CN109771389A - A kind of hydroxypropyl methylcellulose enteric hollow capsule by calcium salt and sodium salt gel - Google Patents
A kind of hydroxypropyl methylcellulose enteric hollow capsule by calcium salt and sodium salt gel Download PDFInfo
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Abstract
A kind of hydroxypropyl methylcellulose enteric hollow capsule by calcium salt and sodium salt gel, belong to Capsules production technical field, hydroxypropyl methylcellulose is stirred in purified water by it first becomes hydroxypropyl methylcellulose solution, it is blended into gelling agent and obtains hydroxypropyl methylcellulose gel solution, it is blended into calcium salt and obtains hydroxypropyl methylcellulose calcium sol solution, it is blended into sodium salt and obtains hydroxypropyl methylcellulose colloidal solution, then dip in glue and hydroxypropyl methylcellulose enteric hollow capsule is made；The beneficial effect is that increasing the moldability that sodium alginate improves colloidal solution, calcium salt is first mixed into during mixing, it is blended into sodium alginate, mixing is added in gelling agent swelling solution by gage distortion when effectively can solve the problems, such as to dip in glue when the temperature than hydroxypropyl methylcellulose solution is high, is deaerated in conjunction with vacuum filtration, fine gas bubbles remaining in solution can thoroughly be discharged, substantially prevent the fine gas bubbles on Capsules body, effectively improve product quality, improves production efficiency.
Description
Technical field
It is especially a kind of to be prepared using hydroxypropyl methylcellulose as raw material the invention belongs to Capsules production technical field
By the vegetalitas enteric hollow capsule of calcium salt and sodium salt gel.
Background technique
Capsules are made of the refined cap of medicinal materials, two section capsule shells of body, for containing solid drugs；As certainly
Powder processed, health care product, medicament etc. solve the problems, such as difficult entrance, poor taste for user, it is no longer bitter to be truly realized good medicine
Mouthful；Since pharmaceutical capsules are easy to swallow, the uncomfortable taste and smell of content can be very effectively covered, increasingly
It is welcome by patient.
Pervious Capsules mainly have the gelatine capsule and various vegetalitas capsules of animality.It is deposited in view of existing capsule
In various defects, our company researched and developed and had declared Patent No. 2013103462277 in 2013, entitled cold by tying
The hydroxypropyl methylcellulose enteric hollow capsule of glue and calcium chloride gel.The patent is main raw material(s) mixing by hydroxypropyl methylcellulose
Gellan gum and calcium chloride are made under specific condition, and in time, water content is low, and it is strong and right to be suitable for hygroscopicity for the capsule disintegration of production
Divide the drug of water sensitive, dissolution medium influences small, medication compliance height on softgel shell；Storage life, is long, and 3-4 never degenerates, right
The requirement of the condition of storage and transport is low, and friability is not easy under low moisture environments, is unlikely to deform under hot environment, is not easy to rot.But
It is by production and using practice in recent years, when discovery is using patented method production Capsules, containing micro- on capsule body
The ratio of bubble and gage distortion is excessive, often has 30% or so product unqualified, causes production efficiency low.
Summary of the invention
The technical problems to be solved by the present invention are: in view of the deficiencies of the prior art, providing and joined sodium salt and using special
Different directions or tendencies method eliminates the hydroxypropyl methylcellulose Capsules of microbubble, to reduce microbubble, increases moldability and reduces gage distortion
The problem of, production efficiency is improved on the whole.
In order to solve the above technical problems, the technical scheme adopted by the invention is that a kind of hydroxypropyl by calcium salt and sodium salt gel
Methylcellulose enteric hollow capsule, it is characterised in that preparation method is as follows.
(1) hydroxypropyl methylcellulose 50kg is taken, is put into the purified water that 110-115L temperature is 87-97 DEG C, quickly stirring is mixed
It is 9-11 minutes even, 60-90min then is stood in 80-90 DEG C of at a temperature of heat preservation, obtains hydroxypropyl methylcellulose solution.
(2) take in the purified water that gelling agent 330-380g stirring swells in 110-115L, temperature is 40-45 DEG C, then heat
To 85-95 DEG C and standing 55-65min is kept the temperature, obtains gelling agent swelling solution.
