EP3813765A1 - Staubfreie kalt wasserdispergierbare zubereitungen - Google Patents
Staubfreie kalt wasserdispergierbare zubereitungenInfo
- Publication number
- EP3813765A1 EP3813765A1 EP19727013.5A EP19727013A EP3813765A1 EP 3813765 A1 EP3813765 A1 EP 3813765A1 EP 19727013 A EP19727013 A EP 19727013A EP 3813765 A1 EP3813765 A1 EP 3813765A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- water
- hydrophobic
- particles according
- coated particles
- dispersant
- Prior art date
- Legal status (The legal status 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 status listed.)
- Pending
Links
Classifications
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- 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
- A23P10/40—Shaping or working of foodstuffs characterised by the products free-flowing powder or instant powder, i.e. powder which is reconstituted rapidly when liquid is added
- A23P10/47—Shaping or working of foodstuffs characterised by the products free-flowing powder or instant powder, i.e. powder which is reconstituted rapidly when liquid is added using additives, e.g. emulsifiers, wetting agents or dust-binding agents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/20—After-treatment of capsule walls, e.g. hardening
- B01J13/22—Coating
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- 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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/67—Vitamins
- A61K8/671—Vitamin A; Derivatives thereof, e.g. ester of vitamin A acid, ester of retinol, retinol, retinal
-
- 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
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
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- 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
- A61K8/0216—Solid or semisolid forms
- A61K8/022—Powders; Compacted Powders
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- 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
- A61K8/0241—Containing particulates characterized by their shape and/or structure
-
- 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
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/25—Silicon; Compounds thereof
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- 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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/34—Alcohols
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- 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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/37—Esters of carboxylic acids
- A61K8/375—Esters of carboxylic acids the alcohol moiety containing more than one hydroxy group
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- 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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/67—Vitamins
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- 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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/67—Vitamins
- A61K8/678—Tocopherol, i.e. vitamin E
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- 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
- A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
- A61K8/86—Polyethers
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- 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
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
- A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
- A61K9/1605—Excipients; Inactive ingredients
- A61K9/1611—Inorganic compounds
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- 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
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
- A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
- A61K9/1682—Processes
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- 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
- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
- A61K9/5005—Wall or coating material
- A61K9/501—Inorganic compounds
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- 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
- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
- A61K9/5005—Wall or coating material
- A61K9/5015—Organic compounds, e.g. fats, sugars
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- 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
- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
- A61K9/5073—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals having two or more different coatings optionally including drug-containing subcoatings
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
- B01J13/043—Drying and spraying
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- 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
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- 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
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/41—Particular ingredients further characterized by their size
- A61K2800/412—Microsized, i.e. having sizes between 0.1 and 100 microns
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- 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
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/60—Particulates further characterized by their structure or composition
- A61K2800/61—Surface treated
- A61K2800/612—By organic compounds
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- 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
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/60—Particulates further characterized by their structure or composition
- A61K2800/61—Surface treated
- A61K2800/62—Coated
- A61K2800/621—Coated by inorganic compounds
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- 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
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/60—Particulates further characterized by their structure or composition
- A61K2800/61—Surface treated
- A61K2800/62—Coated
- A61K2800/63—More than one coating
Definitions
- the present invention relates to a dust-free preparation which is cold water-dispersible, its production and use.
- a difficulty in the preparation of water-insoluble or sparingly water-soluble active ingredients, which according to the invention also include vitamin A, vitamin D, vitamin E and vitamin K-containing and derivatives thereof or carotenoid-containing preparations and mixtures of these preparations is that during the final drying process, which is carried out by spray agglomeration, they form blackberry-like, fragile, highly branched structures, whose average particle size is approx. 150 pm, which is extremely dusty and whose high fine fraction (particles ⁇ 100 pm ) continues to rise under mechanical stress due to the breaking of the highly fragile structures.
- the object of the present invention was to provide preparations which consist of largely dust-free, cold water-dispersible particles.
- This object is achieved by a preparation consisting of particles, the particles having at least one coating layer which contains one or more hydrophobic powdering agents as the main component and which surrounds the particle core containing the active ingredient.
- the proportion of this coating layer on the particle is preferably in the range from 0.5 to 8% by weight, preferably in the range from 0.8 to 6% by weight and particularly preferably in the range from 1 to 5% by weight.
- Suitable hydrophobic powdering agents according to the invention are finely divided oxides which have been rendered hydrophobic and in particular the hydrophobicized oxides of the elements silicon, aluminum or titanium or mixed oxides of these elements or mixtures of the oxides mentioned.
