CN106074432A - A kind of cactus polyoses is combined the method that curdlan prepares Capsules - Google Patents

A kind of cactus polyoses is combined the method that curdlan prepares Capsules Download PDF

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CN106074432A
CN106074432A CN201610468622.6A CN201610468622A CN106074432A CN 106074432 A CN106074432 A CN 106074432A CN 201610468622 A CN201610468622 A CN 201610468622A CN 106074432 A CN106074432 A CN 106074432A
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curdlan
capsules
solution
glue
radix
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张静
盛海丰
王统军
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/48Preparations in capsules, e.g. of gelatin, of chocolate
    • A61K9/4841Filling excipients; Inactive ingredients
    • A61K9/4866Organic macromolecular compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/0003General processes for their isolation or fractionation, e.g. purification or extraction from biomass

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Abstract

The invention discloses a kind of cactus polyoses and be combined the method that curdlan prepares Capsules, belong to Capsules preparing technical field.The present invention takes after Radix et Caulis Opuntiae Dillenii smashs homogenate to pieces, add ethanol solution and carry out microwave digestion, obtain extracting solution and carry out enzymolysis, after enzymolysis, dialysis concentrates and precipitate with ethanol obtains cactus polyoses, taking curdlan and cold water mix again, stirring in water bath prepares curdlan solution, after curdlan solution and cactus polyoses being mixed, add after the mixing such as Polyethylene Glycol, glacial acetic acid, water to obtain Capsules glue, pour into molding in glue groove, be dried, method that cutting, fit obtain Capsules.Preparation process of the present invention is simple, makes full use of cactus polyoses and is combined curdlan and prepares Capsules, with strong points, Capsules can be efficiently solved longer for disintegration, easily becoming fragile during low temperature, after 30 DEG C of temperatures above store, physicochemical property is deteriorated, the low problem of bioavailability.

Description

A kind of cactus polyoses is combined the method that curdlan prepares Capsules
Technical field
The present invention relates to a kind of cactus polyoses and be combined the method that curdlan prepares Capsules, belong to Capsules system Standby technical field.
Background technology
Capsules is added, by pharmagel, the cap that adjuvant refines, body two saves capsule shells and forms.It is mainly used in containing admittedly Body medicine.As made powder, health product, medicament etc. by oneself, solve difficult entrance, the problem of mouthfeel difference for user, be truly realized Good medicine is the most bitter to the taste.Capsules is becoming increasingly popular, first the elongate form of capsule, it is easy to swallow, and is the most joyous by consumer The dosage form met;Additionally, uncomfortable taste and the abnormal smells from the patient of content can very effectively be covered by capsule.China is medicinal at present In Capsules, the biggest number is animal gelatin empty hard capsule.Owing to the raw material sources of gelatin are complicated, quality difficulty control, this determines it There is many performances being difficult to overcome and the defect of secure context, mainly gelatin hollow capsule easily crosslink reaction and affect medicine The release of thing.Plant capsule refers to the capsule made with terrestrial or sea-plant through processing, refinement, chemical improvement.With at present A large amount of animal gelatin Capsuleses used are compared, and the significant advantage of plant hollow capsule is stable chemical nature, anti-without crosslinking Should, wide adaptability;Safety is high, because plant hollow capsule is without the proteotoxin of animal gelatin, without any preservative, nothing Need the advantages such as ethylene oxide sterilizing, but the disintegration of this kind of capsule is longer, and during low temperature, capsule easily becomes fragile, more than 30 DEG C temperature After degree stores, physicochemical property is deteriorated, and bioavailability is low.