(3) it is fine gelling agent swelling solution to be added to hydroxypropyl first with high 4-6 DEG C of temperature of the temperature than hydroxypropyl methylcellulose solution
It ties up in plain solution, hydroxypropyl methylcellulose solution and gelling agent swelling solution is poured into mixing kettle with identical speed simultaneously when addition
In and start to stir when pouring into, 9-11min is persistently stirred and evenly mixed after being finished down, is then cooled to 75-85 DEG C, it is fine to obtain hydroxypropyl first
Tie up plain gel solution；The volume of gelling agent swelling solution is made into this way level off to the volume of hydroxypropyl methylcellulose solution it is equal,
Gelling agent swelling solution can be allow to be put into mixing kettle when mixing with hydroxypropyl methylcellulose solution with identical speed equivalent to stir
It mixes, is easier to be uniformly mixed in this way；The temperature of gelling agent swelling solution is made into and the high 4-6 of the temperature of hydroxypropyl methylcellulose solution
DEG C, gelling agent swelling solution can be made to be easier to be mixed into cellulose solution.
The gelling agent is one of gellan gum, carragheen, konjac glucomannan, xanthan gum, guar gum or a variety of mixing
Object.
(4) take calcium salt 260-290g to be added in hydroxypropyl methylcellulose gel solution, stirred with the speed of 900-1100rpm
Then 2-3min vacuumizes suction filtration degassing 9-11min, and solution is made to be cooled to 65-75 DEG C, obtain hydroxypropyl methylcellulose calcium peptization
Liquid；
The calcium salt is one of calcium chloride, calcium acetate, calcium citrate, calcium lactate, calcium gluconate or a variety of mixtures.
(5) take sodium salt 800-900g to be added in hydroxypropyl methylcellulose calcium sol solution, continue the speed with 900-1100rpm
Stir 2-3min, stir and vacuumize suction filtration degassing 9-11min, then 55-65 DEG C at a temperature of stand 3-5 hours,
It obtains impregnating stable hydroxypropyl methylcellulose colloidal solution；
The sodium salt is sodium alginate.
(6) in the environment of 40-45 DEG C of temperature, relative humidity 45~55%, by capsule die in hydroxypropyl methylcellulose colloid
Glue Cheng Mo is dipped in solution, it is then dry in the environment of 15-23 DEG C of temperature, relative humidity 30~35%, obtain dry capsule
Stick.
(7) capsule stick is immersed in hydroxypropyl methylcellulose phthalic acid rouge organic solution carry out it is secondary dip in glue, in capsule
Coatings are formed outside stick, then take out drying.It in this step, can also be according to the volume ratio of 1%-2% in hydroxypropyl methylcellulose
Tween 80 is added in phthalic acid rouge organic solution, notch breakage can be effectively reduced when cutting capsule in this way.
(8) finally by demoulding, cut, hydroxypropyl methylcellulose enteric hollow capsule is made in fitting.
In practice process of the present invention, research and development group, company adopts after colloidal sol by long-term experiment many times
Fine gas bubbles are eliminated under 20-100 DEG C of environment temperature, or eliminate fine gas bubbles only with vacuum method, and effect is paid no attention to
Think.Gellan gum swelling solution is once added to unintentionally mixing in the case where the temperature than hydroxypropyl methylcellulose solution is high, is sent out
It now can effectively eliminate the fine gas bubbles in colloidal solution in this way.Using repetition test, it is found that same volume can with speed mixing
So that mixed effect is more preferable, fine gas bubbles, the sky of such colloidal solution production can be thoroughly eliminated in conjunction with vacuum filtration degassing
Heart-soothing capsule there is no microbubble.
A large number of experiments did in the problem of about gage distortion, invention group, was initially to increase the component of purified water, but pay no attention to
Think.Just expected being had a try with sodium alginate after trying many materials, usually be added to sodium alginate simultaneously with calcium chloride solidifying
In sol solution, but still there is the problem of gage distortion after dipping in glue, just finds to admix calcium chloride and sodium alginate according to order later
It can be very good to solve the problems, such as gage distortion into gel solution.