- the hydrophobicized pyrogenic or precipitated silica and in particular the hydrophobicized precipitated silica are preferred here.
- hydrophobicized oxides according to the invention and here in particular the hydrophobicized oxides of the elements silicon, aluminum or titanium, mixed oxides thereof and mixtures of the named oxides have a BET value of at least 80m 2 / g and / or an average particle diameter d50 of no longer than 20 pm. As a rule, the average particle diameter is between 10 nm and 20 pm.
- hydrophobicized pyrogenic or precipitated silicas with a BET value of at least 80 m 2 / g and / or an average particle diameter d50 of not more than 20 pm and here in particular the hydrophobized precipitated silica, as represented, for example, by the Sipernat D-17 with a BET value of 100 m 2 / g and an average particle diameter d50 of 10 pm, determined in accordance with laser diffraction ISO 13320-1 ,
- the coating layer made of hydrophobic powdering agent is preferably applied in such a way that it completely surrounds the particle core.
- the degree of occupancy of the particles is at least 70%, preferably at least 75% and particularly preferably at least 80% according to the SEM image evaluation, the particle core having an average particle diameter of 140-400 ⁇ m.
- the SEM images were taken with a Zeiss Ultra 55 device.
- Detector Topographic - see images with secondary electrons (at 8kV).
- the coating layer containing the hydrophobic powdering agent can be applied directly to the particle core or underlaid by one or more additional coating layers.
- the production produces largely dust-free particles which are distinguished by a low dust number of less than 15, but preferably have a dust number of less than 10 and particularly preferably one of less than 8.
- the dust number of the coated particles is determined with the aid of a dust measuring device type DustView II from Palas GmbH, Düsseldorf, DE.
- the device used for the measurement consists of a hopper with a flap, a downpipe and a dust housing with a removable dust box.
- the evaluation is optoelectronic, since the dusting solid content leads to the weakening of a light beam, this is recorded photometrically.
- the measured value registration and evaluation takes place in the control unit.
- the following measured values are displayed as numerical values on the control unit: 1.Measured value after 0.5 seconds (maximum value)
- the dust numbers are rated as follows: Dust number 25 - 100 dusting to heavily dusting Dust number 12 - 25 slightly dusting to dusting Dust number 8 - 12 lightly dusting Dust number ⁇ 8 quasi dust-free to dust-free.
- the particles obtained after coating with a hydrophobic powder meet the criterion of being dust-free, but are not water-dispersible due to the hydrophobic coating.
- a further substance hereinafter referred to as a dispersant
- the dispersant is absorbed by the hydrophobic coating layer, but can also form a further coating layer depending on the amount applied.
- the dispersant can be used to obtain particles whose spreading behavior in °, determined by contact angle measurement after 0.1 seconds at 25 ° C on a pellet made of pure powder, is present on Sipernat D17 compacts carried out, less than or equal to 75 °, preferably less than 70 ° and particularly preferably less than or equal to 60 °.
- dispersant or the dispersant mixture as the main component
- further substances can be added to the dispersant. However, if available, they should be selected so that the contact angle is not increased by more than 15% compared to the pure main component.
- the contact angle of the dispersant is determined on a Sipernat D17 compact. Substances liquid at room temperature are heated to 60 ° C at RT (25 ° C) and at RT highly viscous or semi-solid substances and then measured at RT. For this, a tropical drop the sample substance at RT using a disposable syringe (cannula diameter 1.65mm) from a height of 1.5cm onto the compact. The contact angle formed between the droplet and the compact is determined using the OCAH150plus from Dataphysics. For this purpose, the sessile drop method was set and the data determined by means of elliptical fitting was evaluated.
- Particles are obtained from the production which are distinguished by a dust number of less than 10, but preferably by a dust number of less than 8 and particularly preferably by a dust number of less than 5.
- suitable dispersants according to the invention are in particular those substances which, in addition to the spreading behavior described, have an HLB value of 0.5 to 13, preferably 1 to 12.5 and particularly preferably 1 to 5.5.
- Particularly preferred as the dispersing agent are MCT oil and / or propylene glycol monolaurate (lauroglycol FCC), that is to say hydrophobic substances which one would rather not expect to promote cold water dispersibility and / or lutensoles which show amphiphilic character.