Summary of the invention
The technical problem to be solved: longer for disintegration for current Capsules, during low temperature, capsule is variable Crisp, after 30 DEG C of temperatures above store, physicochemical property is deteriorated, the drawback that bioavailability is low, it is provided that one takes Radix et Caulis Opuntiae Dillenii and smashs to pieces even After slurry, adding ethanol solution and carry out microwave digestion, obtain extracting solution and carry out enzymolysis, it is many that concentration also precipitate with ethanol of dialysing after enzymolysis obtains Radix et Caulis Opuntiae Dillenii Sugar, then to take curdlan with temperature be that 2 DEG C of water mix, stirring in water bath prepares curdlan solution, by curdlan solution and celestial being After people slaps polysaccharide mixing, after adding the mixing such as Polyethylene Glycol, glacial acetic acid, water, obtain Capsules glue, pour molding in glue groove into, do Dry, cutting, the fit method that obtains Capsules.Preparation process of the present invention is simple, makes full use of that cactus polyoses is compound can be obtained so Capsules prepared by glue, with strong points, can efficiently solve Capsules longer for disintegration, easily become fragile during low temperature, 30 DEG C with After upper temperature storage, physicochemical property is deteriorated, the low problem of bioavailability.
For solving above-mentioned technical problem, the present invention uses the technical scheme as described below to be:
(1) weigh 100~200g Radix et Caulis Opuntiae Dilleniis, put it into underhand polish in stone mortar and smash to pieces, then with homogenizer stirring homogenate 50~ 60min, pours in microwave oscillation instrument, and in Radix et Caulis Opuntiae Dillenii is homogenized, 1:5 in mass ratio adds mass fraction 90% ethanol, 150~ Under 250W, microwave pretreatment 30~40min, filter to get filtrate, and filtrate is spray-dried to obtain Radix et Caulis Opuntiae Dillenii powder;
(2) above-mentioned Radix et Caulis Opuntiae Dillenii powder is put in pottery enzymatic vessel, be added thereto to pottery enzymatic vessel volume 1/3 deionization simultaneously Water mixes, and adds mixed liquor gross mass 3~5% compound enzyme, enzymolysis 1~2h at 30~40 DEG C, and goes out at 100~105 DEG C Ferment treatment 10~15min, then centrifugation 10~15min, obtain supernatant;Described compound enzyme by cellulase, pectase and Protease prepares for 1:1:2 is compounding in mass ratio;
(3) above-mentioned supernatant is put in bag filter, dialyse 2~4 days at 4 DEG C, dialysis solution is evaporated to original volume 15 ~20%, in concentrated solution, add its volume 3~5 times of mass fraction 90% ethanol solution, centrifugation after standing 30~40min, Precipitate lyophilization, cactus polyoses, standby;
(4) weigh 20~30g curdlans, be that 2 DEG C of water mix, with 800~1000r/min by it by solid-to-liquid ratio 1:4 and temperature Rotating speed dispersed with stirring 40~50min, obtains curdlan dispersion liquid, is loaded in flask by dispersion liquid, and moves in water-bath, 70~ At 80 DEG C stirring mixing 1~2h, curdlan solution;
(5) being added in the cactus polyoses that step (3) is standby by above-mentioned curdlan solution 1:1 by volume, addition limit, limit exists Stirring mixing 2~4h under 1000~1200r/min rotating speeds so that it is be thoroughly mixed uniformly, obtain curdlan blend solution;
(6) count by weight, choose 100~120 parts of above-mentioned curdlan blend solutions respectively, 10~20 parts of Polyethylene Glycol, 3 ~5 parts of glacial acetic acid, 1~3 part of sodium lauryl sulphate, 60~80 parts of water, first can so glue blend solution, Polyethylene Glycol, 12 Alkyl sodium sulfate and glacial acetic acid add in reactor, and temperature of reactor is increased to 80~90 DEG C, after stirring mixing 5~10min, In reactor, add water, continue stirring mixing 50~70min, after mixing, be cooled to 50~60 DEG C, be incubated 2~3h, To Capsules glue;
(7) pouring in hollow capsule production line glue groove by above-mentioned Capsules glue, controlling film thickness is 0.08~0.10mm, mould Tool temperature be-30~-5 DEG C, carries out dipping in glue, takes out, put in air dry oven after cooling molding, dry at 30~35 DEG C 100~120min, obtain compound blank, then cut, fit, i.e. can get Capsules.
The application process of the present invention: the Capsules present invention prepared is used for containing solid drugs, can be effectively isolated medicine Taste, this Capsules shortens 3~5min disintegration, capsule good toughness at 0~5 DEG C, physics and chemistry after storing at 30~45 DEG C Performance is unchanged, and bioavailability is high, and wide adaptability is worthy to be popularized and uses.
