WO2022143667A1 - 淀粉成膜组合物及其制备胶囊壳的方法 - Google Patents

淀粉成膜组合物及其制备胶囊壳的方法 Download PDF

Info

Publication number
WO2022143667A1
WO2022143667A1 PCT/CN2021/142077 CN2021142077W WO2022143667A1 WO 2022143667 A1 WO2022143667 A1 WO 2022143667A1 CN 2021142077 W CN2021142077 W CN 2021142077W WO 2022143667 A1 WO2022143667 A1 WO 2022143667A1
Authority
WO
WIPO (PCT)
Prior art keywords
starch
forming composition
gelling agent
film
gellan gum
Prior art date
Application number
PCT/CN2021/142077
Other languages
English (en)
French (fr)
Inventor
李绪发
陈琼
杨旭腾
陈洁伟
Original Assignee
仙乐健康科技股份有限公司
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 仙乐健康科技股份有限公司 filed Critical 仙乐健康科技股份有限公司
Priority to CA3164901A priority Critical patent/CA3164901C/en
Priority to US17/792,843 priority patent/US20230051942A1/en
Priority to JP2022533233A priority patent/JP2023512402A/ja
Priority to EP21914401.1A priority patent/EP4074191A4/en
Priority to AU2021411017A priority patent/AU2021411017B2/en
Publication of WO2022143667A1 publication Critical patent/WO2022143667A1/zh

Links

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
    • A61K9/4825—Proteins, e.g. gelatin
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/206—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
    • A23L29/212—Starch; Modified starch; Starch derivatives, e.g. esters or ethers
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/206—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
    • A23L29/231—Pectin; Derivatives thereof
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/206—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
    • A23L29/238—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin from seeds, e.g. locust bean gum or guar gum
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/206—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
    • A23L29/244—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin from corms, tubers or roots, e.g. glucomannan
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/206—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
    • A23L29/256—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin from seaweeds, e.g. alginates, agar or carrageenan
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/269—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of microbial origin, e.g. xanthan or dextran
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/269—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of microbial origin, e.g. xanthan or dextran
    • A23L29/272—Gellan
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/269—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of microbial origin, e.g. xanthan or dextran
    • A23L29/274—Pullulan
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/30—Foods or foodstuffs containing additives; Preparation or treatment thereof containing carbohydrate syrups; containing sugars; containing sugar alcohols, e.g. xylitol; containing starch hydrolysates, e.g. dextrin
    • 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
    • A61K47/30—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
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/11—Encapsulated compositions
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73—Polysaccharides
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73—Polysaccharides
    • A61K8/732—Starch; Amylose; Amylopectin; Derivatives thereof
    • 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
    • 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
    • A61K9/4841—Filling excipients; Inactive ingredients
    • A61K9/4866—Organic macromolecular compounds
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • 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
    • A23P20/00—Coating of foodstuffs; Coatings therefor; Making laminated, multi-layered, stuffed or hollow foodstuffs
    • A23P20/10—Coating with edible coatings, e.g. with oils or fats
    • A23P20/105—Coating with compositions containing vegetable or microbial fermentation gums, e.g. cellulose or derivatives; Coating with edible polymers, e.g. polyvinyalcohol
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/10—General cosmetic use

