DE10013312A1 - Production of oily suspensions of water soluble vitamins comprises milling of vitamins in oil or dry milling and suspension in oil - Google Patents
Production of oily suspensions of water soluble vitamins comprises milling of vitamins in oil or dry milling and suspension in oilInfo
- Publication number
- DE10013312A1 DE10013312A1 DE10013312A DE10013312A DE10013312A1 DE 10013312 A1 DE10013312 A1 DE 10013312A1 DE 10013312 A DE10013312 A DE 10013312A DE 10013312 A DE10013312 A DE 10013312A DE 10013312 A1 DE10013312 A1 DE 10013312A1
- Authority
- DE
- Germany
- Prior art keywords
- vitamin
- oil
- oily suspensions
- water
- vitamins
- 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.)
- Withdrawn
Links
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- 229940088594 vitamin Drugs 0.000 title claims abstract description 50
- 229930003231 vitamin Natural products 0.000 title claims abstract description 49
- 235000013343 vitamin Nutrition 0.000 title claims abstract description 49
- 239000000725 suspension Substances 0.000 title claims abstract description 45
- 238000003801 milling Methods 0.000 title claims abstract description 10
- 238000004519 manufacturing process Methods 0.000 title abstract description 3
- 238000009837 dry grinding Methods 0.000 title abstract 2
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- 150000003722 vitamin derivatives Chemical class 0.000 claims abstract description 15
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- UIERGBJEBXXIGO-UHFFFAOYSA-N thiamine mononitrate Chemical compound [O-][N+]([O-])=O.CC1=C(CCO)SC=[N+]1CC1=CN=C(C)N=C1N UIERGBJEBXXIGO-UHFFFAOYSA-N 0.000 description 1
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- ZCIHMQAPACOQHT-ZGMPDRQDSA-N trans-isorenieratene Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/c1c(C)ccc(C)c1C)C=CC=C(/C)C=Cc2c(C)ccc(C)c2C ZCIHMQAPACOQHT-ZGMPDRQDSA-N 0.000 description 1
- UFTFJSFQGQCHQW-UHFFFAOYSA-N triformin Chemical compound O=COCC(OC=O)COC=O UFTFJSFQGQCHQW-UHFFFAOYSA-N 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
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- 239000011719 vitamin A Substances 0.000 description 1
- 150000003700 vitamin C derivatives Chemical class 0.000 description 1
- MECHNRXZTMCUDQ-RKHKHRCZSA-N vitamin D2 Chemical compound C1(/[C@@H]2CC[C@@H]([C@]2(CCC1)C)[C@H](C)/C=C/[C@H](C)C(C)C)=C\C=C1\C[C@@H](O)CCC1=C MECHNRXZTMCUDQ-RKHKHRCZSA-N 0.000 description 1
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- QUEDXNHFTDJVIY-DQCZWYHMSA-N γ-tocopherol Chemical compound OC1=C(C)C(C)=C2O[C@@](CCC[C@H](C)CCC[C@H](C)CCCC(C)C)(C)CCC2=C1 QUEDXNHFTDJVIY-DQCZWYHMSA-N 0.000 description 1
- 239000002446 δ-tocopherol Substances 0.000 description 1
Classifications
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- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
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- A61K8/044—Suspensions
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/10—Organic substances
- A23K20/174—Vitamins
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K40/00—Shaping or working-up of animal feeding-stuffs
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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- A23K40/30—Shaping or working-up of animal feeding-stuffs by encapsulating; by coating
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- 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
- A23L33/15—Vitamins
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- A61K31/33—Heterocyclic compounds
- A61K31/335—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin
- A61K31/365—Lactones
- A61K31/375—Ascorbic acid, i.e. vitamin C; Salts thereof
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- A61K31/33—Heterocyclic compounds
- A61K31/395—Heterocyclic compounds having nitrogen as a ring hetero atom, e.g. guanethidine or rifamycins
- A61K31/435—Heterocyclic compounds having nitrogen as a ring hetero atom, e.g. guanethidine or rifamycins having six-membered rings with one nitrogen as the only ring hetero atom
- A61K31/44—Non condensed pyridines; Hydrogenated derivatives thereof