The beneficial effects of the invention are as follows using hydroxypropyl methylcellulose as enteric hollow capsule main material, so that Capsules have
For a variety of advantages possessed by hydroxypropyl methylcellulose, it is mainly manifested in chemical property stabilization, without cross-linking reaction, and softgel shell is same
When be disintegrated, so disintegration it is very timely；Water content is low, can be controlled in 8% or so, reduces drug hygroscopicity risk, is suitable for hygroscopicity
By force and to the drug for dividing water sensitive, especially health care product and cosmetics；Dissolution medium is small on softgel shell influence, to the adhesion strength of oesophagus
Small, medication compliance is high；It is easy storage, validity period is long, and 3-4 never degenerates, and requires low, low humidity ring to the condition of storage and transport
It is not easy friability under border, friability≤20% under 35%RH environment is unlikely to deform under hot environment, utricule deformation under 80 DEG C of environment≤
1%, protein is free of in raw material, so that the existence of bacterium and breeding is lost necessary condition, is not easy to rot；Pure plant is fine
Dimension, raw material sources are relatively simple, meet the requirement of all culture backgrounds and religious belief crowd；It is highly-safe, no animal infection
Sick risk, remaining hormone, drug and other harmful substances in no animal body；Almost pollution-free in production process, tailing can two
Secondary back dissolving utilizes；Common surfactant and plasticizer are eliminated, only helps condensation cold glue to reduce gelling temp by calcium chloride
Accelerate gelation rate, reduce additive, reduce production cost, is suitble to large-scale popularization.
Especially increase the moldability that suitable sodium alginate improves colloidal solution, in hydroxypropyl methylcellulose gel solution
It is middle to be first mixed into calcium salt, the problem of being blended into sodium alginate after mixing, gage distortion when dipping in glue can be substantially reduced；In production solution
When, gelling agent swelling solution is added to mixing in the case where the temperature than hydroxypropyl methylcellulose solution is high, it is de- in conjunction with vacuum filtration
Fine gas bubbles remaining in solution can thoroughly be discharged in each step, can substantially prevent Capsules in this way by gas
Fine gas bubbles on body effectively improve product quality, improve production efficiency.
Specific embodiment
Below with reference to embodiment, the invention will be further described, and following embodiment is intended to illustrate invention rather than to this
Further limiting for invention, should not be limited the scope of the invention with this.
Embodiment 1.
(1) hydroxypropyl methylcellulose 50kg is taken, puts into the purified water that 110L temperature is 87 DEG C, quickly stirs and evenly mixs 9 points
Then clock stands 60min in 80 DEG C of at a temperature of heat preservation, obtains hydroxypropyl methylcellulose solution.
(2) take in the purified water that gellan gum 330g stirring swells in 110L, temperature is 40 DEG C, be then heated to 85 DEG C and protect
Temperature stands 55min, obtains gellan gum swelling solution.
(3) gellan gum swelling solution is added to hypromellose with high 4 DEG C of the temperature of temperature than hydroxypropyl methylcellulose solution
In plain solution, hydroxypropyl methylcellulose solution and gellan gum swelling solution are poured into mixing kettle simultaneously with identical speed when addition
And start to stir when pouring into, 9min is persistently stirred and evenly mixed after being finished down, is then cooled to 75 DEG C, obtains hydroxypropyl methylcellulose gel
Solution.
(4) take calcium chloride 260g to be added in hydroxypropyl methylcellulose gel solution, stir 2min with the speed of 900rpm, so
After vacuumize suction filtration degassing 9min, and solution is made to be cooled to 65 DEG C, obtains hydroxypropyl methylcellulose calcium sol solution.
(5) take sodium alginate 800g to be added in hydroxypropyl methylcellulose calcium sol solution, continue to be stirred with the speed of 900rpm
2min is stirred and vacuumize suction filtration degassing 9min, then 55 DEG C at a temperature of stand 3 hours, obtain impregnating stable
Hydroxypropyl methylcellulose colloidal solution.
Sodium alginate, which is added, can be such that colloidal solution is easier into mould.
