CN104840447A - Preparation method of pulullan vacant capsules - Google Patents
Preparation method of pulullan vacant capsules Download PDFInfo
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- CN104840447A CN104840447A CN201510325783.5A CN201510325783A CN104840447A CN 104840447 A CN104840447 A CN 104840447A CN 201510325783 A CN201510325783 A CN 201510325783A CN 104840447 A CN104840447 A CN 104840447A
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Abstract
The invention provides a preparation method of pulullan vacant capsules, wherein pulullan vacant hard capsules comprise the following components by mass: pulullan, a thickener, a glue solution stabilizer, a plasticizer and the balance of equilibrium-amount purified water and the glue solution stabilizer is ethanol. The preparation method comprises the following steps: 1) taking pulullan in the abovementioned component amount, placing the pulullan in a vacuum glue-dissolving kettle, sequentially adding the plasticizer and the thickener, stirring until all the components are uniformly mixed, and completely dissolving to form glue solution; 2) curing at a high temperature, and vacuumizing for defoaming; 3) placing the glue solution in a heat insulation bucket with a temperature of 55-65 DEG C, and adding the glue solution stabilizer; 4) carrying out glue-dipping forming on the glue solution through a die, and preparing finished capsules. The pulullan is completely dissolved through 'high-temperature curing' during a glue-dissolving process, an appropriate amount of ethanol is added to reduce the sensitivity of the temperature changes of the glue solution, so that the viscosity of the glue solution is relatively stable, thereby facilitating forming and increasing the yield of finished products.
Description
Technical field
The present invention relates to a kind of Capsules preparation technique field, particularly a kind of take pulullan polysaccharide as Capsules of primary raw material and preparation method thereof.
Background technology
Capsules is a kind of capsule of being used widely in fields such as medicine, food, health product and cosmetics at present, and it implant is quantitatively encapsulated and forms closed capsule.Especially in medicine and health products trade, outstanding advantage is had, the shortcoming that the use of capsule solves that most medicine entrance is difficult, mouthfeel is poor etc.
The plant capsule of present stage exploitation natural origin becomes a kind of trend, and compared to traditional gelatin hollow capsule, good avoids the antigenicity risk and pollution that may be caused by animal proteinum colloid.At present, study commonplace plant source Capsules and mainly contain three classes.One class take water-soluble cellulose derivative as the capsule that primary raw material is made, and as hypromellose Capsules, but cellulose family capsule exists the defects such as the high and appearance property of disintegrate instability, oxygen transmission rate is poor.Another kind of is vegetable starch capsule, be that primary raw material is made, but technology is ripe not to the utmost by plant amylum and starch derivatives, friability difference and can not carrying liquid material.A class is also had to be take polysaccharide polymer as the capsule that primary raw material is made, particularly pulullan polysaccharide empty capsule, compare other capsules and there is significant advantage: 1) thermostability: the reflection of Powdered pulullan polysaccharide to heat is identical with starch, different from other macromolecular material, its carbonization does not produce poisonous gas; 2) oxygen transmission rate is low: the oxygen permeability of pulullan polysaccharide capsule is approximately 1/8 of gelatine capsule, is 1/300 of hypromellose cellulose capsule, can avoid oxidation by available protecting content, extend shelf life; 3) transparency is good: suitable with gelatine capsule, filling content is clearly visible; 4) storage requirement: according to test pulullan polysaccharide empty capsule friability hardly in low-humidity environment, under high temperature, softgel shell character is still stablized, large for China's north and south temperature difference, the situation that transportation and retail terminal storage condition differ, pulullan polysaccharide plant capsule provides good solution for some pharmaceutical factories and Health Products Enterprises undoubtedly.But, pulullan polysaccharide price higher and in capsule actual production process gelatin viscosity to vary with temperature impact comparatively large, be unfavorable for molding, cause product yield low.So plant capsule field is no doubt that research is popular, but the experience being applied to large-scale production is relatively weak, and gelatin hollow capsule remains main product in the market.
Summary of the invention
The object of the invention is to be to overcome defect of the prior art, plant source pulullan polysaccharide empty capsule that a kind of slaking index is stablized, friability is better, outward appearance is bright, oxygen transmission rate is low, product yield is high and preparation method thereof is provided, the formula of described Capsules is simple, pulullan polysaccharide content is higher and improve product yield by special process, reduce production cost, be of value to large-scale production.
