CN117379388A - Preparation method and application of low-gel-point low-melting-point thermal reversible gelling composition - Google Patents
Preparation method and application of low-gel-point low-melting-point thermal reversible gelling composition Download PDFInfo
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- CN117379388A CN117379388A CN202311435132.2A CN202311435132A CN117379388A CN 117379388 A CN117379388 A CN 117379388A CN 202311435132 A CN202311435132 A CN 202311435132A CN 117379388 A CN117379388 A CN 117379388A
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- 239000000203 mixture Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 230000002441 reversible effect Effects 0.000 title claims abstract description 12
- 239000000499 gel Substances 0.000 claims abstract description 55
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000000679 carrageenan Substances 0.000 claims abstract description 29
- 229920001525 carrageenan Polymers 0.000 claims abstract description 29
- 229940113118 carrageenan Drugs 0.000 claims abstract description 29
- 235000010418 carrageenan Nutrition 0.000 claims abstract description 27
- UHVMMEOXYDMDKI-JKYCWFKZSA-L zinc;1-(5-cyanopyridin-2-yl)-3-[(1s,2s)-2-(6-fluoro-2-hydroxy-3-propanoylphenyl)cyclopropyl]urea;diacetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O.CCC(=O)C1=CC=C(F)C([C@H]2[C@H](C2)NC(=O)NC=2N=CC(=CC=2)C#N)=C1O UHVMMEOXYDMDKI-JKYCWFKZSA-L 0.000 claims abstract description 27
- 239000004373 Pullulan Substances 0.000 claims abstract description 25
- 229920001218 Pullulan Polymers 0.000 claims abstract description 25
- 235000019423 pullulan Nutrition 0.000 claims abstract description 25
- 238000003825 pressing Methods 0.000 claims abstract description 23
- 239000007901 soft capsule Substances 0.000 claims abstract description 23
- 239000001814 pectin Substances 0.000 claims abstract description 21
- 235000010987 pectin Nutrition 0.000 claims abstract description 18
- 229920001277 pectin Polymers 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 15
- 235000011187 glycerol Nutrition 0.000 claims abstract description 14
- 229920001817 Agar Polymers 0.000 claims abstract description 13
- 239000008272 agar Substances 0.000 claims abstract description 13
- 235000010419 agar Nutrition 0.000 claims abstract description 13
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims abstract description 12
- 235000010356 sorbitol Nutrition 0.000 claims abstract description 12
- 239000000600 sorbitol Substances 0.000 claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 claims abstract description 11
- 239000000845 maltitol Substances 0.000 claims abstract description 9
- 235000010449 maltitol Nutrition 0.000 claims abstract description 9
- VQHSOMBJVWLPSR-WUJBLJFYSA-N maltitol Chemical compound OC[C@H](O)[C@@H](O)[C@@H]([C@H](O)CO)O[C@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O VQHSOMBJVWLPSR-WUJBLJFYSA-N 0.000 claims abstract description 9
- 229940035436 maltitol Drugs 0.000 claims abstract description 9
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 claims abstract description 7
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 claims abstract description 7
- 229930195725 Mannitol Natural products 0.000 claims abstract description 7
- 235000010355 mannitol Nutrition 0.000 claims abstract description 7
- 239000000594 mannitol Substances 0.000 claims abstract description 7
- 239000005060 rubber Substances 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims description 33
- 238000003756 stirring Methods 0.000 claims description 31
- 239000006260 foam Substances 0.000 claims description 20
- 239000004014 plasticizer Substances 0.000 claims description 19
- 238000002844 melting Methods 0.000 claims description 17
- 230000008018 melting Effects 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 238000001914 filtration Methods 0.000 claims description 14
- 238000007789 sealing Methods 0.000 claims description 9
- 239000003349 gelling agent Substances 0.000 claims description 7
- 235000013305 food Nutrition 0.000 claims description 5
- 239000007902 hard capsule Substances 0.000 claims description 5
- 230000009435 amidation Effects 0.000 claims description 4
- 238000007112 amidation reaction Methods 0.000 claims description 4
- 238000005192 partition Methods 0.000 claims description 4
- PYMYPHUHKUWMLA-UHFFFAOYSA-N 2,3,4,5-tetrahydroxypentanal Chemical compound OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 claims description 3
- 235000019824 amidated pectin Nutrition 0.000 claims description 3
- 108010010803 Gelatin Proteins 0.000 abstract description 22
- 239000008273 gelatin Substances 0.000 abstract description 22
- 229920000159 gelatin Polymers 0.000 abstract description 22
- 235000019322 gelatine Nutrition 0.000 abstract description 22
- 235000011852 gelatine desserts Nutrition 0.000 abstract description 22
- 239000002775 capsule Substances 0.000 abstract description 11
- 239000000243 solution Substances 0.000 abstract description 11
- 239000001257 hydrogen Substances 0.000 abstract description 8
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 8
- 239000007864 aqueous solution Substances 0.000 abstract description 4
- 239000000084 colloidal system Substances 0.000 abstract description 4
- 150000004676 glycans Chemical class 0.000 abstract description 2
- 229920001282 polysaccharide Polymers 0.000 abstract description 2
- 239000005017 polysaccharide Substances 0.000 abstract description 2
- 239000003292 glue Substances 0.000 description 11
- 241000196324 Embryophyta Species 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 229920002472 Starch Polymers 0.000 description 5
- 238000001125 extrusion Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 239000008107 starch Substances 0.000 description 5
- 235000019698 starch Nutrition 0.000 description 5
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 3
- 235000017491 Bambusa tulda Nutrition 0.000 description 3
- 241001330002 Bambuseae Species 0.000 description 3
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 3