- the proportion of dispersant in the total particle of the preparation is preferably in the range from 0.5 to 6% by weight, preferably 1 to 4.5% by weight and particularly preferably 1.5 to 3% by weight.
- the average diameter d50 of the coated particles produced is preferably ⁇ 400 pm.
- 140 ⁇ d50 ⁇ 300 pm applies, particularly preferably 150 ⁇ d50 ⁇ 275 pm.
- the d10 value of the total distribution of the size distribution curve of the granules used is preferably> 90 pm.
- 90 ⁇ d 10 ⁇ 125 pm applies, particularly preferably 95 ⁇ d10 ⁇ 1 10 pm.
- the d90 value of the total distribution of the size distribution curve of the granules used is preferably ⁇ 550 pm.
- 275 ⁇ d90 ⁇ 540pm applies, 285 ⁇ d90 ⁇ 500pm is particularly preferred.
- the particle sizes of the particles were determined in the context of the invention by laser diffraction using the Mastersizer 2000 device from Malvern. If a silicon-containing hydrophobic powder, such as the Sipernat D-17 and used to apply MCT- ⁇ I as a dispersant, the Si / MCT ratio, calculated from the quotient of g / 100g Si and% MCT, is in the range of 0.2 to 1.2, preferably 0.25 to 1.0 and particularly preferably 0.35 to 0.9.
- the Si content is determined using ICP-OES (optical emission spectroscopy with inductively coupled plasma) at wavelengths Si of 251 and 611 nm (measuring device: IP-OES Varian Vista 725-ES (radial).
- Another advantage of the particles according to the invention is not, or not to be foamed to any appreciable extent, for this purpose it is determined how quickly the foam formed when the particles are dispersed.
- 90g demineralized water are placed in a 250 ml beaker and tempered to a setpoint of 25 ° C in a water bath.
- 10 g of the corresponding particles are added and the mixture is stirred until no solid can be seen on the liquid surface.
- the magnetic stirrer is then removed and the batch is thoroughly mixed with the Ultra-Turrax for 2 minutes at speed 1 (4000 rpm). Care is taken to ensure that liquid and air get into the dispersing tool through the slot in the shaft.
- the foamy solution is transferred to a 250ml measuring cylinder and the initial volume is determined. Further readings are made based on the time of transfer after 10 minutes, as well as after 1, 2, 3 and 4 hours.
- the foam factor is calculated from the ratio of the total filling height, i.e. the total volume of foam and liquid divided by the volume of the liquid.
- the particles according to the invention are distinguished by the fact that they form an unstable foam when dispersed. The foam has almost completely degraded after just 1 hour of standing time, so that a foam factor of less than or equal to 1.2 is determined after 1 hour.
- water-insoluble or only sparingly water-soluble active substances are to be understood as substances whose saturation solubility at room temperature (25 ° C.) is less than 1% by weight in at least one of the following media: water, 0.1 molar aqueous hydrochloric acid, aqueous Phosphate buffer pH 7.2, 0.9% by weight aqueous saline.
- active substances and effect substances are considered as water-insoluble or sparingly water-soluble active substances, in particular pharmaceutical or cosmetic active substances, active substances for food supplements or dietetic agents or food additives.
- Poorly soluble substances in the sense of the invention are, for example: Piroxicam, clotrimazole, carbamazepine, 17-beta-estradiol, sulfathiazole, fenofibrate, benzocaine, lidocaine, dimethindene, biperiden, bisacodyl, clioquinol, droperidol, haloperidol, nifedipine, nit rendipine.
- the carotenoids ß carotene, canthaxanthin, astaxanthin, zeaxanthin, lutein, lycopene,
- the content of the water-insoluble or only sparingly water-soluble active ingredients in the preparations according to the invention is in the range from 0.1 to 60% by weight, preferably in the range from 0.2 to 50% by weight, particularly preferably in the range from 0, 5 to 25% by weight, very particularly preferably in the range from 1 to 20% by weight, based on the dry mass of the preparation.
- a content of 0.5 to 25% by weight is particularly preferred in the preparations according to the invention, very particularly preferably the content is preferably in the range from 1 to 20% by weight.
- Plant gums modified plant gums, gelatin, modified gelatin, starch, modified starch, lignin sulfonate, chitosan, carrageenan, casein, caseinate, whey protein, zein, modified cellulose, pectin, modified pectin, plant proteins and modified plant proteins are used as protective colloids or mixtures thereof.
- polyvinyl alcohol, polyvinyl pyrrolidone, methyl cellulose, carboxymethyl cellulose, hydroxypropyl cellulose and alginates can also be used.