The present invention is compared with additive method, and Advantageous Effects is:
(1) preparation process of the present invention is simple, makes full use of cactus polyoses and is combined curdlan and prepares Capsules, specific aim By force;
(2) products obtained therefrom shortens 3~5min disintegration, capsule good toughness at 0~5 DEG C, manages after storing at 30~45 DEG C Changing performance unchanged, bioavailability is high.
Detailed description of the invention
First weigh 100~200g Radix et Caulis Opuntiae Dilleniis, put it into underhand polish in stone mortar and smash to pieces, then be homogenized with homogenizer stirring 50~60min, pour in microwave oscillation instrument, in Radix et Caulis Opuntiae Dillenii is homogenized, 1:5 in mass ratio adds mass fraction 90% ethanol, 150 ~microwave pretreatment 30~40min under 250W, filter to get filtrate, filtrate is spray-dried to obtain Radix et Caulis Opuntiae Dillenii powder;Then by above-mentioned Radix et Caulis Opuntiae Dillenii powder is put in pottery enzymatic vessel, is added thereto to pottery enzymatic vessel volume 1/3 deionized water mixing simultaneously, and adds Mixed liquor gross mass 3~5% compound enzyme, enzymolysis 1~2h at 30~40 DEG C, and at 100~105 DEG C enzyme denaturing process 10~ 15min, then centrifugation 10~15min, obtain supernatant;Described compound enzyme is pressed matter by cellulase, pectase and protease Amount prepares than for 1:1:2 is compounding;Above-mentioned supernatant is put in bag filter, dialyses 2~4 days at 4 DEG C, dialysis solution is reduced pressure dense It is reduced to original volume 15~20%, in concentrated solution, adds its volume 3~5 times of mass fraction 90% ethanol solution, stand 30~40min Rear centrifugation, obtains precipitate lyophilization, cactus polyoses, standby;Weigh 20~30g curdlans, pressed Solid-to-liquid ratio 1:4 is that 2 DEG C of water mix with temperature, with 800~1000r/min rotating speed dispersed with stirring 40~50min, obtains curdlan and divides Dissipate liquid, dispersion liquid is loaded in flask, and moves in water-bath, at 70~80 DEG C stirring mixing 1~2h, curdlan Solution;Above-mentioned curdlan solution 1:1 by volume is added in standby cactus polyoses, addition limit, limit 1000~ Stirring mixing 2~4h under 1200r/min rotating speed so that it is be thoroughly mixed uniformly, obtain curdlan blend solution;The most by weight Number meter, chooses 100~120 parts of above-mentioned curdlan blend solutions respectively, 10~20 parts of Polyethylene Glycol, 3~5 parts of glacial acetic acid, and 1 ~3 parts of sodium lauryl sulphates, 60~80 parts of water, first can so glue blend solution, Polyethylene Glycol, sodium lauryl sulphate and ice Acetic acid adds in reactor, and temperature of reactor is increased to 80~90 DEG C, after stirring mixing 5~10min, adds in reactor Water, continues stirring mixing 50~70min, is cooled to 50~60 DEG C after mixing, be incubated 2~3h, i.e. can get Capsules glue; Finally pouring in hollow capsule production line glue groove by above-mentioned Capsules glue, controlling film thickness is 0.08~0.10mm, mould Temperature is-30~-5 DEG C, carries out dipping in glue, takes out, put in air dry oven after cooling molding, is dried 100 at 30~35 DEG C ~120min, obtain compound blank, then cut, fit, i.e. can get Capsules.