In order to reach the object solved the problems of the technologies described above, technical scheme of the present invention is:
A kind of pulullan polysaccharide empty capsule, wherein pulullan polysaccharide empty capsule quality ratio of component is: pulullan polysaccharide 68 ~ 98%, thickening agent 0.5 ~ 5%, plasticizer 0.5 ~ 5%, and surplus is aequum purified water;
Wherein, thickening agent is one or more in Wei Lan glue, arabic gum, tamarind gum;
Plasticizer is one or more in polyethylene glycol 6000, triethyl citrate, diethyl phthalate;
Above-mentioned pulullan polysaccharide empty capsule quality ratio of component also comprises glue stabilizing agent 0.3 ~ 3%, and glue stabilizing agent is ethanol;
Above-mentioned pulullan polysaccharide empty capsule preparation method thereof comprises the steps:
1) pulullan polysaccharide of said components amount is got, be placed in vacuum colloidal sol still, add the purified water of 2 ~ 7 times of said components gross weights again, soak 0.5 ~ 2h, then control speed of agitator 30 ~ 50r/min, be heated to 65 ~ 85 DEG C, then by said components, add plasticizer, thickening agent successively, be stirred to each component mix homogeneously and dissolve formation glue completely;
2) stop stirring, high-temperature maturing 1 ~ 4h, then with the rotating speed evacuation froth breaking of 30 ~ 50r/min;
3) discharge glue, be placed in the heat-preserving container of 55 ~ 65 DEG C, add glue stabilizing agent by said components amount, insulation leaves standstill 4 ~ 8h, and obtaining viscosity is 35 ~ 65mm
2the glue of/s;
4) above-mentioned glue is dipped in gum forming through mould, under the condition of temperature 29 ~ 35 DEG C, dry 90 ~ 150min obtains compound blank, then through the demoulding, cutting, fit, sorting, packaging, i.e. obtained capsule finished product.
A kind of pulullan polysaccharide empty capsule preparation method thereof, pulullan polysaccharide empty capsule quality component is: pulullan polysaccharide, thickening agent, glue stabilizing agent and plasticizer, and surplus is aequum purified water;
Wherein above-mentioned glue stabilizing agent is ethanol;
Above-mentioned preparation method comprises the steps:
1) pulullan polysaccharide of said components amount is got, be placed in vacuum colloidal sol still, add the purified water of 2 ~ 7 times of said components gross weights again, soak 0.5 ~ 2h, then control speed of agitator 30 ~ 50r/min, be heated to 65 ~ 85 DEG C, then by said components, add plasticizer, thickening agent successively, be stirred to each component mix homogeneously and dissolve formation glue completely;
2) stop stirring, high-temperature maturing 1 ~ 4h, then with the rotating speed evacuation froth breaking of 30 ~ 50r/min;
3) discharge glue, be placed in the heat-preserving container of 55 ~ 65 DEG C, add glue stabilizing agent by said components amount, insulation leaves standstill 4 ~ 8h, and obtaining viscosity is 35 ~ 65mm
2the glue of/s;
4) above-mentioned glue is dipped in gum forming through mould, under the condition of temperature 29 ~ 35 DEG C, dry 90 ~ 150min obtains compound blank, then through the demoulding, cutting, fit, sorting, packaging, i.e. obtained capsule finished product.
Preferably, the mass ratio of described pulullan polysaccharide empty capsule quality component is: pulullan polysaccharide 68 ~ 98%;
Thickening agent 0.5 ~ 5%;
Glue stabilizing agent 0.3 ~ 3%;
Plasticizer 0.5 ~ 5%.
Preferably, thickening agent is one or more in Wei Lan glue, arabic gum, tamarind gum;
Plasticizer is one or more in polyethylene glycol 6000, triethyl citrate, diethyl phthalate.
Beneficial effect of the present invention and advantage: the preparation method of a kind of pulullan polysaccharide empty capsule provided by the invention compared with prior art, formula, technique are simple, in sol-process, make pulullan polysaccharide dissolve completely through " high-temperature maturing ", add the sensitivity that ethanol in proper amount reduces glue temperature change, make gelatin viscosity relatively stable, be conducive to molding, thus raising product yield, and glue is not filtered in the preparation process of whole Capsules, make pulullan polysaccharide content in the Capsules obtained higher; Therefore the pulullan polysaccharide empty capsule that technical scheme is obtained thus to have oxygen transmission rate low, not easily friability, slaking index is stablized, outward appearance is bright, yield advantages of higher, and on replacing gelatin capsule, be obviously better than starch capsule or cellulose family capsule as plant source, both avoided the pollution that may cause because of animal proteinum, again because of water content and oxygen transmission rate low, be more suitable for filling hygroscopicity or aldehyde-containing type medicine, pulullan polysaccharide empty capsule of the present invention has stronger synthesized competitiveness undoubtedly.
