temperature, by pyrolysis slurries filtering, removes residue and obtains tomato extracting solution；According to parts by weight, by 20 parts
Mass fraction be 3% soybean protein isolate solution, 100 parts of starch base coagulant liquids pour into reaction kettle, start blender with
The revolving speed of 400r/min stirs 15min, then the sodium alginate soln that 5 parts of mass fractions are 5%, heat temperature raising is added to reaction kettle
To 50 DEG C, whipping process adds gelatin viscosity in water management reaction kettle to be 200mPas, and glue in reaction kettle is sent into capsule manufacture
Starch capsule shells are prepared in equipment, it is 45 that starch capsule shells, which are put into tomato extracting solution after sorptivety 2h, and are put into set temperature
DEG C vacuum oven in it is dry, obtain being retained anti-oxidant starch base capsule.
It takes 45g corn flour to be placed in conical flask, 4g alpha-amylase is added into conical flask and adds the di(2-ethylhexyl)phosphate that pH value is 7
Hydrogen sodium-disodium hydrogen phosphate buffer, constant volume 105mL, then the sodium hypochlorite that 9mL mass fraction is 0.1% is added into conical flask
Conical flask is placed in oscillator by solution, and heating water bath is warming up to 43 DEG C, with the speed oscillation of 137r/min, oscillating reactions 3 days
Afterwards, the sodium hydroxide solution that 11mL mass fraction is 40% is added into conical flask and terminates reaction, obtains starch enzymolysis liquid；It will be upper
It states starch enzymolysis liquid to be placed in baking oven, is heated to 65 DEG C, dry 8h obtains enzymatic hydrolysis corn flour, weighs 23g enzymatic hydrolysis corn flour
It is added in the three-necked flask with thermometer and nitrogen conduit, 105mL distilled water is added into three-necked flask, to three-necked flask
47 DEG C are heated to, 13min is preheated, the calcium chloride solution and digest beautiful that 13mL mass fraction is 0.5% is added to three-necked flask
The acrylic acid of rice flour quality 18% continues to be heated to 57 DEG C, causes 33min, obtain performed polymer product under nitrogen protection；
The sodium hydroxide solution that mass fraction is 25% is added to above-mentioned performed polymer product, neutralizing liquid pH in above-mentioned three-necked flask is
6.7, continue to react 3h by above-mentioned reaction condition, obtains graft product, graft product is put into drying box, be heated to 43
DEG C, dry 4h, the forced air drying 3h under the conditions of 125 DEG C obtain grafting corn flour；Above-mentioned grafting corn flour is placed in have and is stirred
It mixes in the water-bath of device, 45mL distilled water is added into water-bath, be heated to 43 DEG C, start blender, with 95r/min's
Revolving speed stirs 23min, and 23g calcium chloride is added to water-bath, continues to stir 43min, obtains starch base coagulant liquid；Tomato is taken to be put into
In beater, mashing crushes 25min, obtains slurries, and the sodium hydroxide solution for being 30% with mass fraction adjusts slurry pH value and is
8.1, alkalization slurries are obtained, alkalization slurries are placed in a beaker, are heated to 55 DEG C, stir 6h, pyrolysis slurries are obtained, to heat
Solution slurry temperature is down to room temperature, by pyrolysis slurries filtering, removes residue and obtains tomato extracting solution；According to parts by weight, by 23 parts
Mass fraction be 3% soybean protein isolate solution, 110 parts of starch base coagulant liquids pour into reaction kettle, start blender with
The revolving speed of 425r/min stirs 17min, then the sodium alginate soln that 7 parts of mass fractions are 5%, heat temperature raising is added to reaction kettle
To 53 DEG C, whipping process adds gelatin viscosity in water management reaction kettle to be 250mPas, and glue in reaction kettle is sent into capsule manufacture
Starch capsule shells are prepared in equipment, it is 47 that starch capsule shells, which are put into tomato extracting solution after sorptivety 2h, and are put into set temperature
DEG C vacuum oven in it is dry, obtain being retained anti-oxidant starch base capsule.
It takes 50g corn flour to be placed in conical flask, 5g alpha-amylase is added into conical flask and adds the di(2-ethylhexyl)phosphate that pH value is 7
Hydrogen sodium-disodium hydrogen phosphate buffer, constant volume 110mL, then the hypochlorous acid that 10mL mass fraction is 0.1% is added into conical flask
Conical flask is placed in oscillator by sodium solution, and heating water bath is warming up to 45 DEG C, with the speed oscillation of 140r/min, oscillating reactions 4
After it, the sodium hydroxide solution that 12mL mass fraction is 40% is added into conical flask and terminates reaction, obtains starch enzymolysis liquid；It will
Above-mentioned starch enzymolysis liquid is placed in baking oven, is heated to 70 DEG C, and dry 9h obtains enzymatic hydrolysis corn flour, weighs 25g enzymatic hydrolysis corn
Powder is added in the three-necked flask with thermometer and nitrogen conduit, and 110mL distilled water is added into three-necked flask, is burnt to three mouthfuls
Bottle is heated to 50 DEG C, preheats 15min, and the calcium chloride solution and enzymatic hydrolysis that 15mL mass fraction is 0.5% is added to three-necked flask
The acrylic acid of corn flour quality 20% continues to be heated to 60 DEG C, causes 35min under nitrogen protection, obtains performed polymer production
Object；The sodium hydroxide solution that mass fraction is 25% is added to above-mentioned performed polymer product, neutralizing liquid pH in above-mentioned three-necked flask is
7.0, continue to react 4h by above-mentioned reaction condition, obtains graft product, graft product is put into drying box, be heated to 45
DEG C, dry 5h, the forced air drying 4h under the conditions of 130 DEG C obtain grafting corn flour；Above-mentioned grafting corn flour is placed in have and is stirred
It mixes in the water-bath of device, 50mL distilled water is added into water-bath, be heated to 45 DEG C, start blender, with 100r/min
Revolving speed stir 25min, to water-bath be added 25g calcium chloride, continue stir 45min, obtain starch base coagulant liquid；Tomato is taken to put
Enter in beater, mashing crushes 30min, obtains slurries, and the sodium hydroxide solution for being 30% with mass fraction adjusts slurry pH value and is
9.0, alkalization slurries are obtained, alkalization slurries are placed in a beaker, are heated to 60 DEG C, stir 7h, pyrolysis slurries are obtained, to heat
Solution slurry temperature is down to room temperature, by pyrolysis slurries filtering, removes residue and obtains tomato extracting solution；According to parts by weight, by 25 parts
Mass fraction be 3% soybean protein isolate solution, 120 parts of starch base coagulant liquids pour into reaction kettle, start blender with
The revolving speed of 450r/min stirs 20min, then the sodium alginate soln that 10 parts of mass fractions are 5%, heat temperature raising is added to reaction kettle
To 55 DEG C, whipping process adds gelatin viscosity in water management reaction kettle to be 300mPas, and glue in reaction kettle is sent into capsule manufacture
Starch capsule shells are prepared in equipment, it is 50 that starch capsule shells, which are put into tomato extracting solution after sorptivety 3h, and are put into set temperature
DEG C vacuum oven in it is dry, obtain being retained anti-oxidant starch base capsule.
The starch base capsule that comparative example is produced with Guangzhou company is as a comparison case to water conservation antioxygen produced by the present invention
The starch base capsule changed in starch base capsule and comparative example is detected, and testing result is as shown in table 1：
Friability measurement
Starch base capsule each 60 in the anti-oxidant starch base capsule of water conservation produced by the present invention and comparative example are taken respectively, are placed in table
In the ware of face, and be put into the drier for filling saturated solution of magnesium sulfate, set 26 DEG C of ± 2 DEG C of constant temperature for 24 hours, take out, immediately respectively by
Grain, which is put into, stands upright on plank（Thickness 2cm）On glass tube（Internal diameter is 25mm, a length of 2600mm）It is interior, by cylindrical counterweight（Material
Matter is polytetrafluoroethylene (PTFE), diameter 23mm, weight 22g ± 0.2g）It freely falls, whether is ruptured depending on capsule, such as from glass nozzle
There is rupture, must not exceed 5.
Disintegration time mensuration takes 6, every kind of sample respectively, fills talcum powder, and disintegration time limited checks the method for pressing simulate the gastric juice
It checks, each grain all should all be dissolved or be disintegrated in 10 minutes.All it cannot dissolve or be disintegrated if any 1, should separately take 6 to answer
Examination, should all meet regulation.
The measurement reference standard QB/T1913-2004 of transparency, is measured using whiteness instrument, and sample is inherent light reflection
The percentage of the difference of factor and light reflectivity and inherent light reflectivity.
The measurement of pliability is measured using shore hardness meter.
The starch base capsule in the anti-oxidant starch base capsule of water conservation produced by the present invention and comparative example is set in moisture retention measurement
The 6h under normal temperature environment, then tested using moisture teller.
1 performance measurement result of table
From the data in table 1, it can be seen that the anti-oxidant starch base capsule of water conservation produced by the present invention, has good moisture retention and stability,
And the features such as safe and non-toxic, raw material sources are extensive, biodegrade is complete, there is important market value and social value.
Claims (7)
1. a kind of preparation method for being retained anti-oxidant starch base capsule, it is characterised in that specifically preparation step is：
（1）It takes 40~50g corn flour to be placed in conical flask, 3~5g alpha-amylase and sodium dihydrogen phosphate-phosphorus is added into conical flask
Sour disodium hydrogen buffer, constant volume is 100~110mL, then 8~10mL liquor natrii hypochloritis is added into conical flask, by conical flask
It is placed in oscillator, heating water bath heating, oscillating reactions is added 10~12mL sodium hydroxide solution into conical flask and terminates instead
It answers, obtains starch enzymolysis liquid；
（2）Above-mentioned starch enzymolysis liquid is placed in baking oven, heat temperature raising, it is dry, enzymatic hydrolysis corn flour is obtained, 20~25g enzyme is weighed
Solution corn flour is added in the three-necked flask with thermometer and nitrogen conduit, and 100~110mL distillation is added into three-necked flask
Water, to three-necked flask heat temperature raising, 10~15mL calcium chloride solution and acrylic acid is added to three-necked flask in preheating, is protected in nitrogen
Under shield, continue heat temperature raising, initiation reaction obtains performed polymer product；
（3）Sodium hydroxide solution is added to above-mentioned performed polymer product, neutralizes liquid pH in above-mentioned three-necked flask, continues by above-mentioned anti-
Conditioned response is answered, graft product is obtained, graft product is put into drying box, is heated to 40~45 DEG C, dry 4~5h,
3~4h of forced air drying under the conditions of 120~130 DEG C obtains grafting corn flour；
（4）Above-mentioned grafting corn flour is placed in the water-bath with blender, 40~50mL distilled water is added into water-bath,
Heat temperature raising, start blender, stir 20~25min, to water-bath be added 20~25g calcium chloride, continue stirring 40~
45min obtains starch base coagulant liquid；
（5）Tomato is taken to be put into beater, mashing crushes, and obtains slurries, adjusts slurries pH with sodium hydroxide solution, is alkalized
Alkalization slurries are placed in a beaker by slurries, and heat temperature raising stirs 5~7h, obtain pyrolysis slurries, and slurry temperature to be pyrolyzed is down to
Pyrolysis slurries filtering is removed residue and obtains tomato extracting solution by room temperature；
（6）According to parts by weight, 20~25 parts of soybean protein isolate solution, 100~120 parts of starch base coagulant liquids are poured into reaction
In kettle, starts blender with the revolving speed of 400~450r/min and stir 15~20min, then 5~10 parts of alginic acids are added to reaction kettle
Sodium solution, heat temperature raising, whipping process add gelatin viscosity in water management reaction kettle, and glue in reaction kettle is sent into capsule manufacture and is set
Starch capsule shells are prepared in standby, starch capsule shells are put into tomato extracting solution after sorptivety to be put into vacuum oven and are done
It is dry, it obtains being retained anti-oxidant starch base capsule.
2. a kind of preparation method for being retained anti-oxidant starch base capsule according to claim 1, it is characterised in that：Step
（1）The sodium dihydrogen phosphate-disodium hydrogen phosphate pH of cushioning fluid is 7, and the mass fraction of liquor natrii hypochloritis is 0.1%, water-bath
Heat temperature raising temperature is 42~45 DEG C, and oscillation revolving speed is 135~140r/min, and the oscillating reactions time is 3~4 days, sodium hydroxide
The mass fraction of solution is 40%.
3. a kind of preparation method for being retained anti-oxidant starch base capsule according to claim 1, it is characterised in that：Step
（2）The heat temperature raising temperature is 60~70 DEG C, and drying time is 8~9h, and heat temperature raising temperature is 45~50 DEG C, when preheating
Between be 10~15min, the mass fraction of calcium chloride solution is 0.5%, the additional amount of acrylic acid be enzymatic hydrolysis corn flour quality 17~
20%, heat temperature raising temperature is 55~60 DEG C, and the initiation time is 30~35min.
4. a kind of preparation method for being retained anti-oxidant starch base capsule according to claim 1, it is characterised in that：Step
（3）The mass fraction of the sodium hydroxide solution is 25%, and neutralizing liquid pH in three-necked flask is 6.5~7.0, is continued by upper
Stating the reaction condition reaction time is 3~4h.
5. a kind of preparation method for being retained anti-oxidant starch base capsule according to claim 1, it is characterised in that：Step
（4）The heating water bath warming temperature is 40~45 DEG C, and speed of agitator is 90~100r/min.
6. a kind of preparation method for being retained anti-oxidant starch base capsule according to claim 1, it is characterised in that：Step
（5）The mashing grinding time is 20~30min, and the mass fraction of sodium hydroxide solution is 30%, adjusts slurry pH value and is
7.5~9.0, heat temperature raising temperature is 50~60 DEG C.
7. a kind of preparation method for being retained anti-oxidant starch base capsule according to claim 1, it is characterised in that：Step
（6）The mass fraction of the soybean protein isolate solution is 3%, and the mass fraction of sodium alginate soln is 5%, heat temperature raising temperature
Degree is 50~55 DEG C, and controlling gelatin viscosity in reaction kettle is 200~300mPas, and the sorptivety time is 2~3h, vacuum oven
Set temperature temperature be 45~50 DEG C.
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| CN113116853A (en) * | 2021-04-16 | 2021-07-16 | 王光丰 | Antibacterial and anti-pollution medicine capsule shell and preparation method thereof |
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| CN113116853A (en) * | 2021-04-16 | 2021-07-16 | 王光丰 | Antibacterial and anti-pollution medicine capsule shell and preparation method thereof |
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