Example 1
First weigh 100g Radix et Caulis Opuntiae Dillenii, put it into underhand polish in stone mortar and smash to pieces, then with homogenizer stirring homogenate 50min, fall Entering in microwave shaker, in Radix et Caulis Opuntiae Dillenii is homogenized, 1:5 in mass ratio adds mass fraction 90% ethanol, and under 150W, microwave is located in advance Reason 30min, filters to get filtrate, filtrate is spray-dried to obtain Radix et Caulis Opuntiae Dillenii powder;Then above-mentioned Radix et Caulis Opuntiae Dillenii powder is put into pottery enzyme Solve in tank, be added thereto to pottery enzymatic vessel volume 1/3 deionized water mixing simultaneously, and it is compound to add mixed liquor gross mass 3% Enzyme, enzymolysis 1h at 30 DEG C, and at 100 DEG C, enzyme denaturing processes 10min, then centrifugation 10min, obtains supernatant;Described answers Synthase is prepared for 1:1:2 is compounding in mass ratio by cellulase, pectase and protease;Above-mentioned supernatant is put into bag filter In, dialyse 2 days at 4 DEG C, dialysis solution is evaporated to original volume 15%, in concentrated solution, adds 3 times of mass fractions of its volume 90% ethanol solution, stands centrifugation after 30min, obtains precipitate lyophilization, cactus polyoses, standby;Weigh 20g curdlan, is that 2 DEG C of water mix by it by solid-to-liquid ratio 1:4 and temperature, with 800r/min rotating speed dispersed with stirring 40min, can Right glue dispersion liquid, dispersion liquid is loaded in flask, and moves in water-bath, at 70 DEG C stirring mixing 1h, can obtain so Sol solution;Being added in standby cactus polyoses by above-mentioned curdlan solution 1:1 by volume, addition limit, limit is at 1000r/ Stirring mixing 2h under min rotating speed so that it is be thoroughly mixed uniformly, obtain curdlan blend solution;Count the most by weight, point Do not choose 100 parts of above-mentioned curdlan blend solutions, 10 parts of Polyethylene Glycol, 3 parts of glacial acetic acid, 1 part of sodium lauryl sulphate, 60 parts Water, first can so glue blend solution, Polyethylene Glycol, sodium lauryl sulphate and glacial acetic acid add in reactor, by reactor temperature Degree is increased to 80 DEG C, after stirring mixing 5min, adds water in reactor, continues stirring mixing 50min, is cooled to 50 after mixing DEG C, it is incubated 2h, i.e. can get Capsules glue;Finally pour above-mentioned Capsules glue into hollow capsule production line glue groove In, control film thickness is 0.08mm, and mold temperature is-30 DEG C, carries out dipping in glue, takes out, put into air dry oven after cooling molding In, at 30 DEG C, be dried 100min, obtain compound blank, then cut, fit, i.e. can get Capsules.
The Capsules present invention prepared is used for containing solid drugs, can be effectively isolated flavour of a drug, this Capsules disintegrate Time limit shortens 3min, capsule good toughness at 0 DEG C, and after storing at 30 DEG C, physicochemical property is unchanged, and bioavailability is high, adapts to Property wide, be worthy to be popularized and use.
Example 2
First weigh 150g Radix et Caulis Opuntiae Dillenii, put it into underhand polish in stone mortar and smash to pieces, then with homogenizer stirring homogenate 55min, fall Entering in microwave shaker, in Radix et Caulis Opuntiae Dillenii is homogenized, 1:5 in mass ratio adds mass fraction 90% ethanol, and under 200W, microwave is located in advance Reason 35min, filters to get filtrate, filtrate is spray-dried to obtain Radix et Caulis Opuntiae Dillenii powder;Then above-mentioned Radix et Caulis Opuntiae Dillenii powder is put into pottery enzyme Solve in tank, be added thereto to pottery enzymatic vessel volume 1/3 deionized water mixing simultaneously, and it is compound to add mixed liquor gross mass 4% Enzyme, enzymolysis 2h at 35 DEG C, and at 103 DEG C, enzyme denaturing processes 13min, then centrifugation 13min, obtains supernatant;Described answers Synthase is prepared for 1:1:2 is compounding in mass ratio by cellulase, pectase and protease;Above-mentioned supernatant is put into bag filter In, dialyse 3 days at 4 DEG C, dialysis solution is evaporated to original volume 18%, in concentrated solution, adds 4 times of mass fractions of its volume 90% ethanol solution, stands centrifugation after 35min, obtains precipitate lyophilization, cactus polyoses, standby;Weigh 25g curdlan, is that 2 DEG C of water mix by it by solid-to-liquid ratio 1:4 and temperature, with 900r/min rotating speed dispersed with stirring 45min, can Right glue dispersion liquid, dispersion liquid is loaded in flask, and moves in water-bath, at 75 DEG C stirring mixing 2h, can obtain so Sol solution;Being added in standby cactus polyoses by above-mentioned curdlan solution 1:1 by volume, addition limit, limit is at 1100r/ Stirring mixing 3h under min rotating speed so that it is be thoroughly mixed uniformly, obtain curdlan blend solution;Count the most by weight, point Do not choose 110 parts of above-mentioned curdlan blend solutions, 15 parts of Polyethylene Glycol, 4 parts of glacial acetic acid, 2 parts of sodium lauryl sulphates, 70 parts Water, first can so glue blend solution, Polyethylene Glycol, sodium lauryl sulphate and glacial acetic acid add in reactor, by reactor temperature Degree is increased to 85 DEG C, after stirring mixing 8min, adds water in reactor, continues stirring mixing 60min, is cooled to 55 after mixing DEG C, it is incubated 3h, i.e. can get Capsules glue;Finally pour above-mentioned Capsules glue into hollow capsule production line glue groove In, control film thickness is 0.09mm, and mold temperature is-18 DEG C, carries out dipping in glue, takes out, put into air dry oven after cooling molding In, at 33 DEG C, be dried 110min, obtain compound blank, then cut, fit, i.e. can get Capsules.
The Capsules present invention prepared is used for containing solid drugs, can be effectively isolated flavour of a drug, this Capsules disintegrate Time limit shortens 4min, capsule good toughness at 3 DEG C, and after storing at 38 DEG C, physicochemical property is unchanged, and bioavailability is high, adapts to Property wide, be worthy to be popularized and use.
Example 3
First weigh 200g Radix et Caulis Opuntiae Dillenii, put it into underhand polish in stone mortar and smash to pieces, then with homogenizer stirring homogenate 60min, fall Entering in microwave shaker, in Radix et Caulis Opuntiae Dillenii is homogenized, 1:5 in mass ratio adds mass fraction 90% ethanol, and under 250W, microwave is located in advance Reason 40min, filters to get filtrate, filtrate is spray-dried to obtain Radix et Caulis Opuntiae Dillenii powder;Then above-mentioned Radix et Caulis Opuntiae Dillenii powder is put into pottery enzyme Solve in tank, be added thereto to pottery enzymatic vessel volume 1/3 deionized water mixing simultaneously, and it is compound to add mixed liquor gross mass 5% Enzyme, enzymolysis 2h at 40 DEG C, and at 105 DEG C, enzyme denaturing processes 15min, then centrifugation 15min, obtains supernatant;Described answers Synthase is prepared for 1:1:2 is compounding in mass ratio by cellulase, pectase and protease;Above-mentioned supernatant is put into bag filter In, dialyse 4 days at 4 DEG C, dialysis solution is evaporated to original volume 20%, in concentrated solution, adds 5 times of mass fractions of its volume 90% ethanol solution, stands centrifugation after 40min, obtains precipitate lyophilization, cactus polyoses, standby;Weigh 30g curdlan, is that 2 DEG C of water mix by it by solid-to-liquid ratio 1:4 and temperature, with 1000r/min rotating speed dispersed with stirring 50min, Curdlan dispersion liquid, loads dispersion liquid in flask, and moves in water-bath, and at 80 DEG C, stirring mixing 2h, gets final product get Ke get So sol solution;Being added in standby cactus polyoses by above-mentioned curdlan solution 1:1 by volume, addition limit, limit is at 1200r/ Stirring mixing 4h under min rotating speed so that it is be thoroughly mixed uniformly, obtain curdlan blend solution;Count the most by weight, point Do not choose 120 parts of above-mentioned curdlan blend solutions, 20 parts of Polyethylene Glycol, 5 parts of glacial acetic acid, 3 parts of sodium lauryl sulphates, 80 parts Water, first can so glue blend solution, Polyethylene Glycol, sodium lauryl sulphate and glacial acetic acid add in reactor, by reactor temperature Degree is increased to 90 DEG C, after stirring mixing 10min, adds water in reactor, continues stirring mixing 70min, is cooled to after mixing 60 DEG C, it is incubated 3h, i.e. can get Capsules glue;Finally pour above-mentioned Capsules glue into hollow capsule production line glue groove In, control film thickness is 0.10mm, and mold temperature is-5 DEG C, carries out dipping in glue, takes out, put into air dry oven after cooling molding In, at 35 DEG C, be dried 120min, obtain compound blank, then cut, fit, i.e. can get Capsules.
The Capsules present invention prepared is used for containing solid drugs, can be effectively isolated flavour of a drug, this Capsules disintegrate Time limit shortens 5min, capsule good toughness at 5 DEG C, and after storing at 45 DEG C, physicochemical property is unchanged, and bioavailability is high, adapts to Property wide, be worthy to be popularized and use.

Claims (1)

1. a cactus polyoses is combined the method that curdlan prepares Capsules, it is characterised in that concrete preparation process is:
(1) weigh 100~200g Radix et Caulis Opuntiae Dilleniis, put it into underhand polish in stone mortar and smash to pieces, then with homogenizer stirring homogenate 50~ 60min, pours in microwave oscillation instrument, and in Radix et Caulis Opuntiae Dillenii is homogenized, 1:5 in mass ratio adds mass fraction 90% ethanol, 150~ Under 250W, microwave pretreatment 30~40min, filter to get filtrate, and filtrate is spray-dried to obtain Radix et Caulis Opuntiae Dillenii powder;
(2) above-mentioned Radix et Caulis Opuntiae Dillenii powder is put in pottery enzymatic vessel, be added thereto to pottery enzymatic vessel volume 1/3 deionization simultaneously Water mixes, and adds mixed liquor gross mass 3~5% compound enzyme, enzymolysis 1~2h at 30~40 DEG C, and goes out at 100~105 DEG C Ferment treatment 10~15min, then centrifugation 10~15min, obtain supernatant;Described compound enzyme by cellulase, pectase and Protease prepares for 1:1:2 is compounding in mass ratio;
(3) above-mentioned supernatant is put in bag filter, dialyse 2~4 days at 4 DEG C, dialysis solution is evaporated to original volume 15 ~20%, in concentrated solution, add its volume 3~5 times of mass fraction 90% ethanol solution, centrifugation after standing 30~40min, Precipitate lyophilization, cactus polyoses, standby;
(4) weigh 20~30g curdlans, be that 2 DEG C of water mix, with 800~1000r/min by it by solid-to-liquid ratio 1:4 and temperature Rotating speed dispersed with stirring 40~50min, obtains curdlan dispersion liquid, is loaded in flask by dispersion liquid, and moves in water-bath, 70~ At 80 DEG C stirring mixing 1~2h, curdlan solution;
(5) being added in the cactus polyoses that step (3) is standby by above-mentioned curdlan solution 1:1 by volume, addition limit, limit exists Stirring mixing 2~4h under 1000~1200r/min rotating speeds so that it is be thoroughly mixed uniformly, obtain curdlan blend solution;
(6) count by weight, choose 100~120 parts of above-mentioned curdlan blend solutions respectively, 10~20 parts of Polyethylene Glycol, 3 ~5 parts of glacial acetic acid, 1~3 part of sodium lauryl sulphate, 60~80 parts of water, first can so glue blend solution, Polyethylene Glycol, 12 Alkyl sodium sulfate and glacial acetic acid add in reactor, and temperature of reactor is increased to 80~90 DEG C, after stirring mixing 5~10min, In reactor, add water, continue stirring mixing 50~70min, after mixing, be cooled to 50~60 DEG C, be incubated 2~3h, To Capsules glue;
(7) pouring in hollow capsule production line glue groove by above-mentioned Capsules glue, controlling film thickness is 0.08~0.10mm, mould Tool temperature be-30~-5 DEG C, carries out dipping in glue, takes out, put in air dry oven after cooling molding, dry at 30~35 DEG C 100~120min, obtain compound blank, then cut, fit, i.e. can get Capsules.
CN201610468622.6A 2016-06-25 2016-06-25 A kind of cactus polyoses is combined the method that curdlan prepares Capsules Pending CN106074432A (en)

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