- A61K31/4415—Pyridoxine, i.e. Vitamin B6
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- A61K31/495—Heterocyclic compounds having nitrogen as a ring hetero atom, e.g. guanethidine or rifamycins having six-membered rings with two or more nitrogen atoms as the only ring heteroatoms, e.g. piperazine or tetrazines
- A61K31/505—Pyrimidines; Hydrogenated pyrimidines, e.g. trimethoprim
- A61K31/519—Pyrimidines; Hydrogenated pyrimidines, e.g. trimethoprim ortho- or peri-condensed with heterocyclic rings
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- A61K31/59—Compounds containing 9, 10- seco- cyclopenta[a]hydrophenanthrene ring systems
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- A61K31/70—Carbohydrates; Sugars; Derivatives thereof
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- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
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- A—HUMAN NECESSITIES
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- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
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- 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
Abstract
Description
Die Erfindung betrifft ölige Suspensionen mindestens eines wasserlöslichen Vitamins sowie ein Verfahren zur Herstellung dieser Suspensionen und deren Verwendung als Zusatz zu Lebens mitteln, Tierfuttermitteln, Pharmazeutika und kosmetischen Zu bereitungen.The invention relates to oily suspensions of at least one water-soluble vitamin and a method of preparation of these suspensions and their use as an adjunct to life medications, animal feed, pharmaceuticals and cosmetics preparations.
Die Verwendung von Vitaminen als Futtermittelzusatzstoffe in der Tierernährung erfolgt mehr und mehr in Form flüssiger Zuberei tungen. Dies hat u. a. den Vorteil, daß die Dosierung einfacher und genauer erfolgen kann. Ferner ist es möglich, bei der soge nannten "post-pellet-application" beispielsweise Futtermittel pellets erst nach deren Herstellung mit einer flüssigen Zuberei tung von Futtermittelzusatzstoffen zu beladen. Dies hat zur Folge, daß selbst oxidations- und temperaturempfindliche Zusatz stoffe wie Vitamine oder Carotinoide ohne größere Verluste einge setzt werden können.The use of vitamins as feed additives in the Animal nutrition is more and more in the form of liquid Zuberei obligations. This has u. a. the advantage that the dosage easier and more accurately. Furthermore, it is possible in the soge For example, "post-pellet-application" called feed Pellets only after their preparation with a liquid Zuberei load of feed additives. This has to Episode that even oxidation and temperature sensitive addition substances such as vitamins or carotenoids without major losses can be set.
Beispiele für "post-pelleting-application" (PPA) finden sich u. a. in GB-A-2 232 573 sowie in EP-A-0 556 883 und der darin zitierten Literatur.Examples of "post-pelleting-application" (PPA) are u. a. in GB-A-2 232 573 and in EP-A-0 556 883 and the cited therein Literature.
Eine bislang noch kritische Anwendung ist die Verabreichung flüs siger Formulierungen von wasserlöslichen Vitaminen in Kombination mit Mineralien und fettlöslichen Vitaminen. Hier kann es durch gegenseitige Wechselwirkungen zu unerwünschten Wirkstoffverlusten kommen.A hitherto still critical application is administration of liquid siger formulations of water-soluble vitamins in combination with minerals and fat-soluble vitamins. Here it can through mutual interactions to undesired drug losses come.
EP-A-0 772 978 beschreibt eine Mischung derartiger Substanzen, bei denen die Vitamine und Mineralien separat aufbewahrt und erst kurz vor der Applikation gemischt werden. Nachteilig bei dieser Vorgehensweise ist die erforderliche Bereitstellung entsprechen der Lagerbehälter, verbunden mit einer aufwendigen Logistik.EP-A-0 772 978 describes a mixture of such substances, in which the vitamins and minerals stored separately and only to be mixed shortly before the application. A disadvantage of this Approach is to meet the required deployment the storage container, combined with a complex logistics.
