CN109846852B - Hydroxypropyl methylcellulose enteric empty capsule formed by gelling sylvite and sodium salt - Google Patents
Hydroxypropyl methylcellulose enteric empty capsule formed by gelling sylvite and sodium salt Download PDFInfo
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Abstract
A hypromellose enteric empty capsule gelling sylvite and sodium salt, it is the empty capsule production technical field, stir hypromellose into purified water to become hypromellose solution at first, mix with gelata and get hypromellose colloidal solution, mix with sylvite and get hypromellose potassium colloidal solution, mix with sodium salt and get hypromellose colloidal solution, then dip in and glue and make hypromellose enteric empty capsule; the method has the beneficial effects that the sodium alginate is added, so that the molding property of the colloid solution is improved, the potassium salt is mixed into the solution, and then the sodium alginate is mixed into the solution, so that the problem of uneven thickness during gum dipping can be greatly reduced; the gel swelling solution is added and mixed when the temperature is higher than that of a hydroxypropyl methylcellulose solution, and the vacuum filtration degassing is combined, so that residual fine bubbles in the solution can be thoroughly released, the fine bubbles on a hollow capsule body are basically eliminated, the product quality is effectively improved, and the production efficiency is improved.
Description
Technical Field
The invention belongs to the technical field of hollow capsule production, and particularly relates to a plant enteric hollow capsule which is prepared by taking hydroxypropyl methylcellulose as a raw material and is gelated by potassium salt and sodium salt.
Background
The hollow capsule consists of a cap and a body which are refined from medicinal materials and are used for containing solid medicines; such as self-made powder, health products, medicaments and the like, solves the problems of difficult taste and poor mouthfeel for users, and really realizes that good medicines are not bitter; because the empty capsules are easy to swallow, they are becoming increasingly popular with patients because they can effectively mask the unpleasant taste and odor of the contents.
The prior hollow capsules mainly comprise gelatin capsules of animal origin and various vegetable capsules. In view of various defects of the existing capsules, the company developed and reported 2013103462309 in 2013, namely a hypromellose enteric empty capsule gelled by gellan gum and potassium chloride. The capsule is prepared by mixing gellan gum and potassium chloride which are used as main raw materials under special conditions, the produced capsule is timely disintegrated, has low water content, is suitable for medicines with strong hygroscopicity and sensitivity to water, and has small influence on the capsule shell by dissolved media and high medication compliance; the storage period is long, the storage period is 3-4 years, the deterioration is avoided, the requirements on storage and transportation conditions are low, the product is not brittle in a low-humidity environment, and is not easy to deform or rot in a high-temperature environment. However, through the production and use practices in recent years, the proportion of microbubbles contained in the capsule body and uneven thickness is too large when the hollow capsule is produced by adopting the method disclosed by the patent, and about 30% of products are unqualified, so that the production efficiency is low.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: aiming at the defects of the prior art, the hydroxypropyl methylcellulose hollow capsule added with sodium salt and adopting a special method to eliminate micro bubbles is provided, so that the micro bubbles are reduced, the moldability is increased, the problem of uneven thickness is solved, and the production efficiency is integrally improved.
In order to solve the technical problems, the invention adopts the technical scheme that the hydroxypropyl methylcellulose enteric empty capsule is prepared by gelling sylvite and sodium salt, and is characterized in that the preparation method is as follows.
The preparation method comprises the steps of taking 50kg of hydroxypropyl methylcellulose, putting the hydroxypropyl methylcellulose into 120-130L of purified water with the temperature of 85-98 ℃, quickly stirring and uniformly mixing for 13-17 minutes, and then keeping the temperature and standing for 60-90 minutes at the temperature of 82-92 ℃ to obtain a hydroxypropyl methylcellulose solution.
And secondly, taking 405g of the gel agent 270-.
Thirdly, adding the gel swelling solution into the hydroxypropyl methylcellulose solution at a temperature 3-5 ℃ higher than that of the hydroxypropyl methylcellulose solution, pouring the hydroxypropyl methylcellulose solution and the gel swelling solution into a mixing kettle at the same speed when adding, starting stirring when pouring, continuously stirring and uniformly mixing for 13-17min after pouring, and then cooling to 75-85 ℃ to obtain the hydroxypropyl methylcellulose gel solution; the volume of the gel swelling solution is made to be approximately equal to that of the hydroxypropyl methylcellulose solution, so that the gel swelling solution and the hydroxypropyl methylcellulose solution can be equivalently put into a mixing kettle at the same speed and stirred when being mixed, and the gel swelling solution and the hydroxypropyl methylcellulose solution are easier to be uniformly mixed; the temperature of the gel swelling solution is made to be 3-5 ℃ higher than that of the hydroxypropyl methylcellulose solution, so that the gel swelling solution can be easily mixed into the cellulose solution.