Definitions

  • the present application relates to the field of edible compositions, in particular to a starch film-forming composition, a method for preparing a capsule shell thereof, and a prepared capsule shell.
  • Soft capsules are widely used in medicine, food, cosmetics and other fields. Because gelatin has excellent film-forming properties and mechanical strength, it is widely used as a traditional soft capsule material. However, due to the characteristics of gelatin itself, there are many quality defects in the application process. For example, gelatin molecules can undergo self-oxidation or cross-linking reaction with functional groups such as aldehyde groups, resulting in a tough and durable layer on the surface of gelatin soft capsules.
  • the elastic water-insoluble film blocks the release of drugs, resulting in unqualified disintegration of soft capsules; coupled with religion, vegetarianism, and the occurrence of mad cow disease, foot-and-mouth disease and other incidents around the world, people have been trying to develop glue. Substitutes and their preparation of soft capsules.
  • Chinese Patent No. CN100528950C proposes a mixture of different acyl gellan and starch, comprising: a. high acyl gellan; b. low acyl gellan; c. starch; and d. plasticizer, using Films made from such mixtures have high modulus and good strength and extensibility, and the resulting soft capsules have good sealing properties.
  • High acyl gellan gum and low acyl gellan gum, as compound gelling agents, can improve the strength and toughness of the rubber skin to a certain extent, but the soft capsules prepared by them have poor transparency, and the joints are not tightly sealed and prone to oil leakage.
  • JP2007153851A proposes a film composition of soft capsules of non-animal origin, obtained by mixing water, starch and natural type gellan gum.
  • European Patent No. EP2815745A1 proposes a soft capsule comprising high acyl gellan gum, at least one starch and at least one plasticizer and a preparation method.
  • the gel formed by high acyl gellan gum has the characteristics of soft texture and elasticity. When combined with starch, the rubber formed has poor toughness. When the pellet is formed, the gap is thin, the rupture force is low, and it is easy to leak oil.
  • Chinese Patent No. CN 108659137 A proposes a new type of gellan gum product with double gel temperature, which has a lower double gel temperature, and the gel formed by it has excellent gel properties and texture, which can be more widely used Applied in the food field.
  • It is an object of the present application to provide a starch film-forming composition comprising gellan gum and starch with a specified acyl content.
  • gellan gum with a specific acyl content between high acyl gellan gum (natural gellan gum) and low acyl gellan gum, its single gel The temperature range is 20-75°C, so that the gel formed by the starch film-forming composition of gellan gum containing the specific acyl content has excellent gel properties and texture, and is used for the preparation of soft capsules.
  • bonding it is obviously superior to the prior art, fully meets the requirements of industrial production of soft capsules, and can be used as an alternative to soft capsule technology.
  • starch compositions comprising a specific range of gellan gum to starch ratios outperform starch compositions not within this range in terms of the combined effect of rubber strength, toughness and form adhesion.
  • the application provides a starch film-forming composition comprising:
  • A the first gelling agent
  • the first gelling agent is single-gel temperature gellan gum, and its total acyl content is 14-34%, and the weight ratio of the single-gel temperature gellan gum to starch is 0.02-0.5.
  • the total acyl group content of gellan gum is 12-26% glyceryl acyl group, and/or the acetyl group content is 2-8%.
  • the content of starch is from 15 wt% to 50 wt%.
  • the content of gellan gum is 1wt%-8wt%, preferably, the content of gellan gum is 2wt%-7wt%.
  • the starch is a native starch selected from one or more of wheat starch, waxy corn starch, pea starch, corn starch, potato starch and tapioca starch.
  • the starch is a starch derivative which is acid-treated starch, hydroxypropyl starch, oxidized starch, acetate starch, oxidized hydroxypropyl starch, hydroxypropyl distarch phosphate, One or more of starch phosphate, sodium starch octenyl succinate, acetylated distarch phosphate and dextrin.
  • the starch film-forming composition further comprises a plasticizer, and the content of the plasticizer is 10wt% to 35wt%, preferably, the plasticizer is selected from glycerol, sorbitol, maltitol, One or more of erythritol, xylitol, fructose and trehalose.
  • the starch film-forming composition further comprises a second gelling agent.
  • the second gelling agent is selected from the group consisting of carrageenan, agar, sodium alginate, pectin, high acyl gellan gum, low acyl gellan gum, konjac gum, xanthan gum, locust bean gum, guar gum and One or more of Lulan polysaccharides; preferably the content of the second gelling agent is 0.2wt%-3.5wt%, preferably the pectin is low methoxyl pectin, high methoxyl pectin and one or more of amide pectin; preferably wherein the low methoxyl pectin has a degree of esterification of DE ⁇ 50%, and the amide pectin has a degree of amidation of DA 5%-25%.
  • the starch film-forming composition comprises 35 wt% to 60 wt% water.
  • the present application provides a method for preparing a capsule shell using the starch film-forming composition of the present application, which comprises 1) A) firstly premixing and uniformly dispersing the first gelling agent and the plasticizer, and adding under stirring into water, heat and stir at 60-98°C until the first gelling agent dissolves; B) add starch, continue to heat and stir at 60-98°C until the starch dissolves; C) remove air bubbles to obtain glue; 2) press pills and 3) drying.
  • Pill pressing can be carried out as follows: using a soft capsule production line, the glue liquid is transported to the plastic box of the soft capsule filling machine, the glue liquid is cooled on the surface of the drum to form a rubber skin, and is compressed and formed by packaging and filling, which can be further passed through the rotating cage. stereotypes. Drying can be carried out as follows: the capsules are dried after forming or tumbler-setting until the rubber skin moisture is 8-25%.
  • said A) further comprises adding a second gelling agent; said A) is that the first gelling agent, the second gelling agent and the plasticizer are premixed and uniformly dispersed, and added to water under stirring , heating and stirring at 60-98° C. until the first gelling agent and the second gelling agent are dissolved.
  • the present application provides capsule shells comprising the starch film-forming compositions of the present application.
  • the water content of the capsule shell is 8-25%.
  • the present application provides the use of the starch film-forming composition of the present application in medicine, food or cosmetics.
  • This application also includes the following options:
  • Embodiment 1 A starch film-forming composition comprising the following ingredients:
  • the first gum gel is selected from one or more of carrageenan, agar, sodium alginate, gellan gum, konjac gum, xanthan gum, locust bean gum, guar gum and pullulan;
  • the second gum gel is pectin.
  • Embodiment 2 The starch film-forming composition of Embodiment 1, wherein the pectin is one or more of low methoxy pectin, high methoxy pectin, and amide pectin.
  • Embodiment 3 The starch film-forming composition of the preceding embodiment, wherein the low methoxy pectin has a degree of esterification of DE ⁇ 50%, or the amido pectin has a degree of amidation DA of 5-25%.
  • Embodiment 4 The starch film-forming composition of the preceding embodiment, wherein the gellan gum is a high acyl gellan gum, a low acyl gellan gum, or a gellan gum with a total acyl content of 14-34%, preferably the Gellan gum is a gellan gum with a total acyl content of 14-34%, preferably a glyceryl acyl content of 12-26% and/or an acetyl content of 2-8% in the total acyl group of the gellan gum.
  • the gellan gum is a high acyl gellan gum, a low acyl gellan gum, or a gellan gum with a total acyl content of 14-34%
  • the Gellan gum is a gellan gum with a total acyl content of 14-34%, preferably a glyceryl acyl content of 12-26% and/or an acetyl content of 2-8% in the total acyl group of the gellan gum.
  • Embodiment 5 The starch film-forming composition of the preceding embodiment, wherein the starch is a native starch selected from the group consisting of wheat starch, waxy corn starch, pea starch, corn starch, potato starch, and tapioca starch. one or more.
  • the starch is a native starch selected from the group consisting of wheat starch, waxy corn starch, pea starch, corn starch, potato starch, and tapioca starch. one or more.
  • Embodiment 6 The starch film-forming composition of the preceding embodiment, wherein the starch is a starch derivative that is acid-treated starch, hydroxypropyl starch, oxidized starch, acetate starch, oxidized hydroxypropyl starch , one or more of hydroxypropyl distarch phosphate, starch phosphate, sodium starch octenyl succinate, acetylated distarch phosphate and dextrin.
  • the starch is a starch derivative that is acid-treated starch, hydroxypropyl starch, oxidized starch, acetate starch, oxidized hydroxypropyl starch , one or more of hydroxypropyl distarch phosphate, starch phosphate, sodium starch octenyl succinate, acetylated distarch phosphate and dextrin.
  • Embodiment 7 The starch film-forming composition of the preceding embodiment, wherein the plasticizer is selected from one or more of glycerol, sorbitol, maltitol, erythritol, xylitol, fructose, and trehalose .
  • the plasticizer is selected from one or more of glycerol, sorbitol, maltitol, erythritol, xylitol, fructose, and trehalose .
  • Embodiment 8 A method of making a capsule shell using the starch film-forming composition of any one of Embodiments 1-7, comprising 1) A) premixing a first gelling agent, a second gelling agent, and a plasticizer Disperse uniformly, add into water with stirring, heat and stir at 60-98°C until the first gelling agent and the second gelling agent dissolve; B) add starch, continue to heat and stir at 60-98°C until the starch dissolves; C ) remove the bubbles to get glue;
  • Embodiment 9 A capsule shell comprising the starch film-forming composition of any one of Embodiments 1-8.
  • Embodiment 10 The capsule shell of Embodiment 9, the capsule shell having a moisture content of 8-25%.
  • Embodiment 11 Use of the starch film-forming composition of any one of Embodiments 1-8 in medicine, food or cosmetics.
  • starch film-forming composition of the present application includes: good film-forming strength and toughness, soft capsules with good forming adhesion and encapsulation can be obtained when applied to soft capsules, no animal-derived ingredients, and suitable for all ethnic groups in the world It can be consumed by the crowd and can be promoted and applied globally.