Vitamin-Emulsionen - als spezielle Form einer flüssigen Formulie rung - haben häufig den Nachteil, daß sie physikalisch (Auftreten von Phasentrennung) und chemisch (Auftreten von unerwünschten Hydrolyse- und/oder Redox-Reaktionen, chemische Inkompatibilität einzelner gelöster Komponenten) instabil sind und zusätzlich häufig die Gefahr einer mikrobiologischen Kontamination auftreten kann. Vitamin emulsions - as a special form of a liquid formula tion - often have the disadvantage that they are physically (occurrence of phase separation) and chemical (occurrence of undesired Hydrolysis and / or redox reactions, chemical incompatibility individual dissolved components) are unstable and in addition often the risk of microbiological contamination occur can.
Ferner sind Systeme bekannt, bei denen u. a. wasserlösliche Vita mine in Ölen oder Fetten dispergiert vorliegen.Furthermore, systems are known in which u. a. water-soluble Vita mine dispersed in oils or fats.
So beschreibt GB-A-1 358 401 die Herstellung von Lebensmittel supplementen basierend auf eßbaren Hartfetten mit Schmelzpunkten von 37 bis 121°C. Den geschmolzenen Hartfetten werden dabei unter Rühren feinverteilte assimilierbare eisenhaltige Substanzen zuge geben. Die homogene Dispersion wird anschließend zu Hartfett pellets sprühgekühlt. Optionell können zudem auch Mikronährstoffe und Vitamine eingearbeitet werden. Eine Anwendung in flüssiger Form ist mit den hier genannten Hartfetten nur bei erhöhter Temperatur möglich, was verfahrenstechnisch aufwendig ist und bei der Verwendung von Vitaminen häufig mit der Gefahr unerwünschter Wirkstoffverluste verbunden ist.Thus, GB-A-1 358 401 describes the production of food supplements based on edible hard fats with melting points from 37 to 121 ° C. The molten hard fats are doing under Stirring finely divided assimilable iron-containing substances added give. The homogeneous dispersion then becomes hard fat pellets are spray-cooled. Optionally, micronutrients can also be added and vitamins are incorporated. An application in liquid Shape is only with elevated with the Hartfetten mentioned here Temperature possible, which is procedurally complex and at the use of vitamins often with the risk of unwanted Drug losses is connected.
Es war daher die Aufgabe der vorliegenden Erfindung, stabile flüssige Formulierungen wasserlöslicher Vitamine bereitzustellen, die die oben genannten Nachteile des Standes der Technik nicht aufweisen.It was therefore the object of the present invention to provide stable to provide liquid formulations of water-soluble vitamins, not the above-mentioned disadvantages of the prior art respectively.
Diese Aufgabe wurde erfindungsgemäß gelöst durch ein Verfahren zur Herstellung öliger Suspensionen wasserlöslicher Vitamine, dadurch gekennzeichnet, daß man mindestens ein wasserlösliches Vitamin in mindestens einem eßbaren Öl bis auf eine mittlere Partikelgröße von 0,1 bis 100 µm mahlt.This object has been achieved by a method for the preparation of oily suspensions of water-soluble vitamins, characterized in that at least one water-soluble Vitamin in at least one edible oil except for one medium Particle size of 0.1 to 100 microns milled.