- a plasticizer to the colloid, such as sugar or sugar alcohols, for example sucrose, glucose, lactose, invert sugar, sorbitol, mannitol, glycerol, palatinite or mixtures thereof.
- the ratio of colloid and plasticizer to carotenoid solution is generally chosen so that a dry product is obtained which contains between 3 and 20% by weight of an active ingredient, 10 to 50% by weight of a colloid, 20 to 70% by weight of a plasticizer.
- stabilizers such as a-tocopherol -Butyl-hydroxytoluene, t-butyl-hydroxyanisole, ascorbic acid, propyl gallate or ethoxyquine.
- emulsifiers for example ascorbyl palmitate, polyglycerol fatty acid esters, sorbitan fatty acid esters, propylene glycol fatty acid esters or lecithin, can be obtained in a concentration of 0 to 200% by weight, preferably 5 to 150% by weight, particularly preferably 10 to 80% by weight be used on the active ingredient.
- a physiologically approved oil such as sesame oil, corn oil, cottonseed oil, soybean oil or peanut oil and esters of medium-chain vegetable fatty acids in a concentration of 0 to 500% by weight, preferably 10 to 300% by weight preferably 20 to 100% by weight, based on the active ingredient.
- the present invention also relates to processes for the preparation of the preparations according to the invention.
- the process comprises the following steps:
- water-miscible, thermally stable, volatile solvents containing only carbon, hydrogen and oxygen such as alcohols, ethers, esters, ketones and acetals
- solvents which are at least 10% water-miscible, have a boiling point below 200 ° C. and / or have less than 10 carbons.
- a deep-colored viscous liquid is obtained after process step b) or b2).
- the solvent can be removed, for example, by extraction with a water-immiscible solvent or, depending on the boiling point, in a manner known per se, e.g. by distillation, if appropriate under reduced pressure.
- the azeotrope obtained when using isopropanol is used directly as a solvent without removing water.
- the solvent is preferably removed together with the removal of the water by spray drying or spray granulation.
- the powdered preparation according to the invention is suitable, inter alia, as an additive to food preparations, for example for coloring foodstuffs such as beverages, as an agent for the production of pharmaceutical and cosmetic preparations and for the production of nutritional supplements, for example multivitamin preparations in the human and animal sectors.
- Another object of the present invention is the use of the powdered formulation according to the invention described above as an additive to animal feed, food, food supplements, personal care products or pharmaceutical agents.
- the present invention likewise relates to animal feed, food, food supplements, personal care products or pharmaceutical compositions which contain the powdered preparation according to the invention.
- Astaxanthin, ascorbyl palmitate and tocopherol are dissolved in an azeotropic mixture of water and isopropanol at a temperature of 100 ° C to 200 ° C and a pressure between 20 bar and 100 bar within less than 10 seconds.
- the batch from 2. is mixed with about 1% NaOH.
- Isopropanol and parts of the water are removed in a multi-stage evaporation at pressures below atmospheric pressure, so that a 15 to 65 percent by weight (suspension) dispersion is formed.
- This dispersion is injected together with hydrophobic silica at the top of a spray tower, forming fine drops which are enveloped by hydrophobic silica.
- the coated free-flowing particles obtained according to the invention as the end product have a dust value of 2.4 and a D50 of 170pm.
- the silicon content is 1.4%
- the MCT content 2.4% which corresponds to a ratio of Si in% to MCT in% of 0.58.
- the contact angle of the particles measured after 0.1 seconds and 25 ° C against the surface of a Siper- nate D17 compact is 54 °.
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Epidemiology (AREA)
- Engineering & Computer Science (AREA)
- Birds (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Organic Chemistry (AREA)
- Pharmacology & Pharmacy (AREA)
- Medicinal Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Polymers & Plastics (AREA)
- Food Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Dispersion Chemistry (AREA)
- Emergency Medicine (AREA)
- Mycology (AREA)
- Nutrition Science (AREA)
- Dermatology (AREA)
- Cosmetics (AREA)
- Medicinal Preparation (AREA)
- Fodder In General (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- General Preparation And Processing Of Foods (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
Description
Claims
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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EP18180115 | 2018-06-27 | ||
PCT/EP2019/063894 WO2020001906A1 (de) | 2018-06-27 | 2019-05-29 | Staubfreie kalt wasserdispergierbare zubereitungen |
Publications (1)
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EP3813765A1 true EP3813765A1 (de) | 2021-05-05 |
Family
ID=62814860
Family Applications (1)
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EP19727013.5A Pending EP3813765A1 (de) | 2018-06-27 | 2019-05-29 | Staubfreie kalt wasserdispergierbare zubereitungen |
Country Status (6)
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US (1) | US11980218B2 (de) |
EP (1) | EP3813765A1 (de) |
JP (1) | JP2021528085A (de) |
KR (1) | KR20210023890A (de) |
CN (1) | CN112292109A (de) |
WO (1) | WO2020001906A1 (de) |
Family Cites Families (16)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1603640A (en) | 1977-07-20 | 1981-11-25 | Gist Brocades Nv | Enzyme particles |
US4486435A (en) | 1983-05-16 | 1984-12-04 | Basf Wyandotte Corporation | Spray-dried vitamin powders using hydrophobic silica |
DE4120918A1 (de) | 1991-06-25 | 1993-01-07 | Basf Ag | Pulverfoermige praeparate aus einer wasserunloeslichen kernsubstanz und einer schutzhuelle |
US6221921B1 (en) * | 1999-10-14 | 2001-04-24 | Advanced Ceramics Research, Inc. | Dispersant system and process for formulating non-aqueous siliceous particulate slurries |
US7105176B2 (en) * | 2000-11-29 | 2006-09-12 | Basf Aktiengesellschaft | Production of solid preparations of water-soluble, sparingly water-soluble or water-insoluble active compounds |
DE10158046A1 (de) * | 2001-11-27 | 2003-06-05 | Basf Ag | Formulierung für den Einsatz in Lebensmitteln, Nahrungsergänzungsmitteln, Futtermitteln, Futterzusatzstoffen, pharmazeutischen und kosmetischen Zubereitungen sowie Verfahren zu deren Herstellung |
DE10311585A1 (de) | 2003-03-14 | 2004-09-23 | Basf Ag | Wirkstoffhaltige Adsorbate |
EP1574534A1 (de) | 2004-03-11 | 2005-09-14 | Rohm And Haas Company | Polymerträger und deren Verwendung |
JP2009536165A (ja) | 2006-05-10 | 2009-10-08 | エボニック デグサ ゲーエムベーハー | 医薬組成物におけるロール圧縮された熱分解的に製造された二酸化ケイ素の使用 |
CA2677185C (en) * | 2007-02-01 | 2013-12-03 | Ofer Toledano | Method for preparing particles comprising metal oxide coating and particles with metal oxide coating |
CN102470112A (zh) | 2009-07-30 | 2012-05-23 | 赢创罗姆有限公司 | 包含阴离子聚合物材料和含6-22个碳原子的饱和单羧酸的盐的组合物 |
EP2910237B1 (de) | 2012-10-17 | 2018-07-04 | Sakai Chemical Industry Co., Ltd. | Oberflächenbehandelte kugelförmige calciumcarbonatteilchen für kosmetika und verfahren zur herstellung davon |
JP5711720B2 (ja) | 2012-11-13 | 2015-05-07 | 株式会社 資生堂 | 油中水型乳化日焼け止め化粧料 |
GB201319791D0 (en) | 2013-11-08 | 2013-12-25 | Sigmoid Pharma Ltd | Formulations |
US20190090529A1 (en) | 2016-03-02 | 2019-03-28 | Basf Se | Vibration droplet formation |
US20190231669A1 (en) | 2016-10-11 | 2019-08-01 | Dsm Ip Assets B.V. | Cosmetic compositions |
-
2019
- 2019-05-29 WO PCT/EP2019/063894 patent/WO2020001906A1/de unknown
- 2019-05-29 KR KR1020207037275A patent/KR20210023890A/ko not_active Application Discontinuation
- 2019-05-29 CN CN201980038388.5A patent/CN112292109A/zh active Pending
- 2019-05-29 US US17/256,385 patent/US11980218B2/en active Active
- 2019-05-29 JP JP2020572651A patent/JP2021528085A/ja active Pending
- 2019-05-29 EP EP19727013.5A patent/EP3813765A1/de active Pending
Also Published As
Publication number | Publication date |
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CN112292109A (zh) | 2021-01-29 |
US20210153540A1 (en) | 2021-05-27 |
KR20210023890A (ko) | 2021-03-04 |
US11980218B2 (en) | 2024-05-14 |
JP2021528085A (ja) | 2021-10-21 |
WO2020001906A1 (de) | 2020-01-02 |
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