The gel is one or more of gellan gum, carrageenan, konjac gum, xanthan gum and guar gum.
And fourthly, adding 270-320g of sylvite into the hydroxypropyl methylcellulose gel solution, stirring at the speed of 900-1100rpm for 2-3min, vacuumizing, filtering, degassing for 9-11min, and cooling the solution to 65-75 ℃ to obtain the hydroxypropyl methylcellulose potassium gel solution.
The potassium salt is one or a mixture of potassium chloride, potassium carbonate, potassium acetate and potassium citrate.
And fifthly, adding 850-950g of sodium salt into the hydroxypropyl methylcellulose potassium glue solution, continuing stirring at the speed of 900-1100rpm for 2-3min, stirring, performing vacuum pumping filtration and degassing for 9-11min, and standing at the temperature of 55-65 ℃ for 3-5 h to obtain the hydroxypropyl methylcellulose colloidal solution with stable impregnation.
The sodium salt is sodium alginate.
Sixthly, dipping a capsule mold in a hydroxypropyl methylcellulose colloidal solution to form a mold under the environment that the temperature is 40-45 ℃ and the relative humidity is 45-55%, and then drying under the environment that the temperature is 15-23 ℃ and the relative humidity is 30-35% to obtain a dried capsule rod.
And immersing the capsule rod into a hydroxypropyl methylcellulose phthalate organic solution for secondary glue dipping, forming a coating layer outside the capsule rod, and taking out and drying.
Finally, the hydroxypropyl methylcellulose enteric empty capsule is prepared by demoulding, cutting and sheathing.
In the practice process of the invention, after numerous experiments for a long time, the company research and development group eliminates fine micro bubbles at the environmental temperature of 20-100 ℃ or only eliminates fine bubbles by a vacuum method after sol is finished, and the effect is not ideal. The gellan gum swelling solution was inadvertently added to the mix at a higher temperature than the hypromellose solution, and this was found to effectively eliminate fine bubbles in the gum solution. Repeated tests show that the mixing effect can be better by uniformly mixing the colloid solution with the same volume and the same speed, fine bubbles can be thoroughly eliminated by combining vacuum filtration and degassing, and the hollow capsule prepared from the colloid solution basically does not contain micro bubbles.
Regarding the problem of uneven thickness, the small group of the invention made extensive tests, initially increasing the amount of purified water, but not desirable. After many materials are tried, a sodium alginate trial is thought, generally, sodium alginate and potassium chloride are added into a gel solution at the same time, but the problem of uneven thickness is still existed after the gel is dipped, and the problem of uneven thickness can be well solved by mixing the potassium chloride and the sodium alginate into the gel solution in order.
The invention has the advantages that the hydroxypropyl methylcellulose is used as the main material of the enteric hollow capsule, so that the hollow capsule has various advantages of the hydroxypropyl methylcellulose, and the hollow capsule is mainly characterized by stable chemical property, no crosslinking reaction and simultaneous disintegration of capsule shells, so that the disintegration is very timely; the water content is low, can be controlled at about 8%, reduces the risk of drug hygroscopicity, and is suitable for drugs with strong hygroscopicity and sensitive to water diversion, especially for health products and cosmetics; the dissolved medium has small influence on the capsule shell, small adhesion to esophagus and high medication compliance; the capsule is easy to store, has long effective period, does not deteriorate for 3-4 years, has low requirements on storage and transportation conditions, is not easy to be brittle in a low-humidity environment, has the brittleness of less than or equal to 20 percent in a 35 percent RH environment, is not easy to deform in a high-temperature environment, does not deform in a capsule body at 80 ℃, does not contain protein in raw materials, loses necessary conditions for the survival and the propagation of bacteria, and is not easy to rot and deteriorate; pure plant fiber, the raw material source is relatively simple, and the requirements of all cultural backgrounds and religious belief crowds are met; the safety is high, the risk of animal infectious diseases is avoided, and residual hormones, medicines and other harmful substances in animals are avoided; the production process is almost pollution-free, and the tailings can be re-dissolved and utilized for the second time; the common surfactant and plasticizer are saved, the gelling speed is accelerated only by reducing the gelling temperature through the potassium chloride-assisted gelling cold gel, the additives are reduced, the production cost is reduced, and the method is suitable for large-scale popularization.