Bei den wasserlöslichen Vitaminen handelt es sich insbesondere um Ascorbinsäure und deren Salze wie Natriumascorbat sowie Vitamin C-Derivate wie Natrium-, Calcium- oder Magnesium-ascorbyl-2-mono phosphat oder Calcium-ascorbyl-2-polyphosphat, Calcium-panto thenat, Panthenol, Vitamin B1 (Thiamin) - als Hydrochlorid, Nitrat oder Pyrophosphat, Vitamin B2 (Riboflavin) und deren Phosphate, Vitamin B6 und Salze, Vitamin B12, Biotin, Folsäure und Folsäure derivate wie Tetrahydrofolsäure, 5-Methyltetrahydrofolsäure, 5-Formyltetrahydrofolsäure, Nicotinsäure und Nicotinsäureamid.The water-soluble vitamins are in particular ascorbic acid and its salts such as sodium ascorbate and vitamin C derivatives such as sodium, calcium or magnesium ascorbyl-2-mono-phosphate or calcium ascorbyl-2-polyphosphate, calcium pantothenate, panthenol , Vitamin B 1 (thiamine) - as hydrochloride, nitrate or pyrophosphate, vitamin B 2 (riboflavin) and its phosphates, vitamin B 6 and salts, vitamin B 12 , biotin, folic acid and folic acid derivatives such as tetrahydrofolic acid, 5-methyltetrahydrofolic acid, 5- Formyltetrahydrofolic acid, nicotinic acid and nicotinic acid amide.
Als wasserlösliches Vitamin sei in diesem Zusammenhang auch Vita min K3 (Menadion) als Natriumbisulfit genannt.As a water-soluble vitamin in this context also Vita min K 3 (menadione) is called sodium bisulfite.
Die oben genannten wasserlöslichen Vitamine können sowohl in kristalliner Form mit einer Reinheit größer 90%, bevorzugt größer 95%, besonders bevorzugt größer 98%, als auch in formulierter Form, beispielsweise als Granulat, Beadlet oder als sprühgetrock netes Pulver eingesetzt werden. Bevorzugt sind die o. g. Vitamine in ihrer kristallinen Form. The above-mentioned water-soluble vitamins can be found both in crystalline form with a purity greater than 90%, preferably greater 95%, more preferably greater than 98%, as well as formulated Form, for example as granules, beadlet or sprayed netes powder are used. Preferably, the o. G. vitamins in their crystalline form.
Als eßbare Öle kommen in der Regel alle physiologisch unbedenk lichen Öle - sowohl pflanzlichen als auch tierischen Ursprungs - in Frage, insbesondere solche Öle, die bei 20°C flüssig sind bzw. die in der Suspension bei 20°C allein oder zusammen mit anderen Ölen die flüssige Phase bilden. Bevorzugt zu nennen sind in die sem Zusammenhang Sonnenblumenöl, Palmöl, Sesamöl, Maiskeimöl, Baumwollsaatöl, Sojabohnenöl oder Erdnußöl, Ester mittelkettiger Triglyceride sowie außerdem Fischöle wie beispielsweise Makre len-, Sprotten- oder Lachsöl. Für die Tierernährung besonders bevorzugt sind Fischöle, Maiskeimöl, Sonnenblumenöl und Erdnußöl. Für den Food-/Pharmabereich zusätzlich von Vorteil sind die Ester mittelkettiger Triglyceride.As edible oils are usually all physiologically acceptable oils - both vegetable and animal origin - in question, in particular those oils which are liquid at 20 ° C or in the suspension at 20 ° C alone or together with others Oils form the liquid phase. Preferred to be mentioned in the sunflower oil, palm oil, sesame oil, corn oil, Cottonseed oil, soybean oil or peanut oil, ester medium chain Triglycerides and also fish oils such as macrolides lemon, sprat or salmon oil. Especially for animal nutrition preferred are fish oils, corn oil, sunflower oil and peanut oil. For the food / pharmaceutical sector additionally advantageous are the esters medium chain triglycerides.
Als eßbares Öl im Sinne der Erfindung sind auch Vitamin E, Vita min E-Derivate oder Mischungen davon zu verstehen. Die Bezeich nung Vitamin E steht in diesem Zusammenhang für natürliches oder synthetisches α-, β-, γ- oder δ-Tocopherol, bevorzugt für natürli ches oder synthetisches α-Tocopherol sowie für Tocotrienol. Vita min E-Derivate sind z. B. Tocopheryl-C1-C20-Alkylester wie Toco pherylacetat oder Tocopherylpalmitat.As edible oil in the context of the invention are also vitamin E, Vita min E derivatives or mixtures thereof to understand. The term vitamin E in this context means natural or synthetic α-, β-, γ- or δ-tocopherol, preferably natural or synthetic α-tocopherol and also tocotrienol. Vita min e-derivatives are z. As tocopheryl-C 1 -C 20 alkyl esters such as Toco pherylacetat or tocopheryl palmitate.