Description of the invention and application are illustrative, and not by scope restriction of the present invention in the above-described embodiments, therefore the present invention is not by the restriction of the present embodiment, and the technical scheme that any employing equivalence replacement obtains is all in the scope of protection of the invention.
Accompanying drawing explanation
Fig. 1 preparation flow figure of the present invention
Tu Zhongtuo garden represents material, and rectangle represents operation, and rhombus represents control, and arrow represents flow process.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described further.
Example 1:
Get pulullan polysaccharide 15kg, be placed in vacuum colloidal sol still, then add purified water 151kg, soak 0.5h, be then heated with stirring to 80 DEG C with the rotating speed of 50r/min, then add triethyl citrate 2.5kg, tamarind gum 2.5kg successively, each component is stirred and dissolves completely and form glue, stop stirring, high-temperature maturing 2h, again with the rotating speed evacuation froth breaking of 30r/min, then discharge glue, be placed in the heat-preserving container of 60 DEG C, add ethanol 1.5kg, insulation leaves standstill 6h, and recording gelatin viscosity is 55mm
2/ s, then dips in gum forming by glue through mould, and under the condition of 32 DEG C, dry 120min obtains compound blank, then through the demoulding, cutting, fit, sorting, packaging, i.e. obtained pulullan polysaccharide empty capsule finished product.
After testing, the water content of pulullan polysaccharide empty capsule is 11.4%, and disintegration is 6min, friability <5%, and product yield is 96%.
Example 2:
Get pulullan polysaccharide 15kg, be placed in colloidal sol still, then add purified water 32kg, soak 2h, be then heated with stirring to 85 DEG C with the rotating speed of 50r/min, then add polyethylene glycol 6000 250g, tamarind gum 100g, Wei Lan glue 150g successively, each component is stirred and dissolves completely and form glue, stop stirring, high-temperature maturing 1h, again with the rotating speed evacuation froth breaking of 30r/min, then discharge glue, be placed in the heat-preserving container of 65 DEG C, add ethanol 150g, insulation leaves standstill 6h, and recording gelatin viscosity is 59mm
2/ s, then dips in gum forming by glue through mould, and under the condition of 35 DEG C, dry 90min obtains compound blank, then through the demoulding, cutting, fit, sorting, packaging, i.e. obtained pulullan polysaccharide empty capsule finished product.
After testing, the water content of pulullan polysaccharide empty capsule is 10.6%, and disintegration is 7min, friability <5%, and product yield is 96%.
Example 3:
Get pulullan polysaccharide 15kg, be placed in colloidal sol still, then add purified water 68kg, soak 1.5h, be then heated with stirring to 65 DEG C with the rotating speed of 50r/min, then add triethyl citrate 500g, Wei Lan glue 580g, arabic gum 420g successively, each component is stirred and dissolves completely and form glue, stop stirring, high-temperature maturing 4h, more then discharge glue with the rotating speed evacuation froth breaking of 30r/min, be placed in the heat-preserving container of 55 DEG C, add ethanol 500g, insulation leaves standstill 4h, and recording gelatin viscosity is 54mm
2/ s, then dips in gum forming by glue through mould, and under the condition of 29 DEG C, dry 150min obtains compound blank, then through the demoulding, cutting, fit, sorting, packaging, i.e. obtained pulullan polysaccharide empty capsule finished product.
After testing, the water content of pulullan polysaccharide empty capsule is 11.2%, and disintegration is 6min, friability <5%, and product yield is 96%.
Example 4:
Get pulullan polysaccharide 15kg, be placed in colloidal sol still, add purified water 92kg again, soak 1h, then 75 DEG C are heated with stirring to the rotating speed of 50r/min, add diethyl phthalate 510g, polyethylene glycol 6000 490g, tamarind gum 1.5kg more successively, each component is stirred and dissolves completely and form glue, stop stirring, high-temperature maturing 2h, then glue is discharged again with the rotating speed evacuation froth breaking of 30r/min, then discharge glue, be placed in the heat-preserving container of 60 DEG C, add ethanol 750g, insulation leaves standstill 8h, and recording gelatin viscosity is 58mm
2/ s, then dips in gum forming by glue through mould, and under the condition of 32 DEG C, dry 120min obtains compound blank, then through the demoulding, cutting, fit, sorting, packaging, i.e. obtained pulullan polysaccharide empty capsule finished product.
After testing, the water content of pulullan polysaccharide empty capsule is 10.9%, and disintegration is 8min, friability <5%, and product yield is 96%.
Contrast case 1:
Get pulullan polysaccharide 15kg, be placed in vacuum colloidal sol still, then add purified water 151kg, soak 0.5h, be then heated with stirring to 80 DEG C with the rotating speed of 50r/min, then add triethyl citrate 2.5kg, tamarind gum 2.5kg successively, each component is stirred and dissolves completely and form glue, stop stirring, high-temperature maturing 2h, then with the rotating speed evacuation froth breaking of 30r/min, then glue is discharged, be placed in the heat-preserving container of 60 DEG C, insulation leaves standstill 6h, and recording gelatin viscosity is 44mm
2/ s, then dips in gum forming by glue through mould, and under the condition of 32 DEG C, dry 120min obtains compound blank, then through the demoulding, cutting, fit, sorting, packaging, i.e. obtained pulullan polysaccharide empty capsule finished product.
After testing, the water content of pulullan polysaccharide empty capsule is 11.4%, and disintegration is 6min, friability <5%, and product yield is 85%.
Contrast case 2:
Get pulullan polysaccharide 15kg, be placed in colloidal sol still, add purified water 92kg again, soak 1h, then 75 DEG C are heated with stirring to the rotating speed of 50r/min, add diethyl phthalate 510g, polyethylene glycol 6000 490g, tamarind gum 1.5kg more successively, each component is stirred and dissolves completely and form glue, stop stirring, high-temperature maturing 2h, more then discharge glue with the rotating speed evacuation froth breaking of 30r/min, then glue is discharged, be placed in the heat-preserving container of 60 DEG C, insulation leaves standstill 8h, and recording gelatin viscosity is 47mm
2/ s, then dips in gum forming by glue through mould, and under the condition of 32 DEG C, dry 120min obtains compound blank, then through the demoulding, cutting, fit, sorting, packaging, i.e. obtained pulullan polysaccharide empty capsule finished product.
After testing, the water content of pulullan polysaccharide empty capsule is 10.9%, and disintegration is 8min, friability <5%, and product yield is 87%.
The pulullan polysaccharide empty capsule that the embodiment of the present invention is made cylindrically, by can fit and sealed cap, body two to save the matter formed hard and have elastic empty pocket, utricule is bright and clean, uniform color, otch are smooth, without distortion, without foreign odor.
Claims (4)
1. a pulullan polysaccharide empty capsule, described pullulan polysaccharide hollow hard capasule mass component ratio is: pulullan polysaccharide 68 ~ 98%, thickening agent 0.5 ~ 5%, plasticizer 0.5 ~ 5%, and surplus is aequum purified water;
Wherein, described thickening agent is one or more in Wei Lan glue, arabic gum, tamarind gum;
Described plasticizer is one or more in polyethylene glycol 6000, triethyl citrate, diethyl phthalate;
It is characterized in that, described pullulan polysaccharide hollow hard capasule mass component comprises glue stabilizing agent 0.3 ~ 3% than also, and described glue stabilizing agent is ethanol;
Described pulullan polysaccharide empty capsule preparation method thereof comprises the steps:
1) pulullan polysaccharide of said components amount is got, be placed in vacuum colloidal sol still, add the purified water of 2 ~ 7 times of said components gross weights again, soak 0.5 ~ 2h, then control speed of agitator 30 ~ 50r/min, be heated to 65 ~ 85 DEG C, then by said components, add plasticizer, thickening agent successively, be stirred to each component mix homogeneously and dissolve formation glue completely;
2) stop stirring, high-temperature maturing 1 ~ 4h, then with the rotating speed evacuation froth breaking of 30 ~ 50r/min;
3) discharge glue, be placed in the heat-preserving container of 55 ~ 65 DEG C, add glue stabilizing agent by said components amount, insulation leaves standstill 4 ~ 8h, and obtaining viscosity is 35 ~ 65mm
2the glue of/s;
4) above-mentioned glue is dipped in gum forming through mould, under the condition of temperature 29 ~ 35 DEG C, dry 90 ~ 150min obtains compound blank, then through the demoulding, cutting, fit, sorting, packaging, i.e. obtained capsule finished product.
2. a pulullan polysaccharide empty capsule preparation method thereof, is characterized in that, described pullulan polysaccharide hollow hard capasule component is: pulullan polysaccharide, thickening agent, glue stabilizing agent and plasticizer, and surplus is aequum purified water;
Wherein said glue stabilizing agent is ethanol;
Described preparation method comprises the steps:
1) pulullan polysaccharide of said components amount is got, be placed in vacuum colloidal sol still, add the purified water of 2 ~ 7 times of said components gross weights again, soak 0.5 ~ 2h, then control speed of agitator 30 ~ 50r/min, be heated to 65 ~ 85 DEG C, then by said components, add plasticizer, thickening agent successively, be stirred to each component mix homogeneously and dissolve formation glue completely;
2) stop stirring, high-temperature maturing 1 ~ 4h, then with the rotating speed evacuation froth breaking of 30 ~ 50r/min;
3) discharge glue, be placed in the heat-preserving container of 55 ~ 65 DEG C, add glue stabilizing agent by said components amount, insulation leaves standstill 4 ~ 8h, and obtaining viscosity is 35 ~ 65mm
2the glue of/s;
4) above-mentioned glue is dipped in gum forming through mould, under the condition of temperature 29 ~ 35 DEG C, dry 90 ~ 150min obtains compound blank, then through the demoulding, cutting, fit, sorting, packaging, i.e. obtained capsule finished product.
3. preparation method as claimed in claim 2, it is characterized in that, the mass ratio of described pullulan polysaccharide hollow hard capasule mass component is: pulullan polysaccharide 68 ~ 98%;
Thickening agent 0.5 ~ 5%;
Glue stabilizing agent 0.3 ~ 3%;
Plasticizer 0.5 ~ 5%.
4. preparation method as claimed in claim 1 or 2, is characterized in that, described thickening agent is one or more in Wei Lan glue, arabic gum, tamarind gum;
Described plasticizer is one or more in polyethylene glycol 6000, triethyl citrate, diethyl phthalate.
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| CN201510325783.5A CN104840447A (en) | 2015-06-15 | 2015-06-15 | Preparation method of pulullan vacant capsules |
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Cited By (7)
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| CN107440036A (en) * | 2017-08-25 | 2017-12-08 | 山东禹王制药有限公司 | A kind of Halth-care composition, its preparation and preparation method for improving memory, improving eyesight |
| CN107474982A (en) * | 2017-08-08 | 2017-12-15 | 诺维信公司 | Synergy capsule |
| CN109745296A (en) * | 2017-11-02 | 2019-05-14 | 浙江华光胶囊股份有限公司 | A kind of capsule and preparation method thereof |
| CN110327852A (en) * | 2019-07-06 | 2019-10-15 | 江西奕方农业科技有限公司 | Colloidal sol equipment and its manufacturing method |
| CN112606277A (en) * | 2020-12-28 | 2021-04-06 | 江苏力凡胶囊有限公司 | Process for preparing triethyl citrate demoulding oil for hollow capsules |
| US11319566B2 (en) | 2017-04-14 | 2022-05-03 | Capsugel Belgium Nv | Process for making pullulan |
| US11576870B2 (en) | 2017-04-14 | 2023-02-14 | Capsugel Belgium Nv | Pullulan capsules |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11319566B2 (en) | 2017-04-14 | 2022-05-03 | Capsugel Belgium Nv | Process for making pullulan |
| US11576870B2 (en) | 2017-04-14 | 2023-02-14 | Capsugel Belgium Nv | Pullulan capsules |
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| CN107440036A (en) * | 2017-08-25 | 2017-12-08 | 山东禹王制药有限公司 | A kind of Halth-care composition, its preparation and preparation method for improving memory, improving eyesight |
| CN109745296A (en) * | 2017-11-02 | 2019-05-14 | 浙江华光胶囊股份有限公司 | A kind of capsule and preparation method thereof |
| CN110327852A (en) * | 2019-07-06 | 2019-10-15 | 江西奕方农业科技有限公司 | Colloidal sol equipment and its manufacturing method |
| CN110327852B (en) * | 2019-07-06 | 2022-07-12 | 江西奕方农业科技有限公司 | Sol device and method for manufacturing the same |
| CN112606277A (en) * | 2020-12-28 | 2021-04-06 | 江苏力凡胶囊有限公司 | Process for preparing triethyl citrate demoulding oil for hollow capsules |
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