Particularly, the addition of a proper amount of sodium alginate improves the molding property of the colloid solution, potassium salt is mixed into the hydroxypropyl methylcellulose gel solution, and the sodium alginate is mixed after the mixture is uniformly mixed, so that the problem of uneven thickness during dipping can be greatly reduced; when the solution is prepared, the gel swelling solution is added and mixed at a temperature higher than that of the hypromellose solution, and vacuum filtration and degassing are combined, so that residual fine bubbles in the solution can be thoroughly released in each step, fine bubbles on a hollow capsule body can be basically stopped, the product quality is effectively improved, and the production efficiency is improved.
Detailed Description
The present invention is further illustrated by the following examples, which are intended to illustrate the invention but not to limit it further, and should not be construed as limiting the scope of the invention.
Example 1.
The preparation method comprises the steps of taking 50kg of hydroxypropyl methylcellulose, putting into 120L of purified water with the temperature of 85 ℃, quickly stirring and uniformly mixing for 13 minutes, and then keeping the temperature of 82 ℃ for standing for 60 minutes to obtain a hydroxypropyl methylcellulose solution.
And secondly, 270g of gellan gum is taken, stirred and swelled in 120L of purified water at the temperature of 40 ℃, and then heated to 85 ℃ and kept warm and kept stand for 55min to obtain the gellan gum swelling liquid.
Thirdly, adding the gellan gum swelling solution into the hydroxypropyl methylcellulose solution at a temperature 3 ℃ higher than that of the hydroxypropyl methylcellulose solution, pouring the hydroxypropyl methylcellulose solution and the gellan gum swelling solution into the mixing kettle at the same speed when adding, starting stirring when pouring, continuously stirring and uniformly mixing for 13min after pouring, and then cooling to 75 ℃ to obtain the hydroxypropyl methylcellulose gel solution.
Fourthly, 270g of potassium chloride is added into the hydroxypropyl methylcellulose gel solution, the mixture is stirred for 2min at the speed of 900rpm, then the mixture is vacuumized, filtered, degassed for 9min, and the solution is cooled to 65 ℃ to obtain the hydroxypropyl methylcellulose potassium gel solution.
Fifthly, adding 850g of sodium alginate into the hydroxypropyl methylcellulose potassium colloid solution, continuing stirring at 900rpm for 2min, stirring, vacuumizing, filtering, degassing for 9min, and standing at 55 ℃ for 3 h to obtain the hydroxypropyl methylcellulose colloid solution with stable impregnation.
The addition of sodium alginate makes the gum solution easier to mold.
The gel solution is improved by adding the potassium chloride first and then adding the sodium alginate, but the potassium chloride and the sodium alginate cannot be added simultaneously, or the potassium chloride cannot be added by heating the sodium alginate first, otherwise, the sodium alginate is uneven in thickness during gel dipping, probably because the sodium alginate has hydrophilicity, and the gel solution can be improved by adding the potassium chloride first and then adding the sodium alginate.
Sixthly, dipping a capsule mold in hydroxypropyl methylcellulose colloidal solution to form a mold under the environment that the temperature is 40 ℃ and the relative humidity is 45%, and then drying under the environment that the temperature is 15 ℃ and the relative humidity is 30% to obtain a dried capsule rod.
And immersing the capsule rod into a hydroxypropyl methylcellulose phthalate organic solution for secondary glue dipping, forming a coating layer outside the capsule rod, and taking out and drying.
Finally, the hydroxypropyl methylcellulose enteric empty capsule is prepared by demoulding, cutting and sheathing.
When 100 hollow capsules are randomly extracted for detection, only 1 capsule containing fine bubbles and only 5 capsules with uneven thickness are found, and compared with the previous reject ratio reaching 30%, the production yield is greatly improved.
Example 2.
The preparation method comprises the steps of taking 50kg of hydroxypropyl methylcellulose, putting the hydroxypropyl methylcellulose into 125L of purified water with the temperature of 92 ℃, quickly stirring and uniformly mixing for 15 minutes, and then keeping the temperature of 85 ℃ for standing for 75min to obtain a hydroxypropyl methylcellulose solution.
And 357g of gellan gum is taken, stirred and swelled in 125L of purified water with the temperature of 42.5 ℃, and then heated to 90 ℃ and kept warm and stood for 60min to obtain the gellan gum swelling liquid.
Thirdly, adding the gellan gum swelling solution into the hydroxypropyl methylcellulose solution at a temperature 4 ℃ higher than that of the hydroxypropyl methylcellulose solution, pouring the hydroxypropyl methylcellulose solution and the gellan gum swelling solution into the mixing kettle at the same speed when adding, starting stirring when pouring, continuously stirring and uniformly mixing for 15min after pouring, and then cooling to 80 ℃ to obtain the hydroxypropyl methylcellulose gel solution.
And fourthly, adding 286g of potassium chloride into the hydroxypropyl methylcellulose gel solution, stirring at the speed of 1000rpm for 2.5min, vacuumizing, filtering, degassing for 10min, and cooling the solution to 70 ℃ to obtain the hydroxypropyl methylcellulose potassium gel solution.
And fifthly, adding 900g of sodium alginate into the hydroxypropyl methylcellulose potassium colloid solution, continuing stirring at 1000rpm for 2.5min, stirring, carrying out vacuum pumping filtration and degassing for 10min, and standing at 60 ℃ for 4 h to obtain the hydroxypropyl methylcellulose colloid solution with stable impregnation.
Sixthly, dipping a capsule mold in hydroxypropyl methylcellulose colloidal solution to form a mold under the environment that the temperature is 42.5 ℃ and the relative humidity is 50%, and then drying under the environment that the temperature is 19 ℃ and the relative humidity is 32.5% to obtain a dried capsule rod.
And immersing the capsule rod into a hydroxypropyl methylcellulose phthalate organic solution for secondary glue dipping, forming a coating layer outside the capsule rod, and taking out and drying.
Finally, the hydroxypropyl methylcellulose enteric empty capsule is prepared by demoulding, cutting and sheathing.
When 100 hollow capsules are randomly extracted for detection, fine bubble hollow capsule particles are not found, and only 2 hollow capsules with uneven thickness are found, so that the reject ratio is greatly improved compared with the previous reject ratio which reaches 30%.
When the gel is gellan gum and the sylvite is potassium chloride, the optimal weight ratio scheme of the hydroxypropyl methylcellulose, the gellan gum, the potassium chloride and the sodium alginate is as follows: 50kg, 357g, 286g and 900 g.
Example 3.
The preparation method comprises the steps of taking 50kg of hydroxypropyl methylcellulose, putting the hydroxypropyl methylcellulose into 130L of purified water with the temperature of 98 ℃, quickly stirring and uniformly mixing for 17 minutes, and then keeping the temperature and standing for 90 minutes at the temperature of 92 ℃ to obtain a hydroxypropyl methylcellulose solution.
And taking 405g of gellan gum, stirring and swelling the gellan gum in 130L of purified water at the temperature of 45 ℃, heating to 95 ℃, preserving heat and standing for 65min to obtain the gellan gum swelling liquid.
Thirdly, adding the gellan gum swelling solution into the hydroxypropyl methylcellulose solution at a temperature 5 ℃ higher than that of the hydroxypropyl methylcellulose solution, pouring the hydroxypropyl methylcellulose solution and the gellan gum swelling solution into the mixing kettle at the same speed when adding, starting stirring when pouring, continuously stirring and uniformly mixing for 17min after pouring, and then cooling to 85 ℃ to obtain the hydroxypropyl methylcellulose gel solution.
310g of potassium chloride is added into the hydroxypropyl methylcellulose gel solution, the mixture is stirred for 3min at the speed of 1100rpm, then the mixture is vacuumized, filtered and degassed for 11min, and the solution is cooled to 75 ℃ to obtain the hydroxypropyl methylcellulose potassium gel solution.
Fifthly, adding 950g of sodium alginate into the hydroxypropyl methylcellulose potassium colloid solution, continuing stirring at 1100rpm for 3min, stirring, vacuumizing, filtering, degassing for 11min, and standing at 65 ℃ for 5 hours to obtain the hydroxypropyl methylcellulose colloid solution with stable impregnation.