Vitamin E und/oder deren Derivate können dabei allein oder zu sammen mit den anderen eßbaren Ölen als Dispergiermedium verwen det werden.Vitamin E and / or their derivatives may be alone or too together with the other edible oils as dispersing medium verwen be.
Die Mahlung kann in an sich bekannter Weise z. B. mit einer Kugel mühle erfolgen. Dabei wird je nach verwendetem Mühlentyp so lange gemahlen, bis die suspendierten Teilchen eine über Fraunhofer Beugung ermittelte mittlere Partikelgröße D[4,3] von 0,1 bis 100 µm, bevorzugt 0,2 bis 50 µm, besonders bevorzugt 0,5 bis 30 µm, ganz besonders bevorzugt 0,8 bis 20 gm, insbesondere 1,0 bis 10 µm aufweisen. Der Begriff D[4,3] bezeichnet den volumen gewichteten mittleren Durchmesser (siehe Handbuch zu Malvern Ma stersizer S, Malvern Instruments Ltd., UK).The grinding can be done in a conventional manner z. B. with a ball mill. Depending on the used mill type so long milled until the suspended particles are above Fraunhofer Diffraction determined mean particle size D [4,3] from 0.1 to 100 microns, preferably 0.2 to 50 microns, more preferably 0.5 to 30 microns, most preferably 0.8 to 20 gm, in particular 1.0 have up to 10 microns. The term D [4,3] denotes the volume weighted mean diameter (see Malvern Ma Stersizer S, Malvern Instruments Ltd., UK).
Nähere Einzelheiten zur Mahlung und den dafür eingesetzten Appa raturen finden sich u. a. in Ullmann's Encyclopedia of Industrial Chemistry, Sixth Edition, 1999, Electronic Release, Size Reduc tion, Kapitel 3.6.: Wet Grinding.Further details on grinding and the Appa used raturen can be found u. a. in Ullmann's Encyclopedia of Industrial Chemistry, Sixth Edition, 1999, Electronic Release, Size Reduc tion, chapter 3.6 .: Wet Grinding.
Bei dem erfindungsgemäßen Mahlverfahren ist es möglich, alle in der Suspension verwendeten Komponenten aus der Gruppe der wasser löslichen Vitamine als Gesamtmischung zu mahlen. Es kann aber auch jede einzelne zu mahlende Komponente in hoher Konzentration in dem zu verwendenden Öl gemahlen werden. Die Endzubereitung ergibt sich dann durch eine Abmischung der jeweiligen Einzel suspensionen.In the grinding method according to the invention, it is possible to use all in The suspension used components from the group of water to grind soluble vitamins as a total mixture. But it can also every single component to be milled in high concentration are ground in the oil to be used. The final preparation then results from a mixture of the respective individual suspensions.
Die erfindungsgemäße Zubereitung kann vor der Anwendung mit Fetten oder Ölen auf die jeweilige Gebrauchskonzentration ver dünnt werden.The preparation according to the invention may be mixed with before use Fats or oils to the respective concentration of use ver be thinned.
Eine besondere Ausführungsform des erfindungsgemäßen Verfahrens ist dadurch gekennzeichnet, daß die Mahlung in Abwesenheit eines Emulgators erfolgt. Überraschenderweise wurde dabei festgestellt, daß sich auch ohne Zusatz eines Tensids feinteilige, homogene Suspensionen wasserlöslicher Vitamine in Ölen herstellen lassen, die auch in hohen Konzentrationen sedimentationsstabil sind.A particular embodiment of the method according to the invention characterized in that the grinding in the absence of Emulsifier takes place. Surprisingly, it was found that even without the addition of a surfactant finely divided, homogeneous Make suspensions of water-soluble vitamins in oils, which are sedimentation-stable even in high concentrations.
