CN101069677A - Pullulan polysaccharide hollow hard capasule and its preparing method - Google Patents
Pullulan polysaccharide hollow hard capasule and its preparing method Download PDFInfo
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- CN101069677A CN101069677A CNA200710028704XA CN200710028704A CN101069677A CN 101069677 A CN101069677 A CN 101069677A CN A200710028704X A CNA200710028704X A CN A200710028704XA CN 200710028704 A CN200710028704 A CN 200710028704A CN 101069677 A CN101069677 A CN 101069677A
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- hard capsule
- pulullan polysaccharide
- empty hard
- capsule
- pulullan
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Abstract
The present invention discloses a hollow hard capsule and its preparation method. It is made up by adopting prolanpolysaccharide as main body material and adding gelling agent, coagulant aids, surfactant and humectant through a certain preparation process. Said invention also provides the concrete steps of its preparation method.
Description
Technical field
The present invention relates to be used for the empty hard capsule and the manufacture method thereof of splendid attire medicine or food.
Background technology
Empty hard capsule is widely used as medicine or packaging for foodstuff carrier, mainly contains three classes at present:
One class is widely used gelatine capsule, the gelatin that skin, bone extracted by animal cooperates some plasticizers, opacifier, pigment to make, but because the influence of Animal diseases such as bovine spongiform encephalopathy, foot and mouth disease in recent years, cause the fear of people to animal product, think that there is potential safety hazard in animal proteinum, some religion to animal product also one to being resisted.In addition, gelatine capsule is relatively more responsive to the variation of temperature humidity, in not hydrolysis easily at that time of temperature humidity, and degeneration, fragmentation, therefore, gelatine capsule constantly is subjected to the refusal of each side.
Another kind of is the plant amylum capsule, cooperates certain plasticizer etc. to make by plant amylum or starch derivatives.As disclosed starch Capsules of Chinese patent prospectus CN1483393A and production technology thereof, make by components such as plant amylum or starch derivatives, plasticizer, water.The disclosed capsule of CN1623529A is made up of potato starch, carrageenan, surfactant, plasticizer.CN1739488A discloses with Konjaku plucosidopolyose through the acid hydrolysis oxidative modification, with modification or unmodified vegetable protein (comprising soybean protein, zein, wheat protein, zein), in animal gelatin or the isinglass one or both are compound to be main component, and auxiliary element such as glycerol, dodecane sulfonate is made Capsules.The disclosed Capsules of CN1895234A is with amylose, and glycerol is that primary raw material makes.CN1903157A is open to be that raw material is made the gastric solubleness Capsules with Sargassum polysaccharides glue.Open extract and the glycerol etc. by amylose or soluble starch such as corn, Rhizoma Solani tuber osi, Maninot esculenta crantz., Ipomoea batatas Lam., Rhizoma Dioscoreae of CN1931145A is made plant hollow capsule.The plant amylum capsule is to develop in recent years, and in order to the new product of alternative gelatine capsule, but technology is ripe not to the utmost, and the plant amylum capsule is crisp, and the product friability is still defective, and in addition, the plant amylum capsule can not be used for the carrying liquid material.
Also having a class is to be the hard capsule that primary raw material is made with the water-soluble cellulose derivative.Open as Chinese patent prospectus CN1418081A, CN1329478A by gelatin or the capsule made as the water-soluble cellulose derivative of hydroxypropyl emthylcellulose, plasticizer etc.Open carboxymethylcellulose calcium of CN1202102A or cross-linking sodium carboxymethyl cellulose, the capsule that gelatinized starch and crospovidone etc. is made.The open plant hard capsule of making by hydrophilic gel, water-soluble cellulose, flocculation aid of CN1292261A.The open capsule of making by gelatin or water-soluble cellulose derivative such as hydroxyprolyl-methylcellulose, plasticizer etc. of CN1646369A.CN1745745A is open by the K-carrageenan, the Capsules that cellulose derivative such as hypromellose, ethyl cellulose, hydroxypropyl cellulose, carboxymethyl cellulose, alcohols are made.Up to the present, be that the Capsules quality made of primary raw material is still unstable with the water-soluble cellulose derivative, particularly in gastrointestinal disintegrate instability, and capsule shells is separated out chemical substance behind the certain hour, and mist is sent out on the surface, yellowing occurs, and face shaping is relatively poor.