Sixthly, dipping a capsule mold in hydroxypropyl methylcellulose colloidal solution to form a mold under the environment that the temperature is 45 ℃ and the relative humidity is 55%, and then drying under the environment that the temperature is 23 ℃ and the relative humidity is 35% to obtain a dried capsule rod.
And immersing the capsule rod into a hydroxypropyl methylcellulose phthalate organic solution for secondary glue dipping, forming a coating layer outside the capsule rod, and taking out and drying.
Finally, the hydroxypropyl methylcellulose enteric empty capsule is prepared by demoulding, cutting and sheathing.
Example 4.
The preparation method comprises the steps of taking 50kg of hydroxypropyl methylcellulose, putting into 120L of purified water with the temperature of 87 ℃, quickly stirring and uniformly mixing for 13 minutes, and then keeping the temperature of 85 ℃ for standing for 60 minutes to obtain a hydroxypropyl methylcellulose solution.
320g of carrageenan is stirred and swelled in 120L of purified water with the temperature of 40 ℃, then the mixture is heated to 85 ℃ and kept warm and kept stand for 55min, and the carrageenan swelling liquid is obtained.
Thirdly, adding the carrageenan swelling solution into the hydroxypropyl methylcellulose solution at a temperature 3 ℃ higher than that of the hydroxypropyl methylcellulose solution, pouring the hydroxypropyl methylcellulose solution and the carrageenan swelling solution into the mixing kettle at the same speed when adding, starting stirring when pouring, continuously stirring and uniformly mixing for 13min after pouring, and then cooling to 75 ℃ to obtain the hydroxypropyl methylcellulose gel solution.
And fourthly, adding 270g of potassium carbonate into the hydroxypropyl methylcellulose gel solution, stirring at 900rpm for 2min, vacuumizing, filtering, degassing for 9min, and cooling the solution to 65 ℃ to obtain the hydroxypropyl methylcellulose potassium gel solution.
Fifthly, adding 850g of sodium alginate into the hydroxypropyl methylcellulose potassium colloid solution, continuing stirring at 900rpm for 2min, stirring, vacuumizing, filtering, degassing for 9min, and standing at 55 ℃ for 3 h to obtain the hydroxypropyl methylcellulose colloid solution with stable impregnation.
The potassium carbonate must be added firstly, then the sodium alginate is added, the potassium carbonate and the sodium alginate cannot be added simultaneously, the sodium alginate cannot be heated firstly and then the potassium carbonate cannot be added, otherwise, the situation of uneven thickness occurs in glue dipping, and the gel solution can be improved by adding the potassium carbonate firstly and then adding the sodium alginate.
Sixthly, dipping a capsule mold in hydroxypropyl methylcellulose colloidal solution to form a mold under the environment that the temperature is 40 ℃ and the relative humidity is 45%, and then drying under the environment that the temperature is 15 ℃ and the relative humidity is 30% to obtain a dried capsule rod.
And immersing the capsule rod into a hydroxypropyl methylcellulose phthalate organic solution for secondary glue dipping, forming a coating layer outside the capsule rod, and taking out and drying.
Finally, the hydroxypropyl methylcellulose enteric empty capsule is prepared by demoulding, cutting and sheathing.
When 100 hollow capsules are randomly extracted for detection, only 1 capsule containing fine bubbles and only 6 capsules with uneven thickness are found, and compared with the previous reject ratio reaching 30%, the production yield is greatly improved.
Example 5.
The preparation method comprises the steps of taking 50kg of hydroxypropyl methylcellulose, putting the hydroxypropyl methylcellulose into 125L of purified water with the temperature of 92 ℃, quickly stirring and uniformly mixing for 15 minutes, and then keeping the temperature and standing for 75min at the temperature of 88 ℃ to obtain a hydroxypropyl methylcellulose solution.
And secondly, 366g of carragheenan is stirred and swelled in 125L of purified water with the temperature of 42.5 ℃, then heated to 90 ℃, kept warm and stood for 60min, so as to obtain the gel swelling liquid.
Thirdly, adding the carrageenan swelling solution into the hydroxypropyl methylcellulose solution at a temperature 4 ℃ higher than that of the hydroxypropyl methylcellulose solution, pouring the hydroxypropyl methylcellulose solution and the carrageenan swelling solution into the mixing kettle at the same speed when adding, starting stirring when pouring, continuously stirring and uniformly mixing for 15min after pouring, and then cooling to 80 ℃ to obtain the hydroxypropyl methylcellulose gel solution.
And fourthly, adding 303g of potassium carbonate into the hydroxypropyl methylcellulose gel solution, stirring at the speed of 1000rpm for 2.5min, vacuumizing, filtering, degassing for 10min, and cooling the solution to 70 ℃ to obtain the hydroxypropyl methylcellulose potassium gel solution.
And fifthly, adding 900g of sodium alginate into the hydroxypropyl methylcellulose potassium colloid solution, continuing stirring at 1000rpm for 2.5min, stirring, carrying out vacuum pumping filtration and degassing for 10min, and standing at 60 ℃ for 4 h to obtain the hydroxypropyl methylcellulose colloid solution with stable impregnation.
Sixthly, dipping a capsule mold in hydroxypropyl methylcellulose colloidal solution to form a mold under the environment that the temperature is 42.5 ℃ and the relative humidity is 50%, and then drying under the environment that the temperature is 19 ℃ and the relative humidity is 32.5% to obtain a dried capsule rod.
And immersing the capsule rod into a hydroxypropyl methylcellulose phthalate organic solution for secondary glue dipping, forming a coating layer outside the capsule rod, and taking out and drying.
Finally, the hydroxypropyl methylcellulose enteric empty capsule is prepared by demoulding, cutting and sheathing.
When 100 hollow capsules are randomly extracted for detection, no fine bubble hollow capsule particles are found, and only 3 hollow capsules with uneven thickness are found, so that the reject ratio is greatly improved compared with the previous reject ratio which reaches 30%.
When the gelling agent is carrageenan and the sylvite is potassium carbonate, the optimal weight ratio scheme of the hydroxypropyl methylcellulose, the carrageenan, the potassium carbonate and the sodium alginate is as follows: 50kg 366g 303g 900 g.
Example 6.
The preparation method comprises the steps of taking 50kg of hydroxypropyl methylcellulose, putting the hydroxypropyl methylcellulose into 130L of purified water with the temperature of 98 ℃, quickly stirring and uniformly mixing for 17 minutes, and then keeping the temperature and standing for 90 minutes at the temperature of 92 ℃ to obtain a hydroxypropyl methylcellulose solution.
And stirring 400g of carragheenan and swelling the carragheenan in 130L of purified water at the temperature of 45 ℃, heating the carragheenan to 95 ℃, and keeping the temperature and standing for 65min to obtain the gel swelling solution.
Thirdly, adding the carrageenan swelling solution into the hydroxypropyl methylcellulose solution at a temperature 5 ℃ higher than that of the hydroxypropyl methylcellulose solution, pouring the hydroxypropyl methylcellulose solution and the carrageenan swelling solution into the mixing kettle at the same speed when adding, starting stirring when pouring, continuously stirring and uniformly mixing for 17min after pouring, and then cooling to 85 ℃ to obtain the hydroxypropyl methylcellulose gel solution.
And fourthly, adding 320g of potassium carbonate into the hydroxypropyl methylcellulose gel solution, stirring for 3min at the speed of 1100rpm, vacuumizing, filtering, degassing for 11min, and cooling the solution to 75 ℃ to obtain the hydroxypropyl methylcellulose potassium gel solution.
Fifthly, adding 950g of sodium alginate into the hydroxypropyl methylcellulose potassium colloid solution, continuing stirring at 1100rpm for 3min, stirring, vacuumizing, filtering, degassing for 11min, and standing at 65 ℃ for 5 hours to obtain the hydroxypropyl methylcellulose colloid solution with stable impregnation.
Sixthly, dipping a capsule mold in hydroxypropyl methylcellulose colloidal solution to form a mold under the environment that the temperature is 45 ℃ and the relative humidity is 55%, and then drying under the environment that the temperature is 23 ℃ and the relative humidity is 35% to obtain a dried capsule rod.
And immersing the capsule rod into a hydroxypropyl methylcellulose phthalate organic solution for secondary glue dipping, forming a coating layer outside the capsule rod, and taking out and drying.
Finally, the hydroxypropyl methylcellulose enteric empty capsule is prepared by demoulding, cutting and sheathing.
When 100 hollow capsules are randomly extracted for detection, only 1 capsule is found to contain fine bubbles, and only 5 capsules with uneven thickness are found, so that the reject ratio is greatly improved compared with the previous reject ratio which reaches about 30 percent.
And (5) effect test. The disintegration time period was measured for each example product. 10 pieces of enteric hollow capsule products produced in six examples were each tested, filled with talc powder as a content, and measured in simulated gastric juice at a temperature of (37 ± 1) ° c and a pH =1.1 for 2 hours to observe the disintegration of the capsules. In the case of no disintegration, all capsules were washed three times with purified water at the same temperature, the disintegration time was measured in simulated intestinal fluid of (37 ± 1) ° c, pH =6.8, and the time required from the start of disintegration to the complete disintegration of 30 capsules was recorded;
therefore, the enteric hollow capsule product produced by the method has good disintegration effect.
Claims (5)
1. A hydroxypropyl methylcellulose enteric empty capsule formed by gelling sylvite and sodium salt is characterized in that the preparation method comprises the following steps:
the preparation method comprises the steps of taking 50kg of hydroxypropyl methylcellulose, putting into 120-phase 130L of purified water with the temperature of 85-98 ℃, quickly stirring and uniformly mixing for 13-17 minutes, and then keeping the temperature and standing for 60-90 minutes at the temperature of 82-92 ℃ to obtain a hydroxypropyl methylcellulose solution;
405g of gel is taken, stirred and swelled in 130L of 120-grade purified water at the temperature of 40-45 ℃, then heated to 85-95 ℃, and kept warm and stood for 55-65min to obtain gel swelling liquid;
thirdly, adding the gel swelling solution into the hydroxypropyl methylcellulose solution at a temperature 3-5 ℃ higher than that of the hydroxypropyl methylcellulose solution, pouring the hydroxypropyl methylcellulose solution and the gel swelling solution into a mixing kettle at the same speed when adding, starting stirring when pouring, continuously stirring and uniformly mixing for 13-17min after pouring, and then cooling to 75-85 ℃ to obtain the hydroxypropyl methylcellulose gel solution;
fourthly, adding 270-320g of sylvite into the hydroxypropyl methylcellulose gel solution, stirring at the speed of 900-1100rpm for 2-3min, then vacuumizing, filtering, degassing for 9-11min, and cooling the solution to 65-75 ℃ to obtain a hydroxypropyl methylcellulose potassium gel solution;
adding 850-950g of sodium salt into the hydroxypropyl methylcellulose potassium glue solution, continuing stirring at the speed of 900-1100rpm for 2-3min, stirring, performing vacuum pumping filtration and degassing for 9-11min, and standing at the temperature of 55-65 ℃ for 3-5 h to obtain a stable-dipping hydroxypropyl methylcellulose colloidal solution;
sixthly, dipping a capsule mold in a hydroxypropyl methylcellulose colloidal solution to form a mold under the environment that the temperature is 40-45 ℃ and the relative humidity is 45-55%, and then drying under the environment that the temperature is 15-23 ℃ and the relative humidity is 30-35% to obtain a dried capsule rod;
immersing the capsule rod into a hydroxypropyl methylcellulose phthalate organic solution for secondary glue dipping, forming a coating layer outside the capsule rod, and taking out and drying;
finally, preparing the hydroxypropyl methylcellulose enteric empty capsule by demoulding, cutting and sheathing;
the sodium salt is sodium alginate.
2. The hypromellose enteric empty capsule gelled with a potassium salt and a sodium salt according to claim 1, characterized in that the gelling agent is a mixture of one or more of gellan gum, carrageenan, konjac gum, xanthan gum, guar gum.
3. The hypromellose enteric empty capsule gelled with potassium and sodium salts according to claim 2, characterised in that the potassium salt is a mixture of one or more of potassium chloride, potassium carbonate, potassium acetate, potassium citrate.
4. The hypromellose enteric empty capsule gelated with potassium salt and sodium salt according to claim 3, characterized in that when the gelling agent is gellan gum and the potassium salt is potassium chloride, the optimal weight ratio of hypromellose, gellan gum, potassium chloride and sodium alginate is as follows: 50kg, 357g, 286g and 900 g.
5. The hypromellose enteric empty capsule gelated with potassium salt and sodium salt according to claim 3, characterized in that when the gelling agent is carrageenan and the potassium salt is potassium carbonate, the optimal weight ratio of hypromellose, carrageenan, potassium carbonate and sodium alginate is as follows: 50kg 366g 303g 900 g.
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