Eine weitere vorteilhafte Ausführungsform des erfindungsgemäßen Verfahrens ist dadurch gekennzeichnet, daß die Mahlung in Abwe senheit eines Schutzkolloids erfolgt.A further advantageous embodiment of the invention Method is characterized in that the grinding in Abwe the severity of a protective colloid.
Trotz Fehlen der o. g. Dispergier- bzw. Formulierhilfsmittel konn ten die an sich hydrophilen Vitamine - für den Fachmann uner wartet - ohne Benetzungsprobleme und Agglomeratbildung in den o. g. hydrophoben Dispergiermedien feinstgemahlen werden.Despite the lack of o. G. Dispersing or formulation aids konn The in itself hydrophilic vitamins - for the expert uner waits - without wetting problems and agglomeration in the o. g. hydrophobic dispersing media are micromilled.
Aufgrund der feinteiligen Verteilung der dispergierten wasser löslichen Vitamine zeichnen sich die nach dem erfindungsgemäßen Verfahren hergestellten öligen Suspensionen durch eine hohe Bio verfügbarkeit der in der Suspension enthaltenen Wirkstoffe aus.Due to the finely divided distribution of the dispersed water soluble vitamins are distinguished by the invention Method produced oily suspensions by a high bio availability of the active substances contained in the suspension.
Neben den eingangs genannten wasserlöslichen Vitaminen können vor, während oder nach der Mahlung zusätzliche fettlösliche Vita mine, wie z. B. die K-Vitamine, Vitamin A und Derivate wie Vitamin A-Acetat, Vitamin A-Propionat oder Vitamin A-Palmitat, Vitamin D2 und Vitamin D3 sowie die bereits genannten E-Vitamine in die ölige Suspension eingetragen und gelöst werden. Bevorzugt erfolgt die Mahlung in Gegenwart fettlöslicher Vitamine.In addition to the water-soluble vitamins mentioned above, before, during or after the grinding additional fat-soluble Vita mine such. As the K vitamins, vitamin A and derivatives such as vitamin A acetate, vitamin A propionate or vitamin A palmitate, vitamin D 2 and vitamin D 3 and the aforementioned E-vitamins are added to the oily suspension and dissolved. The grinding preferably takes place in the presence of fat-soluble vitamins.
Gegenstand der Erfindung sind auch ölige Suspensionen mindestens eines wasserlöslichen Vitamins, erhältlich nach einem Verfahren, das dadurch gekennzeichnet ist, daß man mindestens ein wasserlös liches Vitamin in mindestens einem eßbaren Öl bis auf eine mitt lere Partikelgröße von 0,1 bis 100 µm mahlt.The invention also oily suspensions are at least a water-soluble vitamin obtainable by a process which is characterized in that at least one wasserlös Vitamin L in at least one edible oil except for one Particle size of 0.1 to 100 microns milled.
Die erfindungsgemäßen öligen Suspensionen enthalten dabei 5 bis 70 Gew.-%, bevorzugt 5 bis 60 Gew.-%, besonders bevorzugt 10 bis 55 Gew.-% ganz besonders bevorzugt 15 bis 50 Gew.-% mindestens eines der eingangs genannten wasserlöslichen Vitamine in feinst vermahlener Form.The oily suspensions of the invention contain 5 to 70 wt .-%, preferably 5 to 60 wt .-%, particularly preferably 10 bis 55% by weight, very particularly preferably 15 to 50% by weight, at least one of the aforementioned water-soluble vitamins in fine milled form.
Außerdem können die öligen Suspensionen zusätzlich 0,5 bis 60 Gew.-%, bevorzugt 5 bis 50 Gew.-%, besonders bevorzugt 10 bis 45 Gew.-%, ganz besonders bevorzugt 15 bis 40 Gew.-% mindestens eines der eingangs genannten fettlöslichen Vitamine in gelöster Form enthalten.In addition, the oily suspensions may additionally 0.5 to 60 wt .-%, preferably 5 to 50 wt .-%, particularly preferably 10 bis 45 wt .-%, most preferably 15 to 40 wt .-% at least one of the aforementioned fat-soluble vitamins in dissolved Form included.