Summary of the invention
The objective of the invention is the defective that exists at above-mentioned all kinds of capsules, provide that a kind of disintegrate index is stable, friability is better, smooth surface, and empty hard capsule that can the carrying liquid material.
For achieving the above object, the present invention adopts pulullan polysaccharide as material of main part, comprises following component and percentage by weight: pulullan polysaccharide 58～96%, gel 0～10%, flocculation aid 0～2%, surfactant 0～5%, wetting agent 0～5%, surplus are aequum moisture; Described gel is one or more in carrageenan, agar, pectin, the sodium alginate; Described flocculation aid is one or more in potassium chloride, calcium chloride, potassium phosphate, the potassium citrate; Described surperficial voltinism agent is one or more in dodecyl sodium sulfate, Tween 80, the span; Described wetting agent is one or more in glycerol, dimethicone, the Oleum Ricini.
Pulullan polysaccharide English name pullulan of the present invention, Chinese also is translated into pulullan, pullulan, pullulan, general poly-polysaccharide, can be by glucidtemns, sucrose, or other saccharide direct fermentation produces, it is the extracellular polysaccharide of the mould generation of falx of sprouting, mainly with α-1, the 6-glycosidic bond constitutes the homotype polysaccharide in conjunction with maltose, and promptly glucose is pressed α-1, and the 4-glycosidic bond is combined into maltotriose, two ends are again with α-1, the 6-glycosidic bond is connected to become macromolecule polysaccharide so repeatedly with other maltotriose combination, α-1,4-glycosidic bond and α-1, the ratio of 6-glycosidic bond is 2: 1, the degree of polymerization 10～30000, molecular weight 2.0 * 10
3～5.0 * 10
6Dalton.Pulullan polysaccharide can be got with mode dehydrate such as spraying, fluid bed after sterilization, decolouring, desalination by the pulullan fermentation liquid, also can adopt organic solvent method to extract the dry thing that forms, method as Chinese patent prospectus CN1651467A introduction, after the sterilization of pulullan fermentation liquid, obtain with the drying precipitate after organic solvent decolouring, desalination and the dehydrations such as ethanol, isopropyl alcohol.The present invention can use molecular weight 2.0 * 10
3～5.0 * 10
6Pulullan polysaccharide, preferably mean molecule quantity 5.0 * 10
4～1.0 * 10
6Pulullan polysaccharide.The pulullan polysaccharide that can use mode dehydrate such as spraying, fluid bed to make, but preferably by the sedimentary dry thing of pulullan fermentation liquid after dehydration of organic solvent such as ethanol or isopropyl alcohol, decolouring and desalination.
Tween 80 of the present invention, English name Tweenum 80, chemical name: polyoxyethylene 20 sorbitan monooleate is the mixture of polyoxyethylene 20 sorbitan monooleate and the two sorbitan monooleates of fraction polyoxyethylene, main component molecular formula: C
64H
124O
26
Span of the present invention is a sorbitan fatty acid ester, and desirable span comprises: Arlacel-20 (sorbitan mono-laurate), Arlacel-40 (anhydrous sorbitol acid anhydride monopalmitate) Arlacel-60 (sorbitan monostearate), Arlacel-80 (sorbitan monooleate) or Arlacel-85 (sorbitan monooleate).
Aequum moisture of the present invention is from the hygroscopicity of component among the present invention, wherein pulullan polysaccharide, gel have more intense hygroscopicity, therefore the moisture that generally contains the balance water absorption in the finished product, variation according to ambient humidity, aequum moisture generally can account for gross weight 4～20%, select suitable humidity environment can make aequum moisture between 5～15%, this scope is that the present invention preferably stores and service condition.
Preferred ingredients of the present invention and percentage by weight are: pulullan polysaccharide 68～95%, and gel 1～8%, flocculation aid 0～2%, surfactant 0～2%, wetting agent 0～2%, surplus is an aequum moisture.
Be more preferably: pulullan polysaccharide 77～95%, gel 1～6.5%, flocculation aid 0.3～1%, surfactant 0.04～0.2%, wetting agent 0.04～0.2%, surplus is an aequum moisture.
The present invention can also contain 0.1～5% titanium dioxide makes product color occur as the food coloring of opacifier and dyeing amount.
The manufacture method of empty hard capsule of the present invention may further comprise the steps:
A. by said components and weight ratio, add weight ratio by pulullan polysaccharide and water and be 1: 1～10 pure water, be heated with stirring to 30～95 ℃, fully filter with 80～150 order defecators after the dissolving.
B. filtrate is after adjust gelatin concentration, removing bubble, on capsule manufacture equipment through dipping in glue, 20～60 ℃ of oven dry, the demoulding is cut edge, fit, check becomes empty hard capsule.
Above-mentioned steps A soaked 0.5～6 hour after also can be earlier pulullan polysaccharide being added pure water by 1: 1～10 weight ratio, was heated to 30～95 ℃ of dissolvings then, added described other component heated and stirred again and dissolved.
The weight ratio of above-mentioned pulullan polysaccharide and pure water is preferably 1: 6～and 9, the heating melting temperature is preferably to 60～90 ℃.
The empty hard capsule that the present invention makes is because the pulullan polysaccharide molecule is regular, the molecular weight excursion is little, and product quality is controlled easily, has higher gas barrier property and impact strength, quality stability is good, be difficult for crisp brokenly, the disintegrate index is stable, not facile hydrolysis, long-time placement surface is not sent out the mist jaundice, be better than plant amylum capsule or cellulose-derived composite capsule substituting on the gelatine capsule, can the splendid attire solid, oily liquids, semisolid and plaster material, extensive market prospects and practical value are arranged.
The specific embodiment
Embodiment 1
Be averaged molecular weight 200,000, by 10 kilograms of the pulullan polysaccharides that obtains after ethanol dehydration, decolouring and the desalination (containing 6wt% moisture), join in 65 kilograms of pure water, soaked 1 hour, be heated to 80 ℃ under stirring, after treating that pulullan polysaccharide all dissolves, add carrageenan 350 grams, dodecyl sodium sulfate 5 grams, glycerol 5 grams, add potassium chloride 75 grams after the dissolving again, filter with 100 order defecators after the uniform dissolution.
After removing bubble, on automatic capsule manufacture equipment through dipping in glue, 40 ℃ of drying formings, demouldings then.Through side cut, fit, check becomes transparent empty hard capsule.The empty hard capsule of making can be used as Capsules after tested, can the splendid attire solid material, and also can the fill oily liquids, semisolid or plaster material.
Embodiment 2
Be averaged molecular weight 300,000, by 10 kilograms of the pulullan polysaccharides that obtains after ethanol dehydration, decolouring and the desalination (containing 8wt% moisture), 200 gram pectin, 10 gram Arlacel-20s, 20 gram dimethicones and 40 gram potassium citrates, join in 70 kilograms of pure water, be heated to 90 ℃ under stirring, filter with 100 order defecators after the uniform dissolution.
After removing bubble, on automatic capsule manufacture equipment through dipping in glue, 40 ℃ of drying formings, the demoulding then, through cutting edge, fit, check becomes transparent empty hard capsule.The empty hard capsule of making can be used as Capsules after tested, can the splendid attire solid material, and also can the fill oily liquids, semisolid or plaster material.
Embodiment 3
Be averaged molecular weight 100,000, by 10 kilograms of the pulullan polysaccharides that obtains after ethanol dehydration, decolouring and the desalination (containing 8wt% moisture), join in 70 kilograms of pure water, stir down and be heated to 75 ℃, treat that pulullan polysaccharide all after the dissolving, adds 250 and restrains agar, 10 gram Tween 80s, 15 gram Oleum Ricini and 40 gram calcium chloride, 100 grams, 300 order titania powders, proper amount of edible coloring agent.Filter with 100 order defecators after the uniform dissolution.
After removing bubble, on automatic capsule manufacture equipment through dipping in glue, 40 ℃ of drying formings, the demoulding then, through cutting edge, fit, check becomes painted opaque empty hard capsule.The empty hard capsule of making can be used as Capsules after tested, can the splendid attire solid material, and also can the fill oily liquids, semisolid or plaster material.
Embodiment 4
Be averaged molecular weight 800,000, by 10 kilograms of the pulullan polysaccharides that obtains after ethanol dehydration, decolouring and the desalination (containing 8wt% moisture), join in 90 kilograms of pure water, stir down and be heated to 90 ℃, treat that pulullan polysaccharide all dissolves after, add sodium alginate 650 grams, dodecyl sodium sulfate 10 grams, glycerol 20 grams, the dissolving back adds potassium phosphate 100 grams, 100 grams, 300 order titania powders, the proper amount of edible coloring agent.Filter with 100 order defecators after the uniform dissolution.
After removing bubble, on automatic capsule manufacture equipment through dipping in glue, 40 ℃ of drying formings, the demoulding then, through cutting edge, fit, check becomes painted opaque empty hard capsule.The empty hard capsule of making can be used as Capsules after tested, can the splendid attire solid material, and also can the fill oily liquids, semisolid or plaster material.
Claims (10)
1. a pullulan polysaccharide hollow hard capasule is characterized in that, comprises following component and percentage by weight: pulullan polysaccharide 58～96%, and gel 0～10%, flocculation aid 0～2%, surfactant 0～5%, wetting agent 0～5%, surplus is an aequum moisture; Described gel is one or more in carrageenan, agar, pectin, the sodium alginate; Described flocculation aid is one or more in potassium chloride, calcium chloride, potassium phosphate, the potassium citrate; Described surperficial voltinism agent is one or more in dodecyl sodium sulfate, Tween 80, the span; Described wetting agent is one or more in glycerol, dimethicone, the Oleum Ricini.
2. according to the described empty hard capsule of claim 1, it is characterized in that described pulullan polysaccharide mean molecule quantity is 5.0 * 10
4～1.0 * 10
6
3. according to the described empty hard capsule of claim 1, it is characterized in that described pulullan polysaccharide is to adopt the organic solvent method precipitation to extract by the pulullan fermentation liquid to form.
4. according to the described empty hard capsule of claim 1, it is characterized in that, comprise following component and percentage by weight: pulullan polysaccharide 68～95%, gel 1～8%, flocculation aid 0～2%, surfactant 0～2%, wetting agent 0～2%, surplus are aequum moisture.
5. according to the described empty hard capsule of claim 4, it is characterized in that, comprise following component and percentage by weight: pulullan polysaccharide 77～95%, gel 1～6.5%, flocculation aid 0.3～1%, surfactant 0.04～0.2%, wetting agent 0.04～0.2%, surplus are aequum moisture.
6. according to the described empty hard capsule of claim 1, it is characterized in that, also contain the food coloring of 0.1～5% titanium dioxide and dyeing amount.
7. the manufacture method of the described empty hard capsule of the arbitrary claim of claim 1～6 is characterized in that, may further comprise the steps:
A. by described component of the arbitrary claim of claim 1～6 and weight ratio, add weight ratio by pulullan polysaccharide and water and be 1: 1～10 pure water, be heated with stirring to 30～95 ℃, fully filter with 80～150 order defecators after the dissolving.
B. filtrate is after adjust concentration, removing bubble, on capsule manufacture equipment through dipping in glue, 20～60 ℃ of dryings, the demoulding is cut edge, fit, check becomes empty hard capsule.
8. the manufacture method of the described empty hard capsule of claim 7 is characterized in that, in the described steps A, after pulullan polysaccharide adds pure water by 1: 1～10 weight ratio, soaked 0.5～6 hour, and be heated to 30～95 ℃ of dissolvings then, add described other component heated and stirred dissolving again.
9. the manufacture method of the described empty hard capsule of claim 7 is characterized in that, the weight ratio of described pulullan polysaccharide and pure water is 1: 6～9.
10. the manufacture method of the described empty hard capsule of claim 8 is characterized in that, described pulullan polysaccharide heating melting temperature is preferably to 60～90 ℃.
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|---|---|---|---|
| CNA200710028704XA CN101069677A (en) | 2007-06-15 | 2007-06-15 | Pullulan polysaccharide hollow hard capasule and its preparing method |
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|---|---|---|---|
| CNA200710028704XA CN101069677A (en) | 2007-06-15 | 2007-06-15 | Pullulan polysaccharide hollow hard capasule and its preparing method |
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| CNA200710028704XA Pending CN101069677A (en) | 2007-06-15 | 2007-06-15 | Pullulan polysaccharide hollow hard capasule and its preparing method |
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| CN102499910A (en) * | 2011-12-15 | 2012-06-20 | 山西吉呈生物技术有限公司 | Hard-shell capsule based on pullulan |
| CN101579326B (en) * | 2008-05-13 | 2012-07-18 | 金斐嘉 | Pulullan polysaccharide empty hard capsule and preparation method thereof |
| CN102805871A (en) * | 2011-06-02 | 2012-12-05 | 石法堂 | Material of soybean polysaccharide hollow capsule and production method of capsule |
| CN103070845A (en) * | 2013-01-14 | 2013-05-01 | 北京爱特康科贸有限责任公司 | Starch hollow capsule and preparation method thereof |
| CN103127519A (en) * | 2013-01-04 | 2013-06-05 | 山东大学（威海） | Sea-tangle glue capsule membrane material and manufacturing process thereof |
| CN103211782A (en) * | 2013-04-27 | 2013-07-24 | 青岛益青药用胶囊有限公司 | Empty capsule suitable for being filled with traditional Chinese medicines |
| CN103405775A (en) * | 2013-07-30 | 2013-11-27 | 浙江工业大学 | Hollow gracilaria polysaccharide capsule and preparation method thereof |
| CN103536928A (en) * | 2013-10-31 | 2014-01-29 | 海南大学 | Medicinal hollow hard capsule mainly prepared from inorganic montmorillonoid and preparation method of medicinal hollow hard capsule |
| CN103877067A (en) * | 2014-03-31 | 2014-06-25 | 江苏力凡胶囊有限公司 | Empty capsule capable of controlling disintegration time limit, and preparation method thereof |
| CN103961334A (en) * | 2014-05-22 | 2014-08-06 | 山东津美生物科技有限公司 | Pulullan hollow hard capsule and preparation method thereof |
| CN104274424A (en) * | 2014-09-05 | 2015-01-14 | 韩字光 | Plant empty capsule and manufacturing method thereof |
| CN104436204A (en) * | 2014-12-05 | 2015-03-25 | 通辽梅花生物科技有限公司 | Pullulan polysaccharide capsule and preparation process thereof |
| WO2017197774A1 (en) * | 2016-05-19 | 2017-11-23 | 江苏力凡胶囊有限公司 | Film-forming composition, soft- and hard-shelled capsule manufactured using the composition, and manufacturing method thereof |
| CN107474982A (en) * | 2017-08-08 | 2017-12-15 | 诺维信公司 | Synergy capsule |
| CN107898772A (en) * | 2017-12-21 | 2018-04-13 | 瑞昌市渝瑞实业有限公司 | Chinese yam hard capsules, production method and production line |
| CN109125284A (en) * | 2018-10-12 | 2019-01-04 | 江苏力凡胶囊有限公司 | A kind of pullulan polysaccharide hollow hard capasule and preparation method thereof |
| CN109745297A (en) * | 2017-11-07 | 2019-05-14 | 株式会社瑞兴 | Manufacture the method with the pulullan polysaccharide hard capsule of improved film properties |
| CN110123777A (en) * | 2019-06-03 | 2019-08-16 | 江苏力凡胶囊有限公司 | A kind of quickly disintegrated capsule shells based on polymalic acid |
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| CN111840248A (en) * | 2020-08-07 | 2020-10-30 | 武汉理工大学 | Konjac pullulan hollow capsule and preparation method thereof |
| CN113209040A (en) * | 2021-05-13 | 2021-08-06 | 青岛益青生物科技股份有限公司 | Pullulan hollow capsule with new formula and preparation method thereof |
| US11319566B2 (en) | 2017-04-14 | 2022-05-03 | Capsugel Belgium Nv | Process for making pullulan |
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2007
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| CN101579326B (en) * | 2008-05-13 | 2012-07-18 | 金斐嘉 | Pulullan polysaccharide empty hard capsule and preparation method thereof |
| US10568839B2 (en) | 2011-01-11 | 2020-02-25 | Capsugel Belgium Nv | Hard capsules |
| CN102805871A (en) * | 2011-06-02 | 2012-12-05 | 石法堂 | Material of soybean polysaccharide hollow capsule and production method of capsule |
| CN102805871B (en) * | 2011-06-02 | 2014-02-26 | 石法堂 | Material of soybean polysaccharide hollow capsule and production method of capsule |
| CN102499910B (en) * | 2011-12-15 | 2013-06-05 | 山西吉呈生物技术有限公司 | Hard-shell capsule based on pullulan |
| CN102499910A (en) * | 2011-12-15 | 2012-06-20 | 山西吉呈生物技术有限公司 | Hard-shell capsule based on pullulan |
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| CN103211782B (en) * | 2013-04-27 | 2015-04-08 | 青岛益青药用胶囊有限公司 | Empty capsule suitable for being filled with traditional Chinese medicines |
| CN103211782A (en) * | 2013-04-27 | 2013-07-24 | 青岛益青药用胶囊有限公司 | Empty capsule suitable for being filled with traditional Chinese medicines |
| CN103405775A (en) * | 2013-07-30 | 2013-11-27 | 浙江工业大学 | Hollow gracilaria polysaccharide capsule and preparation method thereof |
| CN103405775B (en) * | 2013-07-30 | 2015-08-05 | 浙江工业大学 | A kind of hollow gracilaria polysaccharide capsule and preparation method thereof |
| CN103536928A (en) * | 2013-10-31 | 2014-01-29 | 海南大学 | Medicinal hollow hard capsule mainly prepared from inorganic montmorillonoid and preparation method of medicinal hollow hard capsule |
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| CN103961334A (en) * | 2014-05-22 | 2014-08-06 | 山东津美生物科技有限公司 | Pulullan hollow hard capsule and preparation method thereof |
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| US11878079B2 (en) | 2017-04-14 | 2024-01-23 | Capsugel Belgium Nv | Pullulan capsules |
| US11576870B2 (en) | 2017-04-14 | 2023-02-14 | Capsugel Belgium Nv | Pullulan capsules |
| US11319566B2 (en) | 2017-04-14 | 2022-05-03 | Capsugel Belgium Nv | Process for making pullulan |
| CN107474982A (en) * | 2017-08-08 | 2017-12-15 | 诺维信公司 | Synergy capsule |
| CN109745297A (en) * | 2017-11-07 | 2019-05-14 | 株式会社瑞兴 | Manufacture the method with the pulullan polysaccharide hard capsule of improved film properties |
| CN109745297B (en) * | 2017-11-07 | 2021-03-09 | 株式会社瑞兴 | Method for manufacturing pullulan hard capsules with improved film properties |
| CN107898772A (en) * | 2017-12-21 | 2018-04-13 | 瑞昌市渝瑞实业有限公司 | Chinese yam hard capsules, production method and production line |
| CN109125284A (en) * | 2018-10-12 | 2019-01-04 | 江苏力凡胶囊有限公司 | A kind of pullulan polysaccharide hollow hard capasule and preparation method thereof |
| EP3881834A4 (en) * | 2018-10-12 | 2022-03-23 | Jiangsu Lefan Capsule Co., Ltd | Pullulan empty hard capsule and preparation method therefor |
| CN110123777A (en) * | 2019-06-03 | 2019-08-16 | 江苏力凡胶囊有限公司 | A kind of quickly disintegrated capsule shells based on polymalic acid |
| CN111840248B (en) * | 2020-08-07 | 2021-11-30 | 武汉理工大学 | Konjac pullulan hollow capsule and preparation method thereof |
| CN111840248A (en) * | 2020-08-07 | 2020-10-30 | 武汉理工大学 | Konjac pullulan hollow capsule and preparation method thereof |
| CN113209040A (en) * | 2021-05-13 | 2021-08-06 | 青岛益青生物科技股份有限公司 | Pullulan hollow capsule with new formula and preparation method thereof |
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