- 239000011425 bamboo Substances 0.000 description 3
- 230000003325 follicular Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000001341 hydroxy propyl starch Substances 0.000 description 3
- 235000013828 hydroxypropyl starch Nutrition 0.000 description 3
- OWEGMIWEEQEYGQ-UHFFFAOYSA-N 100676-05-9 Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC2C(OC(O)C(O)C2O)CO)O1 OWEGMIWEEQEYGQ-UHFFFAOYSA-N 0.000 description 2
- 229920002261 Corn starch Polymers 0.000 description 2
- 229920002148 Gellan gum Polymers 0.000 description 2
- GUBGYTABKSRVRQ-PICCSMPSSA-N Maltose Natural products O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@@H](CO)OC(O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-PICCSMPSSA-N 0.000 description 2
- 229920000881 Modified starch Polymers 0.000 description 2
- 230000001464 adherent effect Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000008120 corn starch Substances 0.000 description 2
- 235000010492 gellan gum Nutrition 0.000 description 2
- 239000000216 gellan gum Substances 0.000 description 2
- 230000009290 primary effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000011257 shell material Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 description 1
- 241000251468 Actinopterygii Species 0.000 description 1
- 241000283690 Bos taurus Species 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 239000004368 Modified starch Substances 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 241001494479 Pecora Species 0.000 description 1
- 241000282898 Sus scrofa Species 0.000 description 1
- 241001464837 Viridiplantae Species 0.000 description 1
- ZNOZWUKQPJXOIG-XSBHQQIPSA-L [(2r,3s,4r,5r,6s)-6-[[(1r,3s,4r,5r,8s)-3,4-dihydroxy-2,6-dioxabicyclo[3.2.1]octan-8-yl]oxy]-4-[[(1r,3r,4r,5r,8s)-8-[(2s,3r,4r,5r,6r)-3,4-dihydroxy-6-(hydroxymethyl)-5-sulfonatooxyoxan-2-yl]oxy-4-hydroxy-2,6-dioxabicyclo[3.2.1]octan-3-yl]oxy]-5-hydroxy-2-( Chemical compound O[C@@H]1[C@@H](O)[C@@H](OS([O-])(=O)=O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H]2OC[C@H]1O[C@H](O[C@H]1[C@H]([C@@H](CO)O[C@@H](O[C@@H]3[C@@H]4OC[C@H]3O[C@H](O)[C@@H]4O)[C@@H]1O)OS([O-])(=O)=O)[C@@H]2O ZNOZWUKQPJXOIG-XSBHQQIPSA-L 0.000 description 1
- 239000002313 adhesive film Substances 0.000 description 1
- 235000021120 animal protein Nutrition 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 239000000337 buffer salt Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 210000002808 connective tissue Anatomy 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 description 1
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 description 1
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 description 1
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- -1 maltose Alcohols Chemical class 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 235000019426 modified starch Nutrition 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 235000010413 sodium alginate Nutrition 0.000 description 1
- 239000000661 sodium alginate Substances 0.000 description 1
- 229940005550 sodium alginate Drugs 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/4816—Wall or shell material
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
- A23P10/00—Shaping or working of foodstuffs characterised by the products
- A23P10/30—Encapsulation of particles, e.g. foodstuff additives
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/06—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
- A61K47/08—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite containing oxygen, e.g. ethers, acetals, ketones, quinones, aldehydes, peroxides
- A61K47/10—Alcohols; Phenols; Salts thereof, e.g. glycerol; Polyethylene glycols [PEG]; Poloxamers; PEG/POE alkyl ethers
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/06—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
- A61K47/26—Carbohydrates, e.g. sugar alcohols, amino sugars, nucleic acids, mono-, di- or oligo-saccharides; Derivatives thereof, e.g. polysorbates, sorbitan fatty acid esters or glycyrrhizin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
- A61K47/36—Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
- B01D19/0042—Degasification of liquids modifying the liquid flow
- B01D19/0052—Degasification of liquids modifying the liquid flow in rotating vessels, vessels containing movable parts or in which centrifugal movement is caused
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F29/00—Mixers with rotating receptacles
- B01F29/60—Mixers with rotating receptacles rotating about a horizontal or inclined axis, e.g. drum mixers
- B01F29/63—Mixers with rotating receptacles rotating about a horizontal or inclined axis, e.g. drum mixers with fixed bars, i.e. stationary, or fixed on the receptacle
Landscapes
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Medicinal Chemistry (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Molecular Biology (AREA)
- Biochemistry (AREA)
- Inorganic Chemistry (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Jellies, Jams, And Syrups (AREA)
Abstract
The invention relates to a preparation method and application of a low-gel-point low-melting-point thermal reversible gel composition, which uses pullulan polysaccharide to crosslink with pectin, carrageenan, agar and other colloids through a large number of hydrogen bonds in aqueous solution to generate a compact network structure, and if sorbitol, maltitol, mannitol and glycerol are added simultaneously to blend into a film, more intermolecular hydrogen bonds can be generated, the mechanical properties of the film are enhanced, and the low-gel-point low-melting-point thermal reversible gel composition is finally formed. The gel composition is very similar to gelatin solution formed by gelatin, and can replace gelatin without replacing soft capsule production equipment. And because the system has good thermal reversibility, the residual rubber in the capsule pressing process can be recycled, thereby reducing the production cost and improving the utilization rate of resources.