Darüberhinaus können die öligen Zubereitungen zusätzlich minde stens ein weiteres Carotinoid enthalten.In addition, the oily preparations may additionally reduce contain at least one other carotenoid.
Unter Carotinoide sind z. B. folgende Verbindungen zu verstehen: β-Carotin, Lycopin, Lutein, Astaxanthin, Zeaxanthin, Crypto xanthin, Citranaxanthin, Canthaxanthin, Bixin, β-Apo-4-carotinal, β-Apo-8-carotinal, β-Apo-8-carotinsäureester, einzeln oder als Mischung. Bevorzugt verwendete Carotinoide sind β-Carotin, Lyco pin, Lutein, Astaxanthin, Zeaxanthin, Citranaxanthin und Cantha xanthin.Under carotenoids z. For example, to understand the following compounds: β-carotene, lycopene, lutein, astaxanthin, zeaxanthin, crypto xanthine, citranaxanthin, canthaxanthin, bixin, β-apo-4-carotenal, β-apo-8-carotenal, β-apo-8-carotenoic acid ester, individually or as Mixture. Preferred carotenoids are β-carotene, Lyco pin, lutein, astaxanthin, zeaxanthin, citranaxanthin and cantha xanthine.
Die Carotinoide können dabei in kristalliner Form oder als Formu lierung - beispielsweise als Trockenpulver, gemäß EP-A-0 065 193 eingesetzt werden.The carotenoids can be in crystalline form or as Formu lation - for example as a dry powder, according to EP-A-0 065 193 be used.
Vorteilhafterweise werden die Carotinoide in der Regel in kri stalliner Form zusammen mit den wasserlöslichen Vitaminen in dem Öl gemahlen. Im Falle von Astaxanthin und Canthaxanthin werden bevorzugt Astaxanthin- bzw. Canthaxanthin-haltige Trockenpulver, beispielsweise Lucantin® Pink bzw. Lucantin® Rot (ein 10%iges Astaxanthin- bzw. Canthaxanthin-Trockenpulver, Fa. BASF AG, Ludwigshafen, Deutschland) zusammen mit den wasserlöslichen Vitaminen eingesetzt.Advantageously, the carotenoids are usually in kri stalliner form together with the water-soluble vitamins in the Ground oil. In the case of astaxanthin and canthaxanthin be preferably astaxanthin or canthaxanthin-containing dry powders, For example, Lucantin® Pink or Lucantin® Red (a 10% Astaxanthin or Canthaxanthin dry powder, BASF AG, Ludwigshafen, Germany) together with the water-soluble Used vitamins.
Der Gehalt an Carotinoide liegt in den Formulierungen im allge meinen zwischen 0,1 und 40 Gew.-%, bevorzugt zwischen 0,3 und 20 Gew.-%, besonders bevorzugt zwischen 0,5 und 10 Gew.-%, ganz besonders bevorzugt zwischen 1 und 5 Gew.-%, bezogen auf die Gesamtmenge der Formulierung.The content of carotenoids is in the formulations in general between 0.1 and 40% by weight, preferably between 0.3 and 20 wt .-%, particularly preferably between 0.5 and 10 wt .-%, completely particularly preferably between 1 and 5 wt .-%, based on the Total amount of formulation.
Je nach Anwendungszweck können die erfindungsgemäßen öligen Zube reitungen bis zu 10 Gew.-% weiterer Zusatzkomponenten wie bei spielsweise Mineralstoffe, Aminosäuren, Proteine oder Enzyme ent halten.Depending on the application, the oily Zube invention Preparations up to 10 wt .-% of other additional components as in For example, minerals, amino acids, proteins or enzymes ent hold.
Diese Zusatzstoffe, ebenso wie die o. g. fettlöslichen Vitamine und Carotinoide, können vor, während oder nach der Mahlung der erfindungsgemäßen Suspension zugesetzt werden. Um eine möglichst feinteilige homogene Suspension aller nicht-öllöslicher Bestand teile zu erhalten, ist es von Vorteil, die o. g. Zusatzstoffe ebenfalls zusammen mit den wasserlöslichen Vitaminen zu mahlen.These additives, as well as the o. G. fat-soluble vitamins and carotenoids, before, during or after the grinding of the suspension according to the invention are added. To one as possible finely divided homogeneous suspension of all non-oil-soluble stock It is an advantage to obtain the o. g. additives also to grind together with the water-soluble vitamins.
Als Mineralstoffe können beispielsweise Eisensulfat, Zinksulfat, Mangansulfat, Kupfersulfat, Calciumsulfat, Natriumsulfat, Kupfer oxid, Magnesiumoxid, Calciumfluorid, Kaliumchlorid, Kaliumjodid, Natriumchlorid, Calciumjodat, Calcium-, Magnesium-, Kalium-, Na trium- oder Eisen-Phosphat, Cobaltcarbonat, Natriumselenat oder Kieselsäure und deren Salze in die Suspension eingearbeitet und mitvermahlen werden. Die Menge an eingesetzten Mineralstoffen, beispielsweise im Tierernährungsbereich, orientiert sich dabei jeweils am Bedarf der zu fütternden Tiere.As minerals, for example, iron sulfate, zinc sulfate, Manganese sulfate, copper sulfate, calcium sulfate, sodium sulfate, copper oxide, magnesium oxide, calcium fluoride, potassium chloride, potassium iodide, Sodium chloride, calcium iodate, calcium, magnesium, potassium, Na trium or iron phosphate, cobalt carbonate, sodium selenate or Silica and its salts incorporated in the suspension and be ground with. The amount of minerals used, For example, in the animal nutrition sector, thereby oriented in each case on the need of the animals to be fed.
Als Aminosäurereste kommen generell alle bekannten physiologisch unbedenklichen α-Aminosäurereste in Frage. Bevorzugt zu nennen sind die Reste folgender Aminosäuren: Alanin, Arginin, Asparagin, Asparaginsäure, Cystein, Cystin, Glutamin, Glutaminsäure, Glycin, Histidin, Isoleucin, Leucin, Lysin, Methionin, Phenylalanin, Hip pursäure, Serin und Taurin. Besonders bevorzugt sind Lysin, Me thionin und Cystein.As amino acid residues generally all known physiological harmless α-amino acid residues in question. Preferred to call are the residues of the following amino acids: alanine, arginine, asparagine, Aspartic acid, cysteine, cystine, glutamine, glutamic acid, glycine, Histidine, isoleucine, leucine, lysine, methionine, phenylalanine, hip acid, serine and taurine. Particularly preferred are lysine, Me thionine and cysteine.
Als Enzyme kommen in diesem Zusammenhang bevorzugt Phosphatasen Glucanasen und gegebenenfalls Esterasen bzw. Lipasen, letztere in verkapselter Form, in Frage.Preferred enzymes in this context are phosphatases Glucanases and optionally esterases or lipases, the latter in encapsulated form, in question.
Weitere Bestandteile der Suspension können sein:Other components of the suspension may be:
Verbindungen mit Vitamin- oder Coenzymcharakter, z. B. Cholin chlorid, Carnitin, γ-Butyrobetain, Liponsäure, Kreatin, Ubichi none, S-Methylmethionin, S-Adenosylmethionin.Compounds with vitamin or coenzyme character, z. Choline chloride, carnitine, γ-butyrobetaine, lipoic acid, creatine, Ubichi none, S-methylmethionine, S-adenosylmethionine.
Mehrfach ungesättigte Fettsäuren, z. B. Linolsäure, Linolensäure, Arachidonsäure, Eicosapentaensäure, Docosahexaensäure.Polyunsaturated fatty acids, e.g. Linoleic acid, linolenic acid, Arachidonic acid, eicosapentaenoic acid, docosahexaenoic acid.
Fütterungsantibiotika für Medizinalfutter sowie Mikroorganismen zur Verbesserung der Verdauung.Feