CN109276554A - A kind of preparation method of high water-retaining type capsule - Google Patents
A kind of preparation method of high water-retaining type capsule Download PDFInfo
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- CN109276554A CN109276554A CN201811135206.XA CN201811135206A CN109276554A CN 109276554 A CN109276554 A CN 109276554A CN 201811135206 A CN201811135206 A CN 201811135206A CN 109276554 A CN109276554 A CN 109276554A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/4816—Wall or shell material
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Abstract
The present invention relates to capsule filmogen preparation technical fields, and in particular to a kind of preparation method of high water-retaining type capsule.Sphagna fiber is made by raw material of sphagna first in the present invention, again it is reacted in the presence of a base with monoxone and etherificate sphagna fiber is made, sphagna fiber will be etherified, potato starch natural plant gum, water, it is put into after sorbierite mixed sols in Capsules manufacturing machine, high water-retaining type capsule is made, sphagna is all-natural product, the water-retaining property of capsule produced by the present invention can be improved in its use, make extended shelf-life, monoxone and sphagna fiber, which carry out reacting in the presence of a base, is made etherificate sphagna fiber, it forms gluing shape liquid after being dissolved in water, potato starch natural plant gum has water retention, sorbierite also has water retention, and it is not volatile polyalcohol, it is good stabilizer, so that manufactured capsule water-retaining property is excellent and has good stability, it has broad application prospects.
Description
Technical field
The present invention relates to capsule filmogen preparation technical fields, and in particular to a kind of preparation side of high water-retaining type capsule
Method.
Background technique
Capsule has very extensive application in medicine, health care product and functional food industry, is present drug and function
One of energy most common dosage form of food.It is with good appearance, conducive to covering content drug odor, insulation blocking, fully absorbing,
Convenient for meeting positioning, delayed release requirement, many advantages, such as preparation process is simple, powder charge is easy to use.
The Capsules that present pharmaceutical factory uses mostly are using animal gelatin as raw material, and animal gelatin is mainly by animal osteoderm
In the gelatine, the hide glue that extract be made.Animal gelatin have the drawback that (1) gelatin molecule easily with formaldehyde, reduced sugar base class
The crosslinking of the drugs such as compound and vitamin C had not only influenced the disintegration of capsule but also had influenced the stability of drug；(2) gelatin quality is by dynamic
Object health status influences, and the edible animal sources gelatin with disease easily propagates pathogeny, causes cross-infection, causes food safety
Hidden danger；(3) its moisture content is higher, hygroscopicity is strong, and easily gives the water transport of absorption to content drug, becomes the drug moisture absorption
Matter causes drug quality unqualified or shortens validity period；(4) animal gelatin source is mostly that the skin of animal and bone pass through fermentation
, and it is added to a large amount of chemical component during the fermentation, serious pollution can be generated to air and water environment.
Starch capsule product is a kind of novel non-gelatin class capsule, has that safe and non-toxic, raw material sources are extensive, can be given birth to
The advantages that object is degraded.But since pure starch and single modified starch have the defects that in performance, such as: viscosity is high, film forming is poor, film
The features such as toughness is strong, poor water retention property, bad mechanical performance makes starch base capsule be difficult to compare favourably with animal gelatin capsule, together
When again be easy the moisture absorption, more demanding to preservation condition, the shelf-life is not grown.So although the patent about starch capsule is more,
The product that industrialized production can be formed is few.
Therefore, needing to develop a kind of capsule for being able to solve the above problem is highly desirable.
Summary of the invention
Present invention mainly solves the technical issues of, have the defects that film forming is poor, poor water retention property for current capsule, provide
A kind of preparation method of high water-retaining type capsule.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
A kind of preparation method of high water-retaining type capsule, it is characterised in that specific preparation step are as follows:
(1) water intaking tongue fur is put into steam-explosion jar, and steam is passed through into steam-explosion jar, until in steam-explosion jar pressure up to 2.2~2.4MPa,
After 30~40s of pressure maintaining, steam-explosion jar discharge valve is opened, is injected into material moment in steam-explosion jar in receiving tank, collected and receive
Material in tank obtains sphagna fiber；
(2) chloroacetic acid solution and isopropanol are obtained into mixed liquor after mixing, by above-mentioned sphagna fiber, mixed liquor and hydroxide
It is fitted into three-necked flask after sodium solution mixing, and is passed through nitrogen until displacing all air, in nitrogen protection into there-necked flask
Under, 30~40 DEG C are heated to, 30~40min is stirred, obtains the reactant containing etherificate sphagna fiber；
(3) pH to 4~5 that the above-mentioned reactant containing etherificate sphagna fiber is adjusted with hydrochloric acid, is filtered after standing 20~30min,
Filter residue is collected, is rinsed filter residue 2~3 times with anhydrous methanol, be removed inorganic salts and the chloroacetic filter residue of unreacted, puts it into
In baking oven, under conditions of temperature is 70~80 DEG C, dry 30~40min collects dried object, as etherificate sphagna fiber；
(4) above-mentioned etherificate sphagna fiber, potato starch natural plant gum, water are poured into glue pot, is 60~80 DEG C in temperature
Under the conditions of, 1~2h of insulated and stirred obtains mixture, then sorbierite is added into mixture, continues under conditions of 60~80 DEG C
Colloidal sol is obtained after 1~2h of heat preservation；
(5) above-mentioned colloidal sol is added in the glue bucket of Capsules manufacturing machine, glue temperature within the barrel is made with the cooling rate of 10 DEG C/min
1~2h is stood after being down to 40~60 DEG C, obtains Capsules, as high water-retaining type capsule.
The temperature of steam described in step (1) is 220~240 DEG C.
The mass ratio of chloroacetic acid solution described in step (2) and isopropanol is 3 ︰ 4, and the mass fraction of chloroacetic acid solution is
40%, the mass ratio of above-mentioned sphagna fiber, mixed liquor and sodium hydroxide solution is 2 ︰, 1 ︰ 1, and the mass fraction of sodium hydroxide solution is
20%。
The mass fraction of hydrochloric acid described in step (3) is 10%.
Above-mentioned etherificate sphagna fiber, potato starch natural plant gum described in step (4), water mass ratio be 1 ︰, 1 ︰ 2, sorb
The quality of alcoholic solution is the 10% of mixture quality.
Glue temperature within the barrel described in step (5) is 90~100 DEG C, 60~90min of constant temperature.
The beneficial effects of the present invention are:
Sphagna fiber is made by raw material of sphagna first in the present invention, then it is reacted under alkaline condition with monoxone, etherificate is made
Sphagna fiber will be put into Capsules manufacture after etherificate sphagna fiber, potato starch natural plant gum, water, sorbierite mixed sols
In machine, Capsules, as high water-retaining type capsule are made, the present invention is made first using sphagna as raw material through high steam explosion
Sphagna fiber, sphagna are all-natural products, and material is clean, without germ, and fiber surface contains great amount of hydroxy group, and hydroxyl has hydrophilic
Property, hydrone can be locked in fiber surface, play the role of shrink, water conservation, therefore its water retention property is good, its use can
The water-retaining property of capsule produced by the present invention is improved, monoxone and sphagna fiber carry out reacting obtained carboxymethyl sphagna in the presence of a base
Fiber, as etherificate sphagna fiber, etherificate sphagna fiber have the effects that film forming, gluing, water conservation, colloid protection, film forming
It is good, gluing shape liquid is formed after being dissolved in water, potato starch natural plant gum has water retention, and sorbierite is as adhesive, simultaneously
Also there is water retention, and it is not volatile polyalcohol, is good stabilizer, so that manufactured capsule water-retaining property is excellent
It is different and have good stability, it has broad application prospects.
Specific embodiment
Water intaking tongue fur is put into steam-explosion jar, and is passed through into steam-explosion jar and is preheated to 220~240 DEG C of steam, until steam-explosion jar
Middle pressure is up to 2.2~2.4MPa, after 30~40s of pressure maintaining, opens steam-explosion jar discharge valve, is injected into material moment in steam-explosion jar
Enter in receiving tank, collects material in receiving tank, obtain sphagna fiber；Mass fraction is pressed for 40% chloroacetic acid solution with isopropanol
Mass ratio is that 3 ︰ 4 obtain mixed liquor after mixing, the hydroxide for being 20% by above-mentioned sphagna fiber, mixed liquor and mass fraction
Sodium solution is to be fitted into three-necked flask after 2 ︰, 1 ︰ 1 is mixed, and be passed through nitrogen until displacing all into there-necked flask in mass ratio
Air is heated to 30~40 DEG C under nitrogen protection, stirs 30~40min, obtains the reaction containing etherificate sphagna fiber
Object；With mass fraction be 10% hydrochloric acid adjust it is above-mentioned containing etherificate sphagna fiber reactant pH to 4~5, stand 20~
Filtered after 30min, collect filter residue, with anhydrous methanol rinse filter residue 2~3 times, be removed inorganic salts and unreacted it is chloroacetic
Filter residue is put it into baking oven, and under conditions of temperature is 70~80 DEG C, dry 30~40min collects dried object, as ether
Change sphagna fiber；It is in mass ratio that 1 ︰, 1 ︰ 2 is poured into glue pot by above-mentioned etherificate sphagna fiber, potato starch natural plant gum, water,
Under conditions of temperature is 60~80 DEG C, 1~2h of insulated and stirred obtains mixture, then mixture quality is added into mixture
10% sorbierite continues to obtain colloidal sol after keeping the temperature 1~2h under conditions of 60~80 DEG C；Capsules are added in above-mentioned colloidal sol
In the glue bucket of manufacturing machine, setting glue temperature within the barrel is 90~100 DEG C, after 60~90min of constant temperature, with the cooling rate of 10 DEG C/min
1~2h is stood after so that glue temperature within the barrel is down to 40~60 DEG C, obtains Capsules, as high water-retaining type capsule.
Example 1
Water intaking tongue fur is put into steam-explosion jar, and is passed through into steam-explosion jar and is preheated to 220 DEG C of steam, until pressure reaches in steam-explosion jar
After 2.2MPa, pressure maintaining 30s, steam-explosion jar discharge valve is opened, is injected into material moment in steam-explosion jar in receiving tank, collection connects
Material in closed cans obtains sphagna fiber；It is 40% chloroacetic acid solution by mass fraction with isopropanol is in mass ratio that 3 ︰ 4 are mixed
Mixed liquor is obtained after even, is in mass ratio 2 ︰ by the sodium hydroxide solution that above-mentioned sphagna fiber, mixed liquor and mass fraction are 20%
Is fitted into three-necked flask after 1 ︰ 1 mixing, and is passed through into there-necked flask nitrogen up to displacing all air, under nitrogen protection,
30 DEG C are heated to, 30min is stirred, obtains the reactant containing etherificate sphagna fiber；The hydrochloric acid tune for being 10% with mass fraction
The pH to 4 for saving the above-mentioned reactant containing etherificate sphagna fiber, filters after standing 20min, collects filter residue, rinsed with anhydrous methanol
Filter residue 2 times, be removed inorganic salts and the chloroacetic filter residue of unreacted, puts it into baking oven, the condition for being 70 DEG C in temperature
Under, dry 30min collects dried object, as etherificate sphagna fiber；By above-mentioned etherificate sphagna fiber, potato starch natural plant gum,
Water is that 1 ︰, 1 ︰ 2 is poured into glue pot in mass ratio, and under conditions of temperature is 60 DEG C, insulated and stirred 1h obtains mixture, then to
The sorbierite of mixture quality 10% is added in mixture, continues to obtain colloidal sol after keeping the temperature 1h under conditions of 60 DEG C；It will be above-mentioned molten
Glue is added in the glue bucket of Capsules manufacturing machine, and setting glue temperature within the barrel is 90 DEG C, after constant temperature 60min, with the drop of 10 DEG C/min
Warm speed stands 1h after so that glue temperature within the barrel is down to 40 DEG C, obtains Capsules, as high water-retaining type capsule.
Example 2
Water intaking tongue fur is put into steam-explosion jar, and is passed through into steam-explosion jar and is preheated to 230 DEG C of steam, until pressure reaches in steam-explosion jar
After 2.3MPa, pressure maintaining 35s, steam-explosion jar discharge valve is opened, is injected into material moment in steam-explosion jar in receiving tank, collection connects
Material in closed cans obtains sphagna fiber；It is 40% chloroacetic acid solution by mass fraction with isopropanol is in mass ratio that 3 ︰ 4 are mixed
Mixed liquor is obtained after even, is in mass ratio 2 ︰ by the sodium hydroxide solution that above-mentioned sphagna fiber, mixed liquor and mass fraction are 20%
Is fitted into three-necked flask after 1 ︰ 1 mixing, and is passed through into there-necked flask nitrogen up to displacing all air, under nitrogen protection,
35 DEG C are heated to, 35min is stirred, obtains the reactant containing etherificate sphagna fiber；The hydrochloric acid tune for being 10% with mass fraction
The pH to 4 for saving the above-mentioned reactant containing etherificate sphagna fiber, filters after standing 25min, collects filter residue, rinsed with anhydrous methanol
Filter residue 2 times, be removed inorganic salts and the chloroacetic filter residue of unreacted, puts it into baking oven, the condition for being 75 DEG C in temperature
Under, dry 35min collects dried object, as etherificate sphagna fiber；By above-mentioned etherificate sphagna fiber, potato starch natural plant gum,
Water is that 1 ︰, 1 ︰ 2 is poured into glue pot in mass ratio, and under conditions of temperature is 70 DEG C, insulated and stirred 1h obtains mixture, then to
The sorbierite of mixture quality 10% is added in mixture, continues to obtain colloidal sol after keeping the temperature 1h under conditions of 70 DEG C；It will be above-mentioned molten
Glue is added in the glue bucket of Capsules manufacturing machine, and setting glue temperature within the barrel is 95 DEG C, after constant temperature 70min, with the drop of 10 DEG C/min
Warm speed stands 1h after so that glue temperature within the barrel is down to 50 DEG C, obtains Capsules, as high water-retaining type capsule.
Example 3
Water intaking tongue fur is put into steam-explosion jar, and is passed through into steam-explosion jar and is preheated to 240 DEG C of steam, until pressure reaches in steam-explosion jar
After 2.4MPa, pressure maintaining 40s, steam-explosion jar discharge valve is opened, is injected into material moment in steam-explosion jar in receiving tank, collection connects
Material in closed cans obtains sphagna fiber；It is 40% chloroacetic acid solution by mass fraction with isopropanol is in mass ratio that 3 ︰ 4 are mixed
Mixed liquor is obtained after even, is in mass ratio 2 ︰ by the sodium hydroxide solution that above-mentioned sphagna fiber, mixed liquor and mass fraction are 20%
Is fitted into three-necked flask after 1 ︰ 1 mixing, and is passed through into there-necked flask nitrogen up to displacing all air, under nitrogen protection,
40 DEG C are heated to, 40min is stirred, obtains the reactant containing etherificate sphagna fiber；The hydrochloric acid tune for being 10% with mass fraction
The pH to 5 for saving the above-mentioned reactant containing etherificate sphagna fiber, filters after standing 30min, collects filter residue, rinsed with anhydrous methanol
Filter residue 3 times, be removed inorganic salts and the chloroacetic filter residue of unreacted, puts it into baking oven, the condition for being 80 DEG C in temperature
Under, dry 40min collects dried object, as etherificate sphagna fiber；By above-mentioned etherificate sphagna fiber, potato starch natural plant gum,
Water is that 1 ︰, 1 ︰ 2 is poured into glue pot in mass ratio, and under conditions of temperature is 80 DEG C, insulated and stirred 2h obtains mixture, then to
The sorbierite of mixture quality 10% is added in mixture, continues to obtain colloidal sol after keeping the temperature 2h under conditions of 80 DEG C；It will be above-mentioned molten
Glue is added in the glue bucket of Capsules manufacturing machine, and setting glue temperature within the barrel is 100 DEG C, after constant temperature 90min, with the drop of 10 DEG C/min
Warm speed stands 2h after so that glue temperature within the barrel is down to 60 DEG C, obtains Capsules, as high water-retaining type capsule.
Comparative example
With the capsule of Shanghai City company production as a comparison case in high water-retaining type capsule produced by the present invention and comparative example
Capsule is detected, and testing result is as shown in table 1:
Friability measurement
Capsule each 60 in high water-retaining type capsule produced by the present invention and comparative example are taken respectively, are placed in surface plate, and be put into
It fills in the drier of saturated solution of magnesium sulfate, sets 26 DEG C of ± 2 DEG C of constant temperature for 24 hours, take out, be put into respectively by grain stand upright on wood immediately
In glass tube (internal diameter 25mm, a length of 2600mm) on plate (thickness 2cm), by cylindrical counterweight (material is polytetrafluoroethylene (PTFE),
Diameter is 23mm, again 22g ± 0.2g) it is freely fallen from glass nozzle, whether ruptured depending on capsule, if any rupture, must not exceed 5
Grain.
Disintegration time mensuration
6, every kind of sample are taken respectively, fills talcum powder, and disintegration time limited checks the method inspection for pressing simulate the gastric juice, and each grain should all be
It all dissolves or is disintegrated in 10 minutes.All it cannot dissolve or be disintegrated if any 1, should separately take 6 retrials, regulation should all be met.
Water-retaining property test
Each 20g of capsule in high water-retaining type capsule produced by the present invention and comparative example is weighed, absorbs water to saturation to it, quality is denoted as
M1.Constant temperature forced air drying in electric heating constant-temperature blowing drying box (30 DEG C) are placed it in, claim mass M when time interval is 96h2.Together
When, record the time that each capsule reaches permanent quality.
According to formula rate-of-loss of coolant=(M1-M2)/M1×100%。
1 performance measurement result of table
From the data in table 1, it can be seen that high water-retaining type capsule produced by the present invention, has good film-forming property, high mechanical strength, water retention property good
Good, can be with long-time storage the features such as, and it is safe and non-toxic, raw material sources are extensive, there is important market value and social value.
Claims (6)
1. a kind of preparation method of high water-retaining type capsule, it is characterised in that specific preparation step are as follows:
(1) water intaking tongue fur is put into steam-explosion jar, and steam is passed through into steam-explosion jar, until in steam-explosion jar pressure up to 2.2~2.4MPa,
After 30~40s of pressure maintaining, steam-explosion jar discharge valve is opened, is injected into material moment in steam-explosion jar in receiving tank, collected and receive
Material in tank obtains sphagna fiber；
(2) chloroacetic acid solution and isopropanol are obtained into mixed liquor after mixing, by above-mentioned sphagna fiber, mixed liquor and hydroxide
It is fitted into three-necked flask after sodium solution mixing, and is passed through nitrogen until displacing all air, in nitrogen protection into there-necked flask
Under, 30~40 DEG C are heated to, 30~40min is stirred, obtains the reactant containing etherificate sphagna fiber；
(3) pH to 4~5 that the above-mentioned reactant containing etherificate sphagna fiber is adjusted with hydrochloric acid, is filtered after standing 20~30min,
Filter residue is collected, is rinsed filter residue 2~3 times with anhydrous methanol, be removed inorganic salts and the chloroacetic filter residue of unreacted, puts it into
In baking oven, under conditions of temperature is 70~80 DEG C, dry 30~40min collects dried object, as etherificate sphagna fiber；
(4) above-mentioned etherificate sphagna fiber, potato starch natural plant gum, water are poured into glue pot, is 60~80 DEG C in temperature
Under the conditions of, 1~2h of insulated and stirred obtains mixture, then sorbierite is added into mixture, continues under conditions of 60~80 DEG C
Colloidal sol is obtained after 1~2h of heat preservation；
(5) above-mentioned colloidal sol is added in the glue bucket of Capsules manufacturing machine, glue temperature within the barrel is made with the cooling rate of 10 DEG C/min
1~2h is stood after being down to 40~60 DEG C, obtains Capsules, as high water-retaining type capsule.
2. a kind of preparation method of high water-retaining type capsule according to claim 1, it is characterised in that: described in step (1)
The temperature of steam is 220~240 DEG C.
3. a kind of preparation method of high water-retaining type capsule according to claim 1, it is characterised in that: described in step (2)
The mass ratio of chloroacetic acid solution and isopropanol is 3 ︰ 4, and the mass fraction of chloroacetic acid solution is 40%, above-mentioned sphagna fiber, mixed liquor
Mass ratio with sodium hydroxide solution is 2 ︰, 1 ︰ 1, and the mass fraction of sodium hydroxide solution is 20%.
4. a kind of preparation method of high water-retaining type capsule according to claim 1, it is characterised in that: described in step (3)
The mass fraction of hydrochloric acid is 10%.
5. a kind of preparation method of high water-retaining type capsule according to claim 1, it is characterised in that: described in step (4)
Above-mentioned etherificate sphagna fiber, potato starch natural plant gum, water mass ratio be 1 ︰, 1 ︰ 2, the quality of sorbitol solution is mixture
The 10% of quality.
6. a kind of preparation method of high water-retaining type capsule according to claim 1, it is characterised in that: described in step (5)
Glue temperature within the barrel is 90~100 DEG C, 60~90min of constant temperature.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811135206.XA CN109276554A (en) | 2018-09-28 | 2018-09-28 | A kind of preparation method of high water-retaining type capsule |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811135206.XA CN109276554A (en) | 2018-09-28 | 2018-09-28 | A kind of preparation method of high water-retaining type capsule |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109939240A (en) * | 2019-03-28 | 2019-06-28 | 亳州职业技术学院 | A kind of production technology of ionising radiation processing Chinese drugs powder |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4697008A (en) * | 1985-12-13 | 1987-09-29 | Dai-Ichi Kogyo Seiyaku Co., Ltd. | Production of water-insoluble alkali metal salts of carboxyalkyl cellulose |
| CN101463091A (en) * | 2009-01-16 | 2009-06-24 | 中国科学院过程工程研究所 | Method for separating stalk carboxymethylation components and preparing stalk carboxymethyl cellulose |
| CN107184562A (en) * | 2017-05-10 | 2017-09-22 | 中象新材料（大连）有限公司 | A kind of corn bran starch hollow capsule and preparation method thereof |
-
2018
- 2018-09-28 CN CN201811135206.XA patent/CN109276554A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4697008A (en) * | 1985-12-13 | 1987-09-29 | Dai-Ichi Kogyo Seiyaku Co., Ltd. | Production of water-insoluble alkali metal salts of carboxyalkyl cellulose |
| CN101463091A (en) * | 2009-01-16 | 2009-06-24 | 中国科学院过程工程研究所 | Method for separating stalk carboxymethylation components and preparing stalk carboxymethyl cellulose |
| CN107184562A (en) * | 2017-05-10 | 2017-09-22 | 中象新材料（大连）有限公司 | A kind of corn bran starch hollow capsule and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109939240A (en) * | 2019-03-28 | 2019-06-28 | 亳州职业技术学院 | A kind of production technology of ionising radiation processing Chinese drugs powder |
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