Description
Technical Field
The invention relates to a preparation method and application of a gel composition, in particular to a preparation method and application of a low-gel-point low-melting-point thermo-reversible gel composition applied to the field of gel compositions.
Background
At present, the soft capsule is mainly prepared from gelatin serving as a raw material, glycerol serving as a plasticizer and water serving as a solvent. Gelatin is an animal protein component extracted from connective tissue such as skin and bone of pig, cattle, sheep and fish, and the product prepared from the gelatin belongs to animal-derived capsules. Based on the innovation of the market and the rise of new generation consumers, natural, healthy and green plant-based soft capsules start to become the future development trend of the market.
The existing plant soft capsule scheme for replacing the gelatin system basically takes modified starch, hydroxypropyl methyl cellulose, gellan gum, sodium alginate, carrageenan and the like as a gel.
Application number 201080069480.7 provides a film-forming composition for soft capsules, comprising an acid-decomposed waxy corn starch, a gelling agent, a plasticizer, and the like, for preparing a film-forming composition for soft capsules. Film-forming compositions for preparing soft capsules are provided which comprise predominantly non-gelatin components wherein the gelling agent is iota carrageenan.
Application No. 201580053770.5 provides a plant-based soft capsule film and a soft capsule which have high film strength and good adhesiveness and can provide excellent film properties. The soft capsule coating contains iota-carrageenan and waxy corn starch which is subjected to damp-heat treatment in the presence of salt.
Application number 201610437197.4 discloses a plant capsule shell material, a soft capsule, a preparation method and application thereof. The plant capsule shell material comprises the following components in parts by weight: 30-80 parts of modified corn starch, 0.03-10 parts of thickening agent, 5-20 parts of film forming agent, 0.05-15 parts of plasticizer, 10-42 parts of glycerol and 50-150 parts of pure water.
The scheme commonly applied in the market at present has the following characteristics: 1. the viscosity of the glue solution is large, and the viscosity of the starch carrageenan system is about 10 times of that of the gelatin system; 2. the gel point of the glue solution is high, the gel point of the starch carrageenan system glue solution is more than 80 ℃, and the gel point of the gelatin system is only about 40 ℃; therefore, in the production of soft capsules, conventional plant soft capsules require specially designed equipment to accommodate the high viscosity and high gel point requirements of plant soft capsules. And the characteristics of high viscosity and high gel point can cause the defects that the glue solution is easy to gel to block a pipeline, the film forming property is poor, the glue skin is difficult to stitch and the like. Meanwhile, due to the characteristics of the starch, the gel prepared by taking the starch as a raw material has thermal irreversibility and can only be used once, so that about 40% of residual rubber in the capsule pressing process cannot be reused, the cost is increased, and the source waste is caused.
Disclosure of Invention
Aiming at the prior art, the technical problems to be solved by the invention are that the gel is generally high in viscosity, high in gel point, irreversible in heat, easy to cause pipeline blockage, poor in film forming property, and easy to waste, and the residual gel cannot be reused.
In order to solve the problems, the invention provides a preparation method of a low-gel-point low-melting-point thermoreversible gelling composition, which comprises at least one of a gelling agent, a plasticizer and water as main components, wherein the gelling agent, the plasticizer and the water are mixed according to volume ratio: and (3) a plasticizer: water = 100:20-60:70-170, wherein the gel is at least one of pullulan, pectin, carrageenan and agar, and the plasticizer is at least one of sorbitol, maltitol, mannitol and glycerol;
the preparation method of the gel composition comprises the following steps:
s1, primarily dispersing a gel and a plasticizer in water according to the proportion, and then adding the primarily dispersed materials into eccentric stirring equipment;
s2, controlling the eccentric stirring equipment to be in a micro-negative pressure state at the temperature of 70-95 ℃, firstly stirring the materials for the first time to dissolve the materials, then stirring the materials for the second time after dissolving to realize defoaming of the materials, and obtaining the low-gel-point low-melting-point thermal reversible gelling composition after defoaming, wherein the gel point of the gelling composition is 35-55 ℃ and the melting point is 40-60 ℃ after detecting.
In the preparation method of the low-gel-point low-melting-point thermal reversible gel composition, pullulan polysaccharide is crosslinked with pectin, carrageenan, agar and other colloids through a large number of hydrogen bonds in aqueous solution to generate a compact network structure, if sorbitol, maltitol, mannitol and glycerol are simultaneously added to blend into a film, more intermolecular hydrogen bonds can be generated, the mechanical properties of the film are enhanced, and finally the low-gel-point low-melting-point thermal reversible gel composition is formed.
As a further improvement of the present application, the pullulan has a viscosity of 80-180 mm2/s, preferably, an oxidatively modified pullulan; the pectin is amidated pectin, and the amidation degree is 1-25%. Preferably, the amidation degree is 19-25%; the carrageenan is kappa-carrageenan, iota-carrageenan or mixed carrageenan.
As a further improvement of the application, the speed of the first stirring in the step S2 is 5-10 times of the speed of the second stirring, and the speed of the second stirring is 3-5r/min.
As a further improvement of this application, eccentric agitated vessel includes urceolus, urceolus upper end fixedly connected with inlet pipe and blast pipe, and sealing door is installed to urceolus middle part lower extreme, urceolus lower extreme fixedly connected with two extension boards, urceolus right-hand member fixedly connected with motor, urceolus are equipped with the adherence eccentric section of thick bamboo, fixedly connected with eccentric pivot on the adherence eccentric section of thick bamboo, motor output shaft activity run through the urceolus and with eccentric pivot fixed connection.
As a further improvement of the application, the eccentric rotating shaft fixedly penetrates through the left end and the right end of the wall-attached eccentric cylinder, a short filter bubble sheet and a long filter bubble sheet are fixedly connected between the eccentric rotating shaft and the inner wall of the wall-attached eccentric cylinder respectively, the same side end faces of the short filter bubble sheet and the long filter bubble sheet are located on the same plane, and the length of the long filter bubble sheet is 1.5-3 times that of the short filter bubble sheet.
As the further improvement of this application, all open on adherence eccentric section of thick bamboo, short follicular piece and the long follicular piece and have a plurality of evenly distributed's pressure cell, and the both ends oral area internal diameter of pressure cell is all greater than the middle part internal diameter.
As another improvement of the application, the eccentric rotating shaft is fixed with the end part of the wall-attached eccentric cylinder, a bubble pressing assembly is fixedly connected between the middle parts of the left and right inner walls of the wall-attached eccentric cylinder, the bubble pressing assembly comprises a positive shaft positioned in the middle, two pairs of sealing partition plates which are fixed with the positive shaft and are vertically symmetrical, and a bubble pressing positive plate which is rotationally connected to the positive shaft through an electric rotating shaft, and two blades of the bubble pressing positive plate are symmetrical about the center of the positive shaft.
The low-gel-point low-melting-point thermo-reversible gelling composition is mainly applied to the manufacture of food rubber, soft capsules and hard capsules.
In summary, pullulan is crosslinked with pectin, carrageenan, agar and other colloids through a large number of hydrogen bonds in aqueous solution to generate a compact network structure, if sorbitol, maltitol, mannitol and glycerol are added simultaneously to blend into a film, more intermolecular hydrogen bonds can be generated, the mechanical properties of the film are enhanced, and finally the low gel point, low melting point and thermal reversible gelling composition is formed. The gel composition is very similar to gelatin solution formed by gelatin, and can replace gelatin without replacing soft capsule production equipment. And because the system has good thermal reversibility, the residual rubber in the capsule pressing process can be recycled, thereby reducing the production cost and improving the utilization rate of resources.
Drawings
FIG. 1 is a diagram showing the proportions of the main components of a gelling composition according to a first embodiment of the present application;
FIG. 2 is a perspective view of an eccentric stirring device according to a first embodiment of the present application;
FIG. 3 is a perspective view of a portion of an eccentric stirring device according to a first embodiment of the present application;
FIG. 4 is a radial cross-sectional view of an eccentric stirring device according to a first embodiment of the present application;
FIG. 5 is a schematic illustration of a defoaming baffle of a first embodiment of the present application;
FIG. 6 is a cross-sectional view of an adherent eccentric cartridge according to a first embodiment of the present application;
FIG. 7 is a schematic view of the track of the attaching eccentric cylinder in the first embodiment of the present application when the attaching eccentric cylinder rotates in the outer cylinder;
FIG. 8 is a schematic view of an attaching eccentric cylinder in a first embodiment of the present application when the attaching eccentric cylinder rotates in an outer cylinder;
fig. 9 is a cross-sectional view of a second embodiment of the present application.