First calcium chloride must be added herein, then sodium alginate is added, calcium chloride and sodium alginate cannot be added simultaneously
Enter, can not first heat sodium alginate and add calcium chloride, otherwise there is the case where gage distortion when dipping in glue, it may be possible to because
There is hydrophily for sodium alginate, first adding sodium alginate after addition calcium chloride can be such that gel solution is improved.
(6) in the environment of 40 DEG C of temperature, relative humidity 45%, capsule die is dipped in hydroxypropyl methylcellulose colloidal solution
Glue Cheng Mo, it is then dry in the environment of 15 DEG C of temperature, relative humidity 30%, obtain dry capsule stick.
(7) capsule stick is immersed in hydroxypropyl methylcellulose phthalic acid rouge organic solution carry out it is secondary dip in glue, in capsule
Coatings are formed outside stick, then take out drying.
(8) finally by demoulding, cut, hydroxypropyl methylcellulose enteric hollow capsule is made in fitting.
It randomly selects 100 Capsules to be detected, only 1 containing fine gas bubbles of discovery, only the 5 of gage distortion
Reaching 30% with pervious disqualification rate compares, and production qualification rate, which has, to be greatly improved.
Embodiment 2.
(1) hydroxypropyl methylcellulose 50kg is taken, puts into the purified water that 113L temperature is 92 DEG C, quickly stirs and evenly mixs 10 points
Then clock stands 75min in 85 DEG C of at a temperature of heat preservation, obtains hydroxypropyl methylcellulose solution.
(2) take in the purified water that gellan gum 357g stirring swells in 113L, temperature is 42.5 DEG C, be then heated to 90 DEG C simultaneously
Heat preservation stands 60min, obtains gelling agent swelling solution.
(3) gellan gum swelling solution is added to hypromellose with high 5 DEG C of the temperature of temperature than hydroxypropyl methylcellulose solution
In plain solution, hydroxypropyl methylcellulose solution and gellan gum swelling solution are poured into mixing kettle simultaneously with identical speed when addition
And start to stir when pouring into, 10min is persistently stirred and evenly mixed after being finished down, is then cooled to 80 DEG C, and it is solidifying to obtain hydroxypropyl methylcellulose
Sol solution.
(4) take calcium chloride 271g to be added in hydroxypropyl methylcellulose gel solution, stir 2.5min with the speed of 1000rpm,
Then suction filtration degassing 10min is vacuumized, and solution is made to be cooled to 70 DEG C, obtains hydroxypropyl methylcellulose calcium sol solution.
(5) take sodium alginate 850g to be added in hydroxypropyl methylcellulose calcium sol solution, continue to be stirred with the speed of 1000rpm
2.5min is stirred and vacuumize suction filtration degassing 10min, then 60 DEG C at a temperature of stand 4 hours, obtain dipping and stablize
Hydroxypropyl methylcellulose colloidal solution；
(6) in the environment of 42.5 DEG C of temperature, relative humidity 50%, capsule die is dipped in into glue in hydroxypropyl methylcellulose colloidal solution
Cheng Mo, it is then dry in the environment of 19 DEG C of temperature, relative humidity 32.5%, obtain dry capsule stick；
(7) capsule stick is immersed in hydroxypropyl methylcellulose phthalic acid rouge organic solution carry out it is secondary dip in glue, outside capsule stick
Coatings are formed, drying is then taken out；
(8) finally by demoulding, cut, hydroxypropyl methylcellulose enteric hollow capsule is made in fitting.
It randomly selects 100 Capsules to be detected, does not find the capsule containing fine gas bubbles, gage distortion is only
2 reach 30% with pervious disqualification rate and compare, and have and greatly improve.
When gelling agent uses calcium chloride using gellan gum, calcium salt, hydroxypropyl methylcellulose, gellan gum, calcium chloride and seaweed
It is optimum proportion scheme that the weight proportion of sour sodium, which takes 50kg:357g:271g:850g,.
Embodiment 3.
(1) hydroxypropyl methylcellulose 50kg is taken, puts into the purified water that 115L temperature is 97 DEG C, quickly stirs and evenly mixs 11 points
Then clock stands 90min in 90 DEG C of at a temperature of heat preservation, obtains hydroxypropyl methylcellulose solution；
(2) take in the purified water that gellan gum 380g stirring swells in 115L, temperature is 45 DEG C, be then heated to 95 DEG C and keep the temperature quiet
65min is set, gelling agent swelling solution is obtained；
(3) it is molten gellan gum swelling solution to be added to hydroxypropyl methylcellulose with high 6 DEG C of the temperature of temperature than hydroxypropyl methylcellulose solution
In liquid, when addition by hydroxypropyl methylcellulose solution and gellan gum swelling solution be poured into mixing kettle simultaneously with identical speed and
Start to stir when pouring into, 11min is persistently stirred and evenly mixed after being finished down, be then cooled to 85 DEG C, it is molten to obtain hydroxypropyl methylcellulose gel
Liquid；
(4) take calcium chloride 290g to be added in hydroxypropyl methylcellulose gel solution, stir 3min with the speed of 1100rpm, then take out
Vacuum filtration degassing 11min, and solution is made to be cooled to 75 DEG C, obtain hydroxypropyl methylcellulose calcium sol solution；
(5) take sodium alginate 900g to be added in hydroxypropyl methylcellulose calcium sol solution, continue the speed stirring 3min with 1100rpm,
Stir and vacuumize suction filtration degassing 11min, then 65 DEG C at a temperature of stand 5 hours, obtain impregnating stable hydroxypropyl
Methylcellulose colloidal solution；
(6) in the environment of temperature 45 C, relative humidity 55%, capsule die is dipped in hydroxypropyl methylcellulose colloidal solution glue at
Mould, it is then dry in the environment of 23 DEG C of temperature, relative humidity 35%, obtain dry capsule stick；
(7) capsule stick is immersed in hydroxypropyl methylcellulose phthalic acid rouge organic solution carry out it is secondary dip in glue, outside capsule stick
Coatings are formed, drying is then taken out；
(8) finally by demoulding, cut, hydroxypropyl methylcellulose enteric hollow capsule is made in fitting.
It randomly selects 100 Capsules to be detected, does not find the capsule containing fine gas bubbles, gage distortion is only
5 reach 30% with pervious disqualification rate and compare, and have and greatly improve.
Embodiment 4.
(1) hydroxypropyl methylcellulose 50kg is taken, puts into the purified water that 110L temperature is 87 DEG C, quickly stirs and evenly mixs 9 points
Then clock stands 60min in 80 DEG C of at a temperature of heat preservation, obtains hydroxypropyl methylcellulose solution.
(2) take in the purified water that konjac glucomannan 330g stirring swells in 110L, temperature is 40 DEG C, be then heated to 85 DEG C and protect
Temperature stands 55min, obtains konjac glucomannan swelling solution.
(3) konjac glucomannan swelling solution is added to hypromellose with high 4 DEG C of the temperature of temperature than hydroxypropyl methylcellulose solution
In plain solution, hydroxypropyl methylcellulose solution and konjac glucomannan swelling solution are poured into mixing kettle simultaneously with identical speed when addition
And start to stir when pouring into, 9min is persistently stirred and evenly mixed after being finished down, is then cooled to 75 DEG C, obtains hydroxypropyl methylcellulose gel
Solution.
(4) take calcium lactate 260g to be added in hydroxypropyl methylcellulose gel solution, stir 2min with the speed of 900rpm, so
After vacuumize suction filtration degassing 9min, and solution is made to be cooled to 65 DEG C, obtains hydroxypropyl methylcellulose calcium sol solution.
(5) take sodium alginate 800g to be added in hydroxypropyl methylcellulose calcium sol solution, continue to be stirred with the speed of 900rpm
2min is stirred and vacuumize suction filtration degassing 9min, then 55 DEG C at a temperature of stand 3 hours, obtain impregnating stable
Hydroxypropyl methylcellulose colloidal solution.
(6) in the environment of 40 DEG C of temperature, relative humidity 45%, capsule die is dipped in hydroxypropyl methylcellulose colloidal solution
Glue Cheng Mo, it is then dry in the environment of 15 DEG C of temperature, relative humidity 30%, obtain dry capsule stick.
(7) capsule stick is immersed in hydroxypropyl methylcellulose phthalic acid rouge organic solution carry out it is secondary dip in glue, in capsule
Coatings are formed outside stick, then take out drying.
(8) finally by demoulding, cut, hydroxypropyl methylcellulose enteric hollow capsule is made in fitting.
It randomly selects 100 Capsules to be detected, only 1 containing fine gas bubbles of discovery, only the 6 of gage distortion
Reaching 30% with pervious disqualification rate compares, and production qualification rate, which has, to be greatly improved.
Embodiment 5.
(1) hydroxypropyl methylcellulose 50kg is taken, puts into the purified water that 113L temperature is 92 DEG C, quickly stirs and evenly mixs 10 points
Then clock stands 75min in 85 DEG C of at a temperature of heat preservation, obtains hydroxypropyl methylcellulose solution.
(2) take in the purified water that konjac glucomannan 346g stirring swells in 113L, temperature is 42.5 DEG C, be then heated to 90 DEG C simultaneously
Heat preservation stands 60min, obtains gelling agent swelling solution.
(3) konjac glucomannan swelling solution is added to hypromellose with high 5 DEG C of the temperature of temperature than hydroxypropyl methylcellulose solution
In plain solution, hydroxypropyl methylcellulose solution and konjac glucomannan swelling solution are poured into mixing kettle simultaneously with identical speed when addition
And start to stir when pouring into, 10min is persistently stirred and evenly mixed after being finished down, is then cooled to 80 DEG C, and it is solidifying to obtain hydroxypropyl methylcellulose
Sol solution.
(4) take calcium lactate 277g to be added in hydroxypropyl methylcellulose gel solution, stir 2.5min with the speed of 1000rpm,
Then suction filtration degassing 10min is vacuumized, and solution is made to be cooled to 70 DEG C, obtains hydroxypropyl methylcellulose calcium sol solution.
(5) take sodium alginate 850g to be added in hydroxypropyl methylcellulose calcium sol solution, continue to be stirred with the speed of 1000rpm
2.5min is stirred and vacuumize suction filtration degassing 10min, then 60 DEG C at a temperature of stand 4 hours, obtain dipping and stablize
Hydroxypropyl methylcellulose colloidal solution.
(6) in the environment of 42.5 DEG C of temperature, relative humidity 50%, by capsule die in hydroxypropyl methylcellulose colloidal solution
Glue Cheng Mo is dipped in, it is then dry in the environment of 19 DEG C of temperature, relative humidity 32.5%, obtain dry capsule stick.
(7) capsule stick is immersed in hydroxypropyl methylcellulose phthalic acid rouge organic solution carry out it is secondary dip in glue, in capsule
Coatings are formed outside stick, then take out drying.
(8) finally by demoulding, cut, hydroxypropyl methylcellulose enteric hollow capsule is made in fitting.
It randomly selects 100 Capsules to be detected, does not find the capsule containing fine gas bubbles, gage distortion is only
3 reach 30% with pervious disqualification rate and compare, and have and greatly improve.
When gelling agent uses calcium lactate using konjac glucomannan, calcium salt, hydroxypropyl methylcellulose, konjac glucomannan, calcium lactate and seaweed
The best weight ratio scheme of sour sodium is 50kg:346g:277g:850g.
Embodiment 6.
(1) hydroxypropyl methylcellulose 50kg is taken, puts into the purified water that 115L temperature is 97 DEG C, quickly stirs and evenly mixs 11 points
Then clock stands 90min in 90 DEG C of at a temperature of heat preservation, obtains hydroxypropyl methylcellulose solution；
(2) take in the purified water that konjac glucomannan 370g stirring swells in 115L, temperature is 45 DEG C, be then heated to 95 DEG C and keep the temperature quiet
65min is set, gelling agent swelling solution is obtained；
(3) it is molten konjac glucomannan swelling solution to be added to hydroxypropyl methylcellulose with high 6 DEG C of the temperature of temperature than hydroxypropyl methylcellulose solution
In liquid, when addition by hydroxypropyl methylcellulose solution and konjac glucomannan swelling solution be poured into mixing kettle simultaneously with identical speed and
Start to stir when pouring into, 11min is persistently stirred and evenly mixed after being finished down, be then cooled to 85 DEG C, it is molten to obtain hydroxypropyl methylcellulose gel
Liquid；
(4) take calcium lactate 290g to be added in hydroxypropyl methylcellulose gel solution, stir 3min with the speed of 1100rpm, then take out
Vacuum filtration degassing 11min, and solution is made to be cooled to 75 DEG C, obtain hydroxypropyl methylcellulose calcium sol solution；
(5) take sodium alginate 900g to be added in hydroxypropyl methylcellulose calcium sol solution, continue the speed stirring 3min with 1100rpm,
Stir and vacuumize suction filtration degassing 11min, then 65 DEG C at a temperature of stand 5 hours, obtain impregnating stable hydroxypropyl
Methylcellulose colloidal solution；
(6) in the environment of temperature 45 C, relative humidity 55%, capsule die is dipped in hydroxypropyl methylcellulose colloidal solution glue at
Mould, it is then dry in the environment of 23 DEG C of temperature, relative humidity 35%, obtain dry capsule stick；
(7) capsule stick is immersed in hydroxypropyl methylcellulose phthalic acid rouge organic solution carry out it is secondary dip in glue, outside capsule stick
Coatings are formed, drying is then taken out；
(8) finally by demoulding, cut, hydroxypropyl methylcellulose enteric hollow capsule is made in fitting.
It randomly selects 100 Capsules to be detected, only finds that 1 capsule contains fine gas bubbles, only the 3 of gage distortion
Reaching 30% or so with pervious disqualification rate compares, and has and greatly improves.
Effect test.Disintegration time mensuration is carried out to each embodiment product.To the enteric hollow glue of five embodiments production
Capsule product respectively takes 10 to be tested, and installs by content of talcum powder, respectively in the mould that temperature is (37 ± 1) DEG C, pH=1.1
It is measured 2 hours in quasi- gastric juice, observes the disintegration situation of capsule.In the case where no disintegration, by whole capsules synthermal
It is lower with purifying water washing three times, be put in the simulated intestinal fluid of (37 ± 1) DEG C, pH=6.8 and measure disintegration time, record 30 capsules
The time required to starting disintegration to complete disintegration.
As it can be seen that the disintegration of the enteric hollow capsule product of the method for the present invention production works well.
Claims (6)
1. a kind of hydroxypropyl methylcellulose enteric hollow capsule by calcium salt and sodium salt gel, it is characterised in that the preparation method is as follows:
(1) hydroxypropyl methylcellulose 50kg is taken, puts into the purified water that 110-115L temperature is 87-97 DEG C, quickly stirs and evenly mixs 9-
11 minutes, 60-90min then is stood in 80-90 DEG C of at a temperature of heat preservation, obtains hydroxypropyl methylcellulose solution；
(2) take in the purified water that gelling agent 330-380g stirring swells in 110-115L, temperature is 40-45 DEG C, be then heated to
85-95 DEG C and keep the temperature stand 55-65min, obtain gelling agent swelling solution；
(3) gelling agent swelling solution is added to hydroxypropyl methylcellulose with high 4-6 DEG C of temperature of the temperature than hydroxypropyl methylcellulose solution
In solution, hydroxypropyl methylcellulose solution and gelling agent swelling solution are poured into mixing kettle simultaneously simultaneously with identical speed when addition
Start to stir when pouring into, 9-11min is persistently stirred and evenly mixed after being finished down, is then cooled to 75-85 DEG C, obtains hydroxypropyl methylcellulose
Gel solution；
(4) take calcium salt 260-290g to be added in hydroxypropyl methylcellulose gel solution, stir 2- with the speed of 900-1100rpm
Then 3min vacuumizes suction filtration degassing 9-11min, and solution is made to be cooled to 65-75 DEG C, obtain hydroxypropyl methylcellulose calcium peptization
Liquid；
(5) take sodium salt 800-900g to be added in hydroxypropyl methylcellulose calcium sol solution, continue to be stirred with the speed of 900-1100rpm
2-3min is stirred and vacuumize suction filtration degassing 9-11min, then 55-65 DEG C at a temperature of stand 3-5 hours, obtain
Impregnate stable hydroxypropyl methylcellulose colloidal solution；
(6) in the environment of 40-45 DEG C of temperature, relative humidity 45~55%, by capsule die in hydroxypropyl methylcellulose colloidal solution
In dip in glue Cheng Mo, it is then dry in the environment of 15-23 DEG C of temperature, relative humidity 30~35%, obtain dry capsule stick；
(7) capsule stick is immersed in hydroxypropyl methylcellulose phthalic acid rouge organic solution carry out it is secondary dip in glue, outside capsule stick
Coatings are formed, drying is then taken out；
(8) finally by demoulding, cut, hydroxypropyl methylcellulose enteric hollow capsule is made in fitting.
2. the hydroxypropyl methylcellulose enteric hollow capsule according to claim 1 by calcium salt and sodium salt gel, feature exist
In the gelling agent be one of gellan gum, carragheen, konjac glucomannan, xanthan gum, guar gum or a variety of mixtures.
3. the hydroxypropyl methylcellulose enteric hollow capsule according to claim 2 by calcium salt and sodium salt gel, feature exist
In the calcium salt be one of calcium chloride, calcium acetate, calcium citrate, calcium lactate, calcium gluconate or a variety of mixtures.
4. the hydroxypropyl methylcellulose enteric hollow capsule according to claim 3 by calcium salt and sodium salt gel, feature exist
In the sodium salt be sodium alginate.
5. the hydroxypropyl methylcellulose enteric hollow capsule according to claim 4 by calcium salt and sodium salt gel, feature exist
In when gelling agent uses calcium chloride using gellan gum, calcium salt, hydroxypropyl methylcellulose, gellan gum, calcium chloride and sodium alginate
Best weight ratio scheme are as follows: 50kg:357g:271g:850g.
6. the hydroxypropyl methylcellulose enteric hollow capsule according to claim 4 by calcium salt and sodium salt gel, feature exist
In when gelling agent uses calcium lactate using konjac glucomannan, calcium salt, hydroxypropyl methylcellulose, konjac glucomannan, calcium lactate and sodium alginate
Best weight ratio scheme is 50kg:346g:277g:850g.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910254934.0A CN109771389B (en) | 2019-04-01 | 2019-04-01 | Hydroxypropyl methylcellulose enteric empty capsule formed by gelling calcium salt and sodium salt |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910254934.0A CN109771389B (en) | 2019-04-01 | 2019-04-01 | Hydroxypropyl methylcellulose enteric empty capsule formed by gelling calcium salt and sodium salt |
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| Publication Number | Publication Date |
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| CN109771389A true CN109771389A (en) | 2019-05-21 |
| CN109771389B CN109771389B (en) | 2020-02-14 |
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| CN201910254934.0A Active CN109771389B (en) | 2019-04-01 | 2019-04-01 | Hydroxypropyl methylcellulose enteric empty capsule formed by gelling calcium salt and sodium salt |
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| CN112587668A (en) * | 2020-12-30 | 2021-04-02 | 湖北人福药用辅料股份有限公司 | Enteric pore-forming agent, preparation method thereof and enteric capsule |
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| CN103330695A (en) * | 2013-06-05 | 2013-10-02 | 绍兴康可胶囊有限公司 | Preparation method for enteric plant cellulose hard hollow capsules |
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| CN103432096A (en) * | 2013-08-11 | 2013-12-11 | 重庆衡生药用胶囊有限责任公司 | Hydroxypropyl methylcellulose enteric empty capsule jellied by carrageenan and potassium citrate |
| CN108576785A (en) * | 2018-04-11 | 2018-09-28 | 扬州大学 | A kind of hydroxypropyl methyl cellulose base edibility is protected from light the preparation method of embedding wall material |
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| CN112587668A (en) * | 2020-12-30 | 2021-04-02 | 湖北人福药用辅料股份有限公司 | Enteric pore-forming agent, preparation method thereof and enteric capsule |
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