  • the present application provides starch film-forming compositions comprising a first gelling agent and starch, the first gelling agent being gellan gum.
  • Gellan gum can be divided into low acyl gellan gum, high acyl gellan gum and partially deacylated gellan gum according to the total acyl content.
  • the total acyl content of gellan gum may be 14-34%, such as 14%, 16%, 17%, 19%, 27%, 28%, 30%, 31%, 32% or 34%.
  • the total acyl content of gellan gum can be calculated as the sum of the content of glyceryl acyl and acetyl groups.
  • the glyceroyl content may be 12-26%, eg 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%, 21%, 22%, 23%, 24% or 25%.
  • the acetyl content may be 2-8%, such as 3%, 4%, 5%, 6% or 7%.
  • the gellan gum content in the starch film-forming composition may be 1 wt% to 8 wt%, such as 2 wt%, 3 wt%, 4 wt%, 5 wt%, 6 wt%, 7 wt% or 8 wt%.
  • the gellan gum content may be 2wt%-7wt%.
  • the starch content in the starch film-forming composition may range from 15wt% to 50wt%, such as 20wt%, 25wt% or 35wt%, 45wt%.
  • Starch can be natural starch or a starch derivative or combination of natural starch prepared by physical, chemical, enzymatic methods and the like.
  • the native starch can be selected from one or a combination of wheat starch, waxy corn starch, pea starch, corn starch, potato starch, and tapioca starch.
  • the starch derivative may be selected from acid-treated starch, hydroxypropyl starch, oxidized starch, acetate starch, oxidized hydroxypropyl starch, hydroxypropyl distarch phosphate, starch phosphate, sodium starch octenyl succinate, acetylated starch One or a combination of distarch phosphate and dextrin.
  • the content of the above various types of starch is independently 7wt%-50wt%, such as 8wt%, 9wt%, 10wt%, 11wt%, 12wt%, 13wt%, 14wt%, 15wt%, 16wt%, 17wt%, 18wt% %, 19 wt %, 20 wt %, 21 wt %, 22 wt %, 23 wt %, 24 wt %, 25 wt % or 30 wt %.
  • the weight ratio of gellan gum to starch may be from 0.02 to 0.5, such as 0.04, 0.06, 0.09, 0.11, 0.12, 0.16, 0.17, 0.20, 0.23, 0.24 or 0.50.
  • the starch film-forming composition may also contain one or more of a plasticizer and a second gelling agent.
  • the plasticizer can be one or more of glycerol, sorbitol, maltitol, erythritol, xylitol, fructose, and trehalose.
  • the second gelling agent can be carrageenan, agar, sodium alginate, low methoxy pectin, high methoxy pectin, amide pectin, high acyl gellan gum, low acyl gellan gum, konjac gum, yellow One or more of native gum, locust bean gum, guar gum, and pullulan.
  • the content of plasticizer may be 10wt%-35wt%, for example 15wt%, 17wt%, 18wt%, 20wt%, 25wt% or 30wt%.
  • the starch film-forming composition of the present application further comprises water, eg, 35 wt% to 60 wt% water, eg, 36 wt%, 39 wt%, 42 wt%, 43 wt%, 46 wt%, 47 wt%, 48 wt%, 49 wt%, or 56 wt%. Water can be used to make up the total amount of the composition to 100 wt%.
  • Soft capsules can be prepared using the starch film-forming compositions of the present application.
  • the preparation of soft capsules may include 1) A) firstly premixing and dispersing the first gelling agent and plasticizer uniformly, adding them to water under stirring, and heating and stirring at 60-98° C. until the first gelling agent is dissolved; B) adding starch, continue to heat and stir at 60-98° C. until the starch dissolves; C) remove air bubbles to obtain glue; 2) press pellets; and 3) dry.
  • the preparation of soft capsules may include 1) A) first premixing the first gelling agent, the second gelling agent and the plasticizer and dispersing them uniformly, adding them to water under stirring, and heating and stirring at 60-98° C. until the first gelatinizer is stirred. The coagulant and the second gelling agent are dissolved; B) add starch, continue to heat and stir at 60-98° C. until the starch is dissolved; C) remove air bubbles to obtain glue; 2) press pellets; and 3) dry.
  • the above-mentioned starch film-forming composition of the present application can be prepared into soft capsules with good forming, adhesive and encapsulating properties, and can be used in medicine, food or cosmetics.
  • the present application provides starch film-forming compositions comprising pectin.
  • the pectin is one or more of low methoxyl pectin, high methoxyl pectin and amide pectin.
  • the content of pectin may be 0.2wt%-3.5wt%, such as 0.50wt%, 1.25wt%, 1.5wt%, 2.50wt% or 3.5wt%.
  • the starch film-forming composition may further comprise one of carrageenan, agar, sodium alginate, gellan gum, konjac gum, xanthan gum, locust bean gum, guar gum, and pullulan. one or more.
  • the starch film-forming composition further comprises gellan gum.
  • the gellan gum is a high acyl gellan gum, a low acyl gellan gum or a gellan gum with a total acyl content of 14-34%, preferably the gellan gum is a gellan with a total acyl content of 14-34%
  • the gum, preferably gellan gum has a glyceryl acyl content of 12-26%, and/or an acetyl content of 2-8% in total acyl groups.
  • the content and acyl content of gellan gum may be as defined above.
  • the starch film-forming composition comprising pectin may also comprise starch, and the type and amount thereof are as defined above.
  • the starch may be hydroxypropyl starch and hydroxypropyl distarch phosphate, eg, 7wt-25wt% each independently, eg 8wt%, 9wt%, 10wt%, 11wt%, 12wt%, 13wt%, 14wt%, 15wt%, 16wt%, 17wt%, 18wt%, 19wt%, 20wt%, 21wt%, 22wt%, 23wt%, or 24wt%.
  • the starch film-forming compositions containing pectin may also contain plasticizers.
  • the kind and content of the plasticizer may be as defined above.
  • the starch film-forming composition comprising pectin can also be water.
  • the water content may be as defined above.
  • the present application demonstrates that starch film-forming compositions that do not contain pectin are disintegrated in the stomach and cannot be delivered to the intestine.
  • the starch film-forming composition containing pectin of the present application complies with the relevant regulations of enteric-coated capsules in the disintegration time limit detection method in the Chinese Pharmacopoeia. This is unexpected.
  • Gellan gum (total acyl content 33.2%, glyceryl acyl content 25.5%, acetyl content 7.7%) (commercially available)
  • Acetate starch (commercially available)
  • Acetylated oxidized starch (commercially available)
  • Acetylated distarch phosphate (commercially available)
  • Amide pectin (amid degree (DA: 5-25%), commercially available)
  • Methods include:
  • Pill pressing The soft capsule production line is used to transport the glue into the plastic box of the soft capsule filling machine.
  • the glue is cooled on the surface of the drum to form a rubber skin, which is pressed and bonded by the packaging and filler, and can be further shaped by the rotating cage. .
  • Drying Dry the capsules after forming or tumble forming until the moisture content of the rubber skin is 8-25%.
  • Example 1-7 Comparative Example 1-3
  • Softgels were prepared with the ingredients and levels described in Table 2, and tested and scored. The measurement results are shown in Table 2.
  • Examples 1-7 adopt the combination of gellan gum and starch with a specific acyl content, and the formed rubber has better strength, toughness and forming adhesion
  • Comparative Examples 1-2 adopt the same film-forming composition of the present application
  • the gellan gum with high acyl content is combined with starch
  • the formed rubber is weak in strength and has a certain toughness, but the forming adhesion is general
  • the formed rubber is The strength is good, the toughness is poor, and it cannot be formed.
  • Comparative Example 3 two kinds of gellan gums with different acyl contents were used.
  • the glyceryl acyl and acetyl contents in the compound rubber were close to the specific acyl content range of the present application, but the molding adhesion was poor. It is shown that the soft capsule prepared by using the combination of gellan gum and starch with specific acyl content of the present application is superior to the prior art.
  • Softgels were prepared with the ingredients and levels described in Table 3, and tested and scored. The measurement results are shown in Table 3.
  • Softgels were prepared with the ingredients and levels described in Table 4, and tested and scored. The measurement results are shown in Table 4.
  • Examples 19-25 illustrate that specific acyl content gellan gum and various types of starch are combined to prepare soft capsules, and the technical effect is obviously better than the prior art.
  • Softgels were prepared with the ingredients and levels described in Table 5, tested and scored. The measurement results are shown in Table 5.
  • Examples 26-31 adopt specific acyl content gellan gum and starch in combination with low acyl gellan gum, agar, locust bean gum, guar gum, and konjac gum to prepare soft capsules.
  • the technical effect is better than the prior art.
  • the soft capsules were prepared with the ingredients and contents described in Table 6, and the disintegration time limit test was carried out according to the relevant regulations of the enteric-coated capsules in the Chinese Pharmacopoeia for the disintegration time limit detection method. The measurement results are shown in Table 6.
  • the disintegration time limit of the samples of Example 22, Example 26, and Example 32-37 was detected.
  • the solution (9 ⁇ 1000) no baffle was added for inspection, and it disintegrated completely within 60 minutes; while the samples of Example 32-37 were inspected without baffle in the hydrochloric acid solution (9 ⁇ 1000), and there was no disintegration in 120 minutes.
  • phosphate buffer (PH6.8) detection add a baffle to each tube, all disintegrate within 60 minutes, which meets the requirements of the disintegration time limit for enteric-coated capsules in the ⁇ Chinese Pharmacopoeia> disintegration time limit inspection method. Therefore, the specific acyl content gellan gum and starch and pectin (such as low methoxyl pectin or amide pectin) used in this application to prepare soft capsules can meet the disintegration time limit of enteric soft capsules.
  • the soft capsules prepared by the combination of gellan gum and starch with a specific acyl content in the present application have good film-forming strength and toughness, and both increase with the increase of the gellan gum ratio within a certain range, while the molding viscosity The compatibility decreases as the proportion of gellan gum increases.
  • the soft capsule prepared by the composition of gellan gum and starch with specific acyl content of the present application is obviously superior to the prior art in terms of rubber skin strength, toughness and forming adhesion, fully meets the requirements of industrial production of soft capsules, and can be used as soft capsule technology. alternative alternative.

Landscapes

  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Polymers & Plastics (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Nutrition Science (AREA)
  • Dispersion Chemistry (AREA)
  • Veterinary Medicine (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Epidemiology (AREA)
  • Medicinal Chemistry (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Birds (AREA)
  • Inorganic Chemistry (AREA)
  • Molecular Biology (AREA)
  • Dermatology (AREA)
  • Medicinal Preparation (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Grain Derivatives (AREA)
  • General Preparation And Processing Of Foods (AREA)

Abstract

提供一种淀粉成膜组合物及其制备胶囊壳的方法。该淀粉成膜组合物包含结冷胶和至少一种淀粉，其中结冷胶的总酰基含量为14-34％。淀粉成膜组合物的优点具有较好的成膜强度和韧性，应用于软胶囊可得到成型粘合包封性好的软胶囊，不含动物来源成分，适合于世界各族人群食用。

Description

淀粉成膜组合物及其制备胶囊壳的方法
本申请要求2020年12月31日提交的申请号为202011619863.9，发明名称为“淀粉成膜组合物及其制备胶囊壳的方法”的中国发明专利申请的优先权。
技术领域
本申请涉及食用组合物领域，具体涉及淀粉成膜组合物、其制备胶囊壳的方法及制备的胶囊壳。
背景技术
软胶囊在医药、食品、化妆品等领域广泛应用，因明胶具有优异的成膜性能和机械强度，作为传统软胶囊材料广泛使用。但由于明胶本身的特性，所以在运用过程中表现出许多质量缺陷，如明胶分子可以通过自身氧化或与功能性基团如醛基发生交联反应，在明胶软胶囊表面产生一层坚韧而有弹性的水不溶性表膜，阻隔药物释放，导致软胶囊的崩解不合格；再加上宗教、素食主义者，以及随着世界各地相继出现疯牛病、口蹄疫等事件，因此人们一直在试图开发明胶的替代品及其制备软胶囊的研究。
例如，中国专利号CN100528950C提出了一种不同酰基结冷胶与淀粉的混合物，包含：a.高酰基结冷胶；b.低酰基结冷胶；c.淀粉；和d.增塑剂，使用这样的混合物制成的薄膜具有高模数以及优良强度和延伸性，制成的软胶囊具有良好密封性。高酰基结冷胶和低酰基结冷胶作为复配凝胶剂，可在一定程度改善胶皮强度和韧性，但其制备的软胶囊透明度不好，且夹缝密封不牢固、易漏油。日本专利号JP2007153851A提出了一种由非动物来源的软胶囊的薄膜组合物，通过混合水、淀粉和天然型结冷胶得到。欧洲专利号EP2815745A1提出了一种包含高酰基结冷胶、至少一种淀粉和至少一种增塑剂的软胶囊及制备方法。高酰基结冷胶形成的凝胶具有质地柔软富有弹性的特性，与淀粉组合时形成的胶皮韧性差，压丸成型时夹缝较薄、破裂力低易漏油。中国专利号CN 108659137 A提出了一种具有双凝胶温度的新型结冷胶产品，具有较低的双凝胶温度，其形成的凝胶具有优良的凝胶特性和质构，可更广泛地应用于食品领域。
综上所述，现有技术报道的以结冷胶为主要囊材的软胶囊制备过程中存 在胶液粘度高，高温储存时容易凝胶，且形成的胶皮强度低、韧性差、压丸成型夹缝薄易漏油等缺陷，无法实现软胶囊工业化生产。
发明内容
本申请的目的是提供淀粉成膜组合物，其包含特定酰基含量的结冷胶和淀粉。发明人在淀粉成膜组合物的研究过程中发现，酰基含量介于高酰基结冷胶(天然结冷胶)和低酰基结冷胶间的特定酰基含量的结冷胶，其单一的凝胶温度范围为20-75℃，使包含该特定酰基含量的结冷胶的淀粉成膜组合物形成的凝胶具有优良的凝胶特性和质构，用于制备软胶囊时胶皮强度、韧性和成型粘合方面明显优于现有技术，完全满足软胶囊工业化生产要求，可以作为软胶囊技术的备选替代。发明人还发现包含特定范围的结冷胶与淀粉比的淀粉组合物在胶皮强度、韧性和成型粘合的综合效果上优于不在该范围内的淀粉组合物。
在一方面，本申请提供了一种淀粉成膜组合物，该淀粉成膜组合物包含：
A、第一胶凝剂；
B、淀粉；
所述第一胶凝剂为单凝胶温度结冷胶，其总酰基含量为14-34％，所述单凝胶温度结冷胶与淀粉的重量比为0.02～0.5。
在一个实施方案中，结冷胶总酰基中甘油酰基含量为12-26％，和/或乙酰基含量为2-8％。
在一个实施方案中，淀粉的含量为15wt％-50wt％。
在一个实施方案中，结冷胶的含量为1wt％-8wt％，优选地，结冷胶含量为2wt％-7wt％。
在一个实施方案中，所述淀粉为天然淀粉，所述天然淀粉选自小麦淀粉、蜡质玉米淀粉、豌豆淀粉、玉米淀粉、马铃薯淀粉和木薯淀粉中的一种或多种。
在一个实施方案中，所述淀粉为淀粉衍生物，所述淀粉衍生物是酸处理淀粉、羟丙基淀粉、氧化淀粉、醋酸酯淀粉、氧化羟丙基淀粉、羟丙基二淀粉磷酸酯、淀粉磷酸酯、辛烯基琥珀酸淀粉钠、乙酰化二淀粉磷酸酯和糊精中的一种或多种。
在一个实施方案中，淀粉成膜组合物还包含增塑剂，所述增塑剂的含量 为10wt％～35wt％，优选地，所述增塑剂选自甘油、山梨糖醇、麦芽糖醇、赤藓糖醇、木糖醇、果糖和海藻糖中一种或多种。
在一个实施方案中，该淀粉成膜组合物还包含第二胶凝剂。优选地，第二胶凝剂选自卡拉胶、琼脂、海藻酸钠、果胶、高酰基结冷胶、低酰基结冷胶、魔芋胶、黄原胶、刺槐豆胶、瓜尔胶和普鲁兰多糖中的一种或多种；优选地所述第二胶凝剂含量为0.2wt％-3.5wt％，优选地所述果胶是低甲氧基果胶、高甲氧基果胶和酰胺果胶中的一种或多种；优选地其中低甲氧基果胶具有DE<50％的酯化度，酰胺果胶具有DA 5％-25％的酰胺度。
在一个实施方案中，淀粉成膜组合物包含35wt％-60wt％水。
在另一个方面，本申请提供了使用本申请的淀粉成膜组合物制备胶囊壳的方法，其包括1)A)先将第一胶凝剂和增塑剂预混并且分散均匀，搅拌下加入到水中，在60～98℃下加热搅拌至第一胶凝剂溶解；B)加入淀粉，继续在60～98℃下加热搅拌至淀粉溶解；C)除去气泡即得胶液；2)压丸；和3)干燥。压丸可以如下进行：采用软胶囊生产线，将胶液输送至软胶囊填充机的胶盒中，胶液在转鼓表面上冷却形成胶皮，经封装填充物压制粘合成型，可进一步通过转笼定型。干燥可以如下进行：将成型或转笼定型后胶丸进行干燥，直至胶皮水分为8-25％。
在一个实施方案中，所述A)还包括加入第二胶凝剂；所述A)为第一胶凝剂、第二胶凝剂和增塑剂预混并且分散均匀，搅拌下加入到水中，在60～98℃下加热搅拌至第一胶凝剂和第二胶凝剂溶解。
在另一个方面，本申请提供了包含本申请的淀粉成膜组合物的胶囊壳。
在一个实施方案中，该胶囊壳的含水量为8-25％。
在另一个方面，本申请提供了本申请的淀粉成膜组合物在医药、食品或化妆品中的应用。
本申请还包括以下方案：
实施方案1.一种淀粉成膜组合物，该淀粉成膜组合物包含以下成分：
1wt％-8wt％第一胶凝剂；
0.2wt％-3.5wt％第二胶凝剂；
15wt％-50wt％淀粉；
10wt％～35wt％增塑剂；和
水，补足至100wt％；
其中第一胶凝胶选自卡拉胶、琼脂、海藻酸钠、结冷胶、魔芋胶、黄原胶、刺槐豆胶、瓜尔胶和普鲁兰多糖中的一种或多种；
第二胶凝胶是果胶。
实施方案2.实施方案1的淀粉成膜组合物，其中所述果胶是低甲氧基果胶、高甲氧基果胶和酰胺果胶中的一种或多种。
实施方案3.上述实施方案的淀粉成膜组合物，其中低甲氧基果胶具有DE<50％的酯化度，或酰胺果胶具有5-25％的酰胺度DA。
实施方案4.上述实施方案的淀粉成膜组合物，其中所述结冷胶为高酰基结冷胶、低酰基结冷胶或总酰基含量为14-34％的结冷胶，优选地所述结冷胶为总酰基含量为14-34％的结冷胶，优选地结冷胶总酰基中甘油酰基含量为12-26％，和/或乙酰基含量为2-8％。
实施方案5.上述实施方案的淀粉成膜组合物，其中所述淀粉为天然淀粉，所述天然淀粉选自小麦淀粉、蜡质玉米淀粉、豌豆淀粉、玉米淀粉、马铃薯淀粉和木薯淀粉中的一种或多种。
实施方案6.上述实施方案的淀粉成膜组合物，其中所述淀粉为淀粉衍生物，所述淀粉衍生物是酸处理淀粉、羟丙基淀粉、氧化淀粉、醋酸酯淀粉、氧化羟丙基淀粉、羟丙基二淀粉磷酸酯、淀粉磷酸酯、辛烯基琥珀酸淀粉钠、乙酰化二淀粉磷酸酯和糊精中的一种或多种。
实施方案7.上述实施方案的淀粉成膜组合物，其中所述增塑剂选自甘油、山梨糖醇、麦芽糖醇、赤藓糖醇、木糖醇、果糖和海藻糖中一种或多种。
实施方案8.使用实施方案1-7中任一项的淀粉成膜组合物制备胶囊壳的方法，其包括1)A)将第一胶凝剂、第二胶凝剂和增塑剂预混分散均匀，搅拌下加入到水中，在60～98℃下加热搅拌至第一胶凝剂和第二胶凝剂溶解；B)加入淀粉，继续在60～98℃下加热搅拌至淀粉溶解；C)除去气泡即得胶液；
2)压丸；和
3)干燥。
实施方案9.包含实施方案1-8中任一项的淀粉成膜组合物的胶囊壳。
实施方案10.实施方案9的胶囊壳，该胶囊壳的含水量为8-25％。
实施方案11.实施方案1-8中任一项的淀粉成膜组合物在医药、食品或化妆品中的应用。
本申请的淀粉成膜组合物的优点包括：具有较好的成膜强度和韧性，应用于软胶囊可得到成型粘合包封性好的软胶囊，不含动物来源成分，适合于世界各族人群食用，可以在全球推广应用。
具体实施方式
提供以下内容以进一步说明本申请。
在本文中使用时，若无相反说明，“％”或“wt％”指重量百分比。
本申请提供了淀粉成膜组合物，该淀粉成膜组合物包含第一胶凝剂和淀粉，该第一胶凝剂是结冷胶。结冷胶根据总酰基含量可以分为低酰基结冷胶、高酰基结冷胶和部分脱酰基结冷胶。在本申请中，结冷胶的总酰基含量可以为14-34％，例如14％、16％、17％、19％、27％、28％、30％、31％、32％或34％。结冷胶的总酰基含量可以以甘油酰基和乙酰基的含量之和计。甘油酰基含量可以为12-26％，例如13％、14％、15％、16％、17％、18％、19％、20％、21％、22％、23％、24％或25％。乙酰基含量可以为2-8％，例如3％、4％、5％、6％或7％。
淀粉成膜组合物中的结冷胶含量可以为1wt％～8wt％，例如2wt％、3wt％、4wt％、5wt％、6wt％、7wt％或8wt％。优选地，结冷胶含量可以为2wt％-7wt％。
淀粉成膜组合物中的淀粉含量可以为15wt％-50wt％，例如20wt％、25wt％或35wt％、45wt％。
淀粉可以是天然淀粉或者天然淀粉通过物理、化学、酶法等方式制成的淀粉衍生物或组合。天然淀粉可以选自小麦淀粉、蜡质玉米淀粉、豌豆淀粉、玉米淀粉、马铃薯淀粉、木薯淀粉中的一种或组合。淀粉衍生物可以选自酸处理淀粉、羟丙基淀粉、氧化淀粉、醋酸酯淀粉、氧化羟丙基淀粉、羟丙基二淀粉磷酸酯、淀粉磷酸酯、辛烯基琥珀酸淀粉钠、乙酰化二淀粉磷酸酯、糊精中的一种或组合。例如，上述各种类型的淀粉的含量各自独立为7wt-50wt％，例如8wt％、9wt％、10wt％、11wt％、12wt％、13wt％、14wt％、15wt％、16wt％、17wt％、18wt％、19wt％、20wt％、21wt％、22wt％、23wt％、24wt％、25wt％或30wt％。结冷胶与淀粉的重量比可以为0.02～0.5，例如0.04、0.06、0.09、0.11、0.12、0.16、0.17、0.20、0.23、0.24或0.50。
淀粉成膜组合物还可以包含增塑剂和第二胶凝剂中的一种或多种。增塑 剂可以是甘油、山梨糖醇、麦芽糖醇、赤藓糖醇、木糖醇、果糖和海藻糖中一种或多种。第二胶凝剂可以是卡拉胶、琼脂、海藻酸钠、低甲氧基果胶、高甲氧基果胶、酰胺果胶、高酰基结冷胶、低酰基结冷胶、魔芋胶、黄原胶、刺槐豆胶、瓜尔胶和普鲁兰多糖中的一种或多种。增塑剂的含量可以为10wt％-35wt％，例如15wt％、17wt％、18wt％、20wt％、25wt％或30wt％。
本申请的淀粉成膜组合物还包含水，例如35wt％-60wt％的水，例如36wt％、39wt％、42wt％、43wt％、46wt％、47wt％、48wt％、49wt％或56wt％。水可以用于补足组合物的总量至100wt％。
可以使用本申请的淀粉成膜组合物制备软胶囊。制备软胶囊可以包括1)A)先将第一胶凝剂和增塑剂预混分散均匀，搅拌下加入到水中，在60～98℃下加热搅拌至第一胶凝剂溶解；B)加入淀粉，继续在60～98℃下加热搅拌至淀粉溶解；C)除去气泡即得胶液；2)压丸；和3)干燥。
制备软胶囊可以包括1)A)先将第一胶凝剂、第二胶凝剂和增塑剂预混并且分散均匀，搅拌下加入到水中，在60～98℃下加热搅拌至第一胶凝剂和第二胶凝剂溶解；B)加入淀粉，继续在60～98℃下加热搅拌至淀粉溶解；C)除去气泡即得胶液；2)压丸；和3)干燥。本申请的上述淀粉成膜组合物可以制备成成型粘合包封性好的软胶囊，并且可以在医药、食品或化妆品中的应用。
本申请提供了包含果胶的淀粉成膜组合物。优选地，果胶是低甲氧基果胶、高甲氧基果胶和酰胺果胶中的一种或多种。果胶的含量可以为0.2wt％-3.5wt％，例如0.50wt％、1.25wt％、1.5wt％、2.50wt％或3.5wt％。在这种情况下，该淀粉成膜组合物还可以包含卡拉胶、琼脂、海藻酸钠、结冷胶、魔芋胶、黄原胶、刺槐豆胶、瓜尔胶和普鲁兰多糖中的一种或多种。在此方面的一个实施方案中，该淀粉成膜组合物还包含结冷胶。例如，结冷胶是高酰基结冷胶、低酰基结冷胶或总酰基含量为14-34％的结冷胶，优选地所述结冷胶为总酰基含量为14-34％的结冷胶，优选地结冷胶总酰基中甘油酰基含量为12-26％，和/或乙酰基含量为2-8％。结冷胶的含量和酰基含量可以如上文所定义。
包含果胶的淀粉成膜组合物还可以包含淀粉，并且其种类和含量如上文所定义。在一个实施方案中，淀粉可以是羟丙基淀粉和羟丙基二淀粉磷酸酯，例如各自独立为7wt-25wt％，例如8wt％、9wt％、10wt％、11wt％、12wt％、 13wt％、14wt％、15wt％、16wt％、17wt％、18wt％、19wt％、20wt％、21wt％、22wt％、23wt％、或24wt％。
包含果胶的淀粉成膜组合物还可以包含增塑剂。增塑剂的种类和含量可以如上文所定义。包含果胶的淀粉成膜组合物还可以水。水含量可以如上文所定义。本申请证明了不包含果胶的淀粉成膜组合物在胃中即被崩解而不能被递送到肠中。相反，本申请的包含果胶的淀粉成膜组合物符合中国药典中崩解时限检测法中肠溶胶囊的相关规定。这是意料不到的。
为了便于理解本申请，下文提供了示例性的实施例。应当理解这些实施例仅仅是示例性的而非限制性的。本申请的范围仅由所附权利要求书的范围确定。
实施例
评判方法
为了更好说明本申请的效果，采用以下软胶囊性能指标进行评价说明：
1)胶皮强度和韧性指标：采用物性测试仪，选择球形探头与穿刺模式，测试速度1.0mm/s，记录胶皮在破裂时力值(g)，及对应的破裂距离(mm)。胶皮的破裂力表示胶皮强度，破裂力越大，说明胶皮强度越好；破裂距离表示胶皮韧性，破裂距离越大，说明胶皮的韧性越好。
2)成型夹缝粘合指标：取本申请实施例样品，从胶囊在非夹缝上剪开，挤压排空内容物，然后保持与夹缝垂直从中间剪取一个含有两条夹缝的环圈，使环圈置于载玻片上，并使两条夹缝垂直载玻片，在显微镜下测量两条夹缝处的厚度及囊壳的厚度，计算最薄夹缝厚度占囊壳厚度的比值P(％)。
表1软胶囊胶皮强度、韧性和成型粘合指标评价标准
Figure PCTCN2021142077-appb-000001
Figure PCTCN2021142077-appb-000002
以胶皮强度指标、韧性指标和成型粘合指标进行综合评价，满分5分，各分值(X)表示：
0分：无法制成软胶囊；
0<X≤1分：软胶囊成型较差、易漏油；
1<X≤2分：软胶囊成型差、易漏油；
2<X≤3分：软胶囊成型良好；
3<X≤4分：软胶囊成型优异；
4<X≤5分：软胶囊成型非常优异。
材料
本申请采用以下物料进行举例说明，但本申请并不限于以下物料，具体如下。
结冷胶(总酰基含量14.4％，甘油酰基12.1％，乙酰基2.3％)(市售)
结冷胶(总酰基含量16.5％，甘油酰基12.8％，乙酰基3.7％)(市售)
结冷胶(总酰基含量19.0％，甘油酰基15.1％，乙酰基3.9％)(市售)
结冷胶(总酰基含量27.5％，甘油酰基19.8％，乙酰基7.7％)(市售)
结冷胶(总酰基含量28.0％，甘油酰基23.4％，乙酰基4.6％)(市售)
结冷胶(总酰基含量30.6％，甘油酰基25.1％，乙酰基5.5％)(市售)
结冷胶(总酰基含量33.2％，甘油酰基25.5％，乙酰基含量7.7％)(市售)
高酰基结冷胶(总酰基含量37.3％，甘油酰基20.4％，乙酰基16.9％)(市售)
低酰基结冷胶(总酰基含量11.2％，甘油酰基8.1％，乙酰基3.1％)(市售)
氧化淀粉(市售)
羟丙基淀粉(市售)
氧化羟丙基淀粉(市售)
羟丙基二淀粉磷酸酯(市售)
氧化淀粉(市售)
醋酸酯淀粉(市售)
乙酰化氧化淀粉(市售)
乙酰化二淀粉磷酸酯(市售)
甘油(市售)
琼脂(市售)
刺槐豆胶(市售)
瓜尔胶(市售)
酰胺果胶(酰胺度(DA：5-25％)，市售)
低甲氧基果胶(酯化度(DE：<50％)，市售)
魔芋胶(市售)
软胶囊制备的方法
方法包括：
1)溶胶：A)先将第一胶凝剂和增塑剂预混分散均匀，搅拌下加入到适量水中，在60～98℃下加热搅拌至第一胶凝剂溶解；若含有第二胶凝剂，则先将第一胶凝剂、第二胶凝剂和增塑剂预混并且分散均匀，搅拌下加入到水中，在60～98℃下加热搅拌至第一胶凝剂和第二胶凝剂溶解；B)加入淀粉，继续在60～98℃下加热搅拌至淀粉溶解；C)除去气泡即得胶液；
2)压丸：采用软胶囊生产线，将胶液输送至软胶囊填充机的胶盒中，胶液在转鼓表面上冷却形成胶皮，经封装填充物压制粘合成型，可进一步通过转笼定型。
3)干燥：将成型或转笼定型后胶丸进行干燥，直至胶皮水分为8-25％。
实施例1-7、对照例1-3
如表2中所述的成分和含量制备软胶囊，并且进行测试和评分。测定结果如表2中所示。
表2：实施例1-7、对照例1-3
Figure PCTCN2021142077-appb-000003
Figure PCTCN2021142077-appb-000004
Figure PCTCN2021142077-appb-000005
根据表2可知，实施例1-7采用特定酰基含量的结冷胶与淀粉组合，形成的胶皮强度、韧性和成型粘合较好，而对照例1-2采用本申请的成膜组合物相同的组分含量，当酰基含量高的结冷胶和淀粉组合时，形成的胶皮强度弱、有一定韧性，但成型粘合一般，而酰基含量低的结冷胶和淀粉组合时，形成的胶皮强度较好，韧性差，无法成型。对照例3采用两种不同酰基含量的结冷胶复配胶，复配胶中的甘油酰基和乙酰基含量接近本申请特定酰基含量范围，但成型粘合较差。说明采用本申请的特定酰基含量的结冷胶和淀粉组合制备的软胶囊优于现有技术。
实施例8-18
如表3中所述的成分和含量制备软胶囊，并且进行测试和评分。测定结果如表3中所示。
表3实施例8-18
Figure PCTCN2021142077-appb-000006
Figure PCTCN2021142077-appb-000007
实施例8-18随着结冷胶用量的增加，形成的胶皮强度增强，韧性接近，但成型粘合有减弱。包含特定范围的结冷胶与淀粉比的淀粉组合物在综合效果上优于不在该范围内的淀粉组合物，这是意料不到的。
实施例19-25
如表4中所述的成分和含量制备软胶囊，并且进行测试和评分。测定结果如表4中所示。
表4实施例19-25
Figure PCTCN2021142077-appb-000008
Figure PCTCN2021142077-appb-000009
实施例19-25举例说明特定酰基含量结冷胶与各类淀粉组合制备软胶囊，技术效果明显优于现有技术。
实施例26-31
如表5中所述的成分和含量制备软胶囊，并且进行测试和评分。测定结果如表5中所示。
表5实施例26-31
Figure PCTCN2021142077-appb-000010
实施例26-31采用特定酰基含量结冷胶和淀粉分别与低酰基结冷胶、琼脂、刺槐豆胶、瓜尔胶、魔芋胶组合制备软胶囊技术效果优于现有技术。
实施例32-37
如表6中所述的成分和含量制备软胶囊，并且按照中国药典中崩解时限检测法中肠溶胶囊的相关规定，进行崩解时限测试。测定结果如表6中所示。
Figure PCTCN2021142077-appb-000011
按<中国药典>崩解时限检查法中肠溶胶囊相关规定，检测实施例22、实施例26、实施例32-37样品的崩解时限，结果发现：实施例22、实施例26样品在盐酸溶液(9→1000)中不加挡板检查，60分钟内完全崩解；而实施例32-37样品在盐酸溶液(9→1000)中不加挡板检查，120分钟内没有崩解，改在磷酸盐缓冲液(PH6.8)检测，每管添加一个挡板，60分钟内全部崩解，符合<中国药典>崩解时限检查法中肠溶胶囊对崩解时限规定要求。因此，本申请采用的特定酰基含量结冷胶和淀粉与果胶(如低甲氧基果胶或酰胺果胶)组合制备软胶囊，可以满足肠溶软胶囊对崩解时限规定。
本申请采用具有特定酰基含量的结冷胶和淀粉的组合物制备的软胶囊具有良好的成膜强度和韧性，且两者在一定范围内随着结冷胶比例的增加而增加，而成型粘合性则随着结冷胶比例的增加而下降。本申请的具有特定酰基含量的结冷胶和淀粉的组合物制备的软胶囊在胶皮强度、韧性和成型粘合方面明显优于现有技术，完全满足软胶囊工业化生产要求，可以作为软胶囊技术的备选替代。
上述实施例为本申请较佳的实施方式，但本申请的实施方式并不受上述实施例的限制，其他的任何未背离本申请的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本申请的保护范围之内。

Claims (14)

  1. 一种淀粉成膜组合物，该淀粉成膜组合物包含：
    A、第一胶凝剂；
    B、淀粉；
    所述第一胶凝剂为单凝胶温度结冷胶，其总酰基含量为14％-34％，所述单凝胶温度结冷胶与淀粉的重量比为0.02～0.5。
  2. 权利要求1的淀粉成膜组合物，其中结冷胶总酰基中甘油酰基含量为12％-26％，和/或乙酰基含量为2％-8％。
  3. 权利要求1的淀粉成膜组合物，其中淀粉的含量为15wt％-50wt％。
  4. 权利要求1的淀粉成膜组合物，其中结冷胶的含量为1wt％-8wt％，优选地，结冷胶含量为2wt％-7wt％。
  5. 权利要求1-4任一所述的淀粉成膜组合物，其中所述淀粉为天然淀粉，所述天然淀粉选自小麦淀粉、蜡质玉米淀粉、豌豆淀粉、玉米淀粉、马铃薯淀粉和木薯淀粉中的一种或多种。
  6. 权利要求1-4任一所述的淀粉成膜组合物，其中所述淀粉为淀粉衍生物，所述淀粉衍生物是酸处理淀粉、羟丙基淀粉、氧化淀粉、醋酸酯淀粉、氧化羟丙基淀粉、羟丙基二淀粉磷酸酯、淀粉磷酸酯、辛烯基琥珀酸淀粉钠、乙酰化二淀粉磷酸酯和糊精中的一种或多种。
  7. 权利要求1的淀粉成膜组合物，该淀粉成膜组合物还包含增塑剂，所述增塑剂的含量为10wt％-35wt％，优选地，所述增塑剂选自甘油、山梨糖醇、麦芽糖醇、赤藓糖醇、木糖醇、果糖和海藻糖中一种或多种。
  8. 权利要求1的淀粉成膜组合物，该淀粉成膜组合物还包含第二胶凝剂，优选地，所述第二胶凝剂选自卡拉胶、琼脂、海藻酸钠、果胶、高酰基结冷胶、低酰基结冷胶、魔芋胶、黄原胶、刺槐豆胶、瓜尔胶和普鲁兰多糖中的一种或多种；优选地所述第二胶凝剂含量为0.2wt％-3.5wt％，优选地所述果胶是低甲氧基果胶、高甲氧基果胶和酰胺果胶中的一种或多种；优选地其中低甲氧基果胶具有DE<50％的酯化度，酰胺果胶具有DA 5％-25％的酰胺度。
  9. 权利要求1的淀粉成膜组合物，还包含35wt％-60wt％水。
  10. 使用权利要求7的淀粉成膜组合物制备胶囊壳的方法，其包括1)A)先将第一胶凝剂和增塑剂预混分散均匀，搅拌下加入到水中，在60～98℃下加热搅拌至第一胶凝剂溶解；B)加入淀粉，继续在60～98℃下加热搅拌至淀 粉溶解；C)除去气泡即得胶液；
    2)压丸；和
    3)干燥。
  11. 权利要求10的制备胶囊壳的方法，所述A)还包括加入第二胶凝剂；所述A)为第一胶凝剂、第二胶凝剂和增塑剂预混分散均匀，搅拌下加入到水中，在60～98℃下加热搅拌至第一胶凝剂和第二胶凝剂溶解。
  12. 包含权利要求1-9中任一项所述的淀粉成膜组合物的胶囊壳。
  13. 权利要求12的胶囊壳，该胶囊壳的含水量为8-25％。
  14. 权利要求1-9中任一项所述的淀粉成膜组合物在医药、食品或化妆品中的应用。
PCT/CN2021/142077 2020-12-31 2021-12-28 淀粉成膜组合物及其制备胶囊壳的方法 WO2022143667A1 (zh)

Priority Applications (5)

Application Number Priority Date Filing Date Title
CA3164901A CA3164901C (en) 2020-12-31 2021-12-28 Starch film-forming compositions and methods of their use for preparing capsule shells
US17/792,843 US20230051942A1 (en) 2020-12-31 2021-12-28 Starch film-forming compositions and methods of their use for preparing capsule shells
JP2022533233A JP2023512402A (ja) 2020-12-31 2021-12-28 デンプンフィルム形成用組成物およびそれを使用したカプセルシェルの製造方法
EP21914401.1A EP4074191A4 (en) 2020-12-31 2021-12-28 STARCH FILM-FORMING COMPOSITION AND CAPSULE SHELL PREPARATION METHOD
AU2021411017A AU2021411017B2 (en) 2020-12-31 2021-12-28 Starch film-forming composition and method for preparing capsule shell

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN202011619863.9 2020-12-31
CN202011619863.9A CN113768137B (zh) 2020-12-31 2020-12-31 淀粉成膜组合物及其制备胶囊壳的方法

Publications (1)

Publication Number Publication Date
WO2022143667A1 true WO2022143667A1 (zh) 2022-07-07

Family

ID=78835277

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/CN2021/142077 WO2022143667A1 (zh) 2020-12-31 2021-12-28 淀粉成膜组合物及其制备胶囊壳的方法

Country Status (7)

Country Link
US (1) US20230051942A1 (zh)
EP (1) EP4074191A4 (zh)
JP (1) JP2023512402A (zh)
CN (1) CN113768137B (zh)
AU (1) AU2021411017B2 (zh)
CA (1) CA3164901C (zh)
WO (1) WO2022143667A1 (zh)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113768137B (zh) * 2020-12-31 2023-01-20 仙乐健康科技股份有限公司 淀粉成膜组合物及其制备胶囊壳的方法
CN114424823B (zh) * 2022-01-20 2023-07-04 江苏海王健康生物科技有限公司 一种含天然提取物的降血脂软胶囊及其制备方法
CN114672072B (zh) * 2022-04-26 2023-07-04 仙乐健康科技股份有限公司 一种淀粉成膜组合物、软胶囊囊壳及其在软胶囊的应用
CN114642648B (zh) * 2022-04-26 2023-10-03 仙乐健康科技股份有限公司 一种淀粉成膜组合物及其在软胶囊的应用
CN114794430B (zh) * 2022-05-05 2023-05-30 安徽农业大学 一种蓝莓渣耐焙烤果酱及其制备方法
CN118141779A (zh) * 2024-05-08 2024-06-07 广东亿超生物科技有限公司 一种卡拉胶植物软胶囊皮的制备方法

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1663989A (zh) * 2004-03-02 2005-09-07 国家淀粉及化学投资控股公司 不同酰基结冷胶与淀粉的混合物
JP2007153851A (ja) 2005-12-08 2007-06-21 Maruichi Kasei Kk ソフトカプセル用皮膜組成物、ソフトカプセル及びその製造方法
CN1995115A (zh) * 2005-12-02 2007-07-11 国家淀粉及化学投资控股公司 凝胶化和非凝胶化淀粉与结冷胶和增塑剂的共混物
JP2009040716A (ja) * 2007-08-08 2009-02-26 Oyo Seikagaku Kenkyusho 軟カプセル皮膜組成物
EP2815745A1 (en) 2013-06-21 2014-12-24 Swiss Caps Rechte und Lizenzen AG Soft shell capsule and process for its manufacture
CN108659137A (zh) 2017-03-30 2018-10-16 帝斯曼知识产权资产管理有限公司 一种具有双凝胶温度的结冷胶及其生产方法和应用
CN113768137A (zh) * 2020-12-31 2021-12-10 仙乐健康科技股份有限公司 淀粉成膜组合物及其制备胶囊壳的方法

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1086140B1 (en) * 1998-06-10 2003-01-22 CP Kelco ApS Modified gellan gum composition process for preparation of same and use thereof
US20070034827A1 (en) * 2005-12-02 2007-02-15 Zhixin Li Blends of gelling and non-gelling starches with gellan gums and plasticizer
CN101406704B (zh) * 2008-11-25 2011-10-26 吴国庆 一种新型植物胶囊膜材料及其生产方法
JP2016199737A (ja) * 2015-04-10 2016-12-01 森永製菓株式会社 高分子多糖の改質方法、および、改質高分子多糖
CN111388442A (zh) * 2020-03-24 2020-07-10 广州普正生物科技有限公司 一种凝胶糖果型植物软胶囊
CN113332257B (zh) * 2021-06-28 2023-05-05 仙乐健康科技股份有限公司 软胶囊囊壳和软胶囊

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1663989A (zh) * 2004-03-02 2005-09-07 国家淀粉及化学投资控股公司 不同酰基结冷胶与淀粉的混合物
CN100528950C (zh) 2004-03-02 2009-08-19 布鲁诺布二世有限公司 不同酰基结冷胶与淀粉的混合物
CN1995115A (zh) * 2005-12-02 2007-07-11 国家淀粉及化学投资控股公司 凝胶化和非凝胶化淀粉与结冷胶和增塑剂的共混物
JP2007153851A (ja) 2005-12-08 2007-06-21 Maruichi Kasei Kk ソフトカプセル用皮膜組成物、ソフトカプセル及びその製造方法
JP2009040716A (ja) * 2007-08-08 2009-02-26 Oyo Seikagaku Kenkyusho 軟カプセル皮膜組成物
EP2815745A1 (en) 2013-06-21 2014-12-24 Swiss Caps Rechte und Lizenzen AG Soft shell capsule and process for its manufacture
US20160151243A1 (en) * 2013-06-21 2016-06-02 Swiss Caps Rechte Und Lizenzen Ag Soft shell capsule and process for its manufacture
CN108659137A (zh) 2017-03-30 2018-10-16 帝斯曼知识产权资产管理有限公司 一种具有双凝胶温度的结冷胶及其生产方法和应用
CN113768137A (zh) * 2020-12-31 2021-12-10 仙乐健康科技股份有限公司 淀粉成膜组合物及其制备胶囊壳的方法

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See also references of EP4074191A4

Also Published As

Publication number Publication date
EP4074191A1 (en) 2022-10-19
EP4074191A4 (en) 2024-04-10
AU2021411017A1 (en) 2022-08-25
CA3164901A1 (en) 2022-07-07
CN113768137A (zh) 2021-12-10
CA3164901C (en) 2024-04-09
CN113768137B (zh) 2023-01-20
JP2023512402A (ja) 2023-03-27
AU2021411017B2 (en) 2023-11-30
US20230051942A1 (en) 2023-02-16

Similar Documents

Publication Publication Date Title
WO2022143667A1 (zh) 淀粉成膜组合物及其制备胶囊壳的方法
WO2021136169A1 (zh) 含结冷胶和淀粉的成膜组合物及在软胶囊中应用
CA2272633C (en) Polymer film compositions for capsules
WO2023273254A1 (zh) 软胶囊囊壳和软胶囊
CA2807314C (en) Film-forming composition for soft capsules
EP4134071A1 (en) Soft capsule shell and soft capsule
WO2012070577A1 (ja) 軟カプセル皮膜
CN111040256A (zh) 制备淀粉基质空心胶囊的原料组合物及淀粉基质空心胶囊
CN104784148B (zh) 一种制备植物胶囊的成膜组合物及其制备方法
JP2011026262A (ja) ソフトカプセルの製造方法
WO2003011257A1 (en) Composition and process the manufacture of soluble containers with improved gel-strength
CN116919915B (zh) 一种双层软胶囊、制备方法和应用
CN117462510A (zh) 淀粉成膜组合物及其软胶囊的制备方法
CN115887405A (zh) 一种用于保健品封装的硬胶囊及其制备方法
CN115429771A (zh) 一种胶囊用复合胶及其制备方法和应用

Legal Events

Date Code Title Description
ENP Entry into the national phase

Ref document number: 2022533233

Country of ref document: JP

Kind code of ref document: A

WWE Wipo information: entry into national phase

Ref document number: 2021411017

Country of ref document: AU

ENP Entry into the national phase

Ref document number: 3164901

Country of ref document: CA

ENP Entry into the national phase

Ref document number: 2021914401

Country of ref document: EP

Effective date: 20220715

121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 21914401

Country of ref document: EP

Kind code of ref document: A1

ENP Entry into the national phase

Ref document number: 2021411017

Country of ref document: AU

Date of ref document: 20211228

Kind code of ref document: A

NENP Non-entry into the national phase

Ref country code: DE