The reference numerals in the figures illustrate:
1 outer cylinder, 101 sealing door, 2 motor, 3 support plates, 41 feeding pipe, 42 exhaust pipe, 5 adherence eccentric cylinder, 501 press hole, 6 eccentric rotating shaft, 61 short filter bubble sheet, 62 long filter bubble sheet, 71 sealing baffle, 72 press bubble positive plate, 73 positive shaft.
Detailed Description
Two embodiments of the present application are described in detail below with reference to the accompanying drawings.
First embodiment:
the preparation method of the low-gel-point low-melting-point thermoreversible gelling composition comprises the following main components of at least one of a gelling agent, a plasticizer and water, wherein the gelling composition shown in fig. 1 comprises the following components in volume: and (3) a plasticizer: water = 100:20-60:70-170, preferably in the proportion of gelling agent: and (3) a plasticizer: water = 100:25-45:80-150. Wherein the gel is at least one of pullulan, pectin, carrageenan and agar, and the plasticizer is at least one of sorbitol, maltitol, mannitol and glycerol;
the viscosity of the pullulan is 80-180 mm < 2 >/s (detected according to the standard GB 28402-2012), and the pullulan is preferably oxidized modified pullulan; the pectin is amidated pectin and has an amidation degree of 1-25% (according to standard GB 25533-2010), preferably 19-25%; the carrageenan is kappa-type carrageenan or iota-type carrageenan or kappa 2-type mixed carrageenan.
Notably, pullulan/(pullulan+pectin+carrageenan+agar) =51-99% in the gel. The preferred ratio is pullulan/(pullulan+pectin+carrageenan+agar) =70-95%.
The preparation method of the gel composition comprises the following steps:
s1, primarily dispersing a gel and a plasticizer in water according to the proportion, and then adding the primarily dispersed materials into eccentric stirring equipment;
s2, controlling the eccentric stirring equipment to be in a micro-negative pressure state at the temperature of 70-95 ℃, firstly stirring the materials for the first time to dissolve the materials, and then stirring the materials for the second time after dissolving to realize defoaming of the materials, so that the low-gel-point low-melting-point thermoreversible gelling composition is obtained after defoaming.
Specifically, according to the above ratio range and the preparation method, different proportions are selected for preparation, and the specific proportions are as follows:
| sample numbering | Design principle | The proportion of the rubber powder: pullulan/(pullulan+pectin+card) Pulling glue + agar) | Plasticizer amount | Water volume |
| Sample 1 | Sample No. 1 (hydroxypropyl starch + carrageenan) | 100 | 36 glycerin | 130 |
| Sample 2 | Sample No. 2 (hydroxypropyl starch+hydroxypropyl starch two) Starch phosphate + gellan gum) | 100 | 36 sorbitol | 130 |
| Sample 3 | Counter example of common pullulan 3 | 100 | 36 sorbitol | 130 |
| Sample 4 | General pullulan+pectin HSC200 upper limit | 100（95%） | 20 maltitol | 170 |
| Sample 5 | Ordinary pullulan+pectin HSC220+carrageenan Median position of Ka120E+ agar QS10X | 100 (91%) | 50 glycerol+maltitol | 140 |
| Sample 6 | Oxidized pullulan + carrageenan IA100deg.G + pectin HSC220+ agar QS10X optima | 100(85%) | 36 glycerin+sorbitol | 90 |
| Sample 7 | Oxidized pullulan+pectin hsc200+carrageenan BLK8120 | 100 (89%) | 45 sorbitol + maltose Alcohols | 100 |
| Sample 8 | Oxidized pullulan pectin hsc200+ card Lower limit of Lajiao IA100deg.G+agar QS10X | 100 (49%) | 60 sorbitol + maltose Alcohol + glycerol | 70 |
| Sample 9 | Gelatin control | 100 | 36/Glycerol | 90 |
By comparing the above proportions, the gel composition has the following results of the gum viscosity and the gel temperature:
| sample numbering | Glue solution viscosity (mPa.s) | Gel point (. Degree. C.) | Melting point |
| Sample 1 | 420,726 | 85.1 | NA* |
| Sample 2 | 376,200 | 80.3 | NA* |
| Sample 3 | 2,909 | NA** | NA** |
| Sample 4 | 5,269 | 37.3 | 40.7 |
| Sample 5 | 70,100 | 45.2 | 48.3 |
| Sample 6 | 8,862 | 36.1 | 39.2 |
| Sample 7 | 10,523 | 43.2 | 47.5 |
| Sample 8 | 108,793 | 54.9 | 59.3 |
| Sample 9 | 5,134 | 35.6 | 39.4 |
The low gel point and low melting point thermal reversible gel composition is mainly applied to the manufacture of food adhesive films, soft capsules and hard capsules, wherein the preparation method of the capsules is as follows: according to the formula, the thickening gel, the plasticizer, the film forming agent, the buffer salt and the water are weighed, the materials are put into a material dissolving tank, the materials are stirred and dissolved at 70-95 ℃, then the glue solution is obtained by vacuum defoaming, a soft capsule machine is used for preparing a film skin, the thickness of the film skin is 1mm, and food glue films, soft capsules and hard capsules can be manufactured according to the film skin.
According to the data, the gel composition is very similar to the gelatin solution formed by gelatin, has good thermal reversibility, can recycle the residual gelatin skin in the capsule pressing process, and can be used for food gelatin skin, capsule materials of soft capsules, hard capsules and the like. The capsule device can be designed based on a gelatin system for production, thereby reducing the device cost of the plant-based soft capsule.
The specific preparation modes of the melting point and the gel point are as follows:
the prepared membrane is placed under a clamp, the clamp is a 40mm parallel plate with the interval of 1mm, pre-balanced for 5 minutes after sample loading, 0.5% of frequency 1 Rad/S is applied, the temperature is increased from 25 ℃ to 95 ℃, the heating rate is 1 ℃/min, and dynamic viscoelasticity temperature scanning is adopted to detect gel points. Then the temperature is increased from 25 ℃ to 95 ℃ at a heating rate of 1 ℃/min, dynamic viscoelasticity temperature scanning is adopted to detect the melting point, the gel point of the gel composition is detected to be 35-55 ℃, and the melting point is detected to be 40-60 ℃.
The speed of the first stirring in the step S2 is 5-10 times of the speed of the second stirring, the speed of the second stirring is 3-5r/min, the primary effect of the first stirring is mixing, and the primary effect of the second stirring is auxiliary defoaming, so that the stirring speed can be properly reduced, the high-temperature effect is matched, the air bubbles which expand and become large during stirring are continuously subjected to the physical extrusion effect, and the two-way effect effectively accelerates the breakage of the air bubbles, so that the defoaming effect is achieved.
As shown in fig. 2-3, the eccentric stirring device comprises an outer cylinder 1, wherein the upper end of the outer cylinder 1 is fixedly connected with a feed pipe 41 and an exhaust pipe 42, the lower end of the middle part of the outer cylinder 1 is provided with a sealing door 101, the lower end of the outer cylinder 1 is fixedly connected with two support plates 3, the right end of the outer cylinder 1 is fixedly provided with a motor 2, the outer cylinder 1 is provided with an adherence eccentric cylinder 5, the adherence eccentric cylinder 5 is in contact with the inner wall of the outer cylinder 1, the adherence eccentric cylinder 5 is fixedly connected with an eccentric rotating shaft 6, the output shaft of the motor 2 movably penetrates through the outer cylinder 1 and is fixedly connected with the eccentric rotating shaft 6, and when stirring, the exhaust pipe 42 can be connected with an external air extractor to form micro negative pressure in the outer cylinder 1, so that bubbles are convenient to overflow after being broken, and the situation that big bubbles are difficult to be discharged outside in glue liquid with large viscosity after being broken into small bubbles is effectively avoided.
In addition, as shown in fig. 7, a shows a track when the adherence eccentric cylinder 5 is in adherence rotation, because the adherence eccentric cylinder 5 is eccentrically arranged with the outer cylinder 1, when the adherence eccentric cylinder 5 is in contact with the outer cylinder 1 during rotation, the adherence eccentric cylinder 5 is always in contact with the outer cylinder 1 during rotation, when the adherence eccentric cylinder rotates to the lower side, extrusion force can be generated on part of materials, part of the materials are forced to penetrate through the extrusion holes 501 into the adherence eccentric cylinder 5, the materials are forced to be extruded, the breakage of bubbles is facilitated, the defoaming efficiency is accelerated, as shown in fig. 8, when the adherence eccentric cylinder 5 is rotated to the inclined state of the short filtering foam piece 61 and the long filtering foam piece 62, part of the materials are forced to penetrate through the extrusion holes 501 again due to gravity during the inclination, the materials continuously penetrate through the extrusion holes 501 for a plurality of times during defoaming, the materials are continuously extruded, and the materials are matched with high positions and micro negative pressure, so that the outer discharge of the bubbles is effectively accelerated.
As shown in fig. 4-5, the eccentric rotating shaft 6 fixedly penetrates through the left end and the right end of the wall-attached eccentric cylinder 5, a short filter bubble piece 61 and a long filter bubble piece 62 are fixedly connected between the eccentric rotating shaft 6 and the inner wall of the wall-attached eccentric cylinder 5 respectively, the end faces of the same sides of the short filter bubble piece 61 and the long filter bubble piece 62 are positioned on the same plane, and the length of the long filter bubble piece 62 is 1.5-3 times of the length of the short filter bubble piece 61, so that the short filter bubble piece 61 and the long filter bubble piece 62 adapt to eccentric rotation of the wall-attached eccentric cylinder 5, and the defoaming effect on materials is better.
As shown in figure 6, a plurality of uniformly distributed foam pressing holes 501 are formed in the wall-attached eccentric cylinder 5, the short foam filtering sheet 61 and the long foam filtering sheet 62, and the inner diameters of the two end opening parts of the foam pressing holes 501 are larger than the inner diameter of the middle part, so that when the wall-attached eccentric cylinder 5, the short foam filtering sheet 61 and the long foam filtering sheet 62 are forced to pass through the foam pressing holes 501 in the rotating process, the inner diameter difference is extruded, and under the action of high temperature, the air bubbles in the materials are enlarged, and when the air bubbles are extruded in the positions passing through the foam pressing holes 501, the air bubbles are broken, and compared with the prior art, the air bubbles are broken fast, the defoaming speed is improved, and the preparation efficiency of the gel composition is further effectively accelerated
In summary, pullulan is crosslinked with pectin, carrageenan, agar and other colloids through a large number of hydrogen bonds in aqueous solution to generate a compact network structure, if sorbitol, maltitol, mannitol and glycerol are added simultaneously to blend into a film, more intermolecular hydrogen bonds can be generated, the mechanical properties of the film are enhanced, and finally the low gel point, low melting point and thermal reversible gelling composition is formed. The gel composition is very similar to gelatin solution formed by gelatin, and can replace gelatin without replacing soft capsule production equipment. And because the system has good thermal reversibility, the residual rubber in the capsule pressing process can be recycled, thereby reducing the production cost and improving the utilization rate of resources.
Second embodiment:
fig. 9 shows that the eccentric rotating shaft 6 is fixed only with the end of the attached eccentric cylinder 5, a bubble pressing assembly is fixedly connected between the middle parts of the left and right inner walls of the attached eccentric cylinder 5, the bubble pressing assembly comprises a positive shaft 73 positioned in the middle, two pairs of sealing partition plates 71 which are fixed with the positive shaft 73 and are vertically symmetrical, and a bubble pressing positive plate 72 which is connected to the positive shaft 73 through the rotation of the electric rotating shaft, wherein two blades of the bubble pressing positive plate 72 are centrally symmetrical with respect to the positive shaft 73.
It is noted that, each pair of sealing partition plates 71 and the wall-attached eccentric cylinder 5 enclose a liquid level compensation space, and the wall-attached eccentric cylinder 5 of the mirror is not provided with a pressure bubble 501 in the compensation space, so that the compensation space is sealed, no material is in or out, when one of the compensation spaces is located right below, part of the material can be discharged, so that the liquid level of the material is higher at this time, and when the compensation space is located at or near the middle part along with rotation, the bottom is more of the wall-attached eccentric cylinder 5 provided with the pressure bubble 501, more glue solution can enter the wall-attached eccentric cylinder 5, so that the liquid level of the material is relatively lower, and a larger liquid level difference can be presented between different positions, so that when the material is extruded by the pressure bubble positive plate 72 and discharged out of the wall-attached eccentric cylinder 5, a higher falling space is provided, or a longer moving path is provided, so that the bubbles are better cut, broken and defoaming is facilitated.
In the present embodiment, the short and long follicular sheets 61 and 62 in the first embodiment are replaced by the above-described structure inside the adherent eccentric cylinder 5, and the remaining portions remain the same as in the first embodiment.
The scope of protection of the above-described embodiments employed in the present application is not limited to the above-described embodiments, and various changes made by those skilled in the art without departing from the spirit of the present application are still within the scope of protection of the present invention.
Claims (8)
1. A method for preparing a low gel point and low melting point thermal reversible gelling composition, which is characterized in that: the main components of the gelling composition are at least one of a gelling agent, a plasticizer and water, and the gelling composition comprises the following components in volume ratio: and (3) a plasticizer: water = 100:20-60:70-170, wherein the gel is at least one of pullulan, pectin, carrageenan and agar, and the plasticizer is at least one of sorbitol, maltitol, mannitol and glycerol;
the preparation method of the gelling composition comprises the following steps:
s1, primarily dispersing a gel and a plasticizer in water according to the proportion, and then adding the primarily dispersed materials into eccentric stirring equipment;
s2, controlling the eccentric stirring equipment to be in a micro-negative pressure state at the temperature of 70-95 ℃, firstly stirring the materials for the first time to dissolve the materials, then stirring the materials for the second time after dissolving to realize defoaming of the materials, and obtaining the low-gel-point low-melting-point thermal reversible gelling composition after defoaming, wherein the gel point of the gelling composition is 35-55 ℃ and the melting point is 40-60 ℃ after detecting.
2. The method for preparing the low gel point and low melting point thermoreversible gelling composition according to claim 1, wherein the method comprises the following steps: the viscosity of the pullulan is 80-180 mm < 2 >/s; the pectin is amidated pectin, and the amidation degree is 1-25%; the carrageenan is kappa-type carrageenan or iota-type carrageenan or mixed carrageenan.
3. The method for preparing the low gel point and low melting point thermoreversible gelling composition according to claim 1, wherein the method comprises the following steps: the speed of the first stirring in the step S2 is 5-10 times of the speed of the second stirring, and the speed of the second stirring is 3-5r/min.
4. A method of preparing a low gel point and low melting point thermoreversible gelling composition according to claim 3, wherein: the eccentric stirring equipment comprises an outer cylinder (1), wherein the upper end of the outer cylinder (1) is fixedly connected with a feeding pipe (41) and an exhaust pipe (42), a sealing door (101) is arranged at the lower end of the middle part of the outer cylinder (1), two support plates (3) are fixedly connected with the lower end of the outer cylinder (1), a motor (2) is fixedly arranged at the right end of the outer cylinder (1), an adherence eccentric cylinder (5) is arranged on the outer cylinder (1), an adherence eccentric rotating shaft (6) is fixedly connected to the adherence eccentric cylinder (5), and an output shaft of the motor (2) movably penetrates through the outer cylinder (1) and is fixedly connected with the eccentric rotating shaft (6).
5. The method for preparing a low gel point and low melting point thermoreversible gelling composition according to claim 4, wherein: the eccentric rotating shaft (6) fixedly penetrates through the left end and the right end of the adherence eccentric cylinder (5), a short filtering foam piece (61) and a long filtering foam piece (62) are fixedly connected between the eccentric rotating shaft (6) and the inner wall of the adherence eccentric cylinder (5), the same side end surfaces of the short filtering foam piece (61) and the long filtering foam piece (62) are located on the same plane, and the length of the long filtering foam piece (62) is 1.5-3 times that of the short filtering foam piece (61).
6. The method for preparing a low gel point and low melting point thermoreversible gelling composition according to claim 5, wherein: a plurality of evenly distributed foam pressing holes (501) are formed in the wall-attached eccentric cylinder (5), the short foam filtering sheet (61) and the long foam filtering sheet (62), and the inner diameters of two end opening parts of the foam pressing holes (501) are larger than the inner diameter of the middle part.
7. The method for preparing a low gel point and low melting point thermoreversible gelling composition according to claim 6, wherein: the eccentric rotating shaft (6) is only fixed with the end part of the adherence eccentric cylinder (5), a bubble pressing assembly is fixedly connected between the middle parts of the left and right inner walls of the adherence eccentric cylinder (5), the bubble pressing assembly comprises a positive shaft (73) positioned in the middle, two pairs of sealing partition plates (71) which are fixed with the positive shaft (73) and are vertically symmetrical, and a bubble pressing positive plate (72) which is rotationally connected to the positive shaft (73) through an electric rotating shaft, and two blades of the bubble pressing positive plate (72) are centrally symmetrical with respect to the positive shaft (73).
8. Use of a low gel point, low melting point, thermoreversible gelling composition characterized by: the gel composition is applied to the manufacture of food rubber, soft capsules and hard capsules.
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|---|---|---|---|---|
| JPH0724285A (en) * | 1993-07-13 | 1995-01-27 | Nobuyuki Kiko Kk | Mixing device |
| WO2003061633A1 (en) * | 2002-01-18 | 2003-07-31 | Banner Pharmacaps, Inc. | Non-gelatin capsule shell formulation comprising iota-carrageenan and kappa-carrageenan |
| US20040052839A1 (en) * | 2002-01-18 | 2004-03-18 | Archibald Don A. | Non-gelatin film and method and apparatus for producing same |
| CN107635656A (en) * | 2015-05-29 | 2018-01-26 | 花王株式会社 | The manufacture method of hydrogel particle |
| US20180154327A1 (en) * | 2016-05-19 | 2018-06-07 | Jiangsu Lefan Capsule Co., Ltd. | A membrane-forming composition, soft and hard capsules prepared based on this composition and the preparation methods |
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2023
- 2023-11-01 CN CN202311435132.2A patent/CN117379388A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0724285A (en) * | 1993-07-13 | 1995-01-27 | Nobuyuki Kiko Kk | Mixing device |
| WO2003061633A1 (en) * | 2002-01-18 | 2003-07-31 | Banner Pharmacaps, Inc. | Non-gelatin capsule shell formulation comprising iota-carrageenan and kappa-carrageenan |
| US20040052839A1 (en) * | 2002-01-18 | 2004-03-18 | Archibald Don A. | Non-gelatin film and method and apparatus for producing same |
| CN107635656A (en) * | 2015-05-29 | 2018-01-26 | 花王株式会社 | The manufacture method of hydrogel particle |
| US20180154327A1 (en) * | 2016-05-19 | 2018-06-07 | Jiangsu Lefan Capsule Co., Ltd. | A membrane-forming composition, soft and hard capsules prepared based on this composition and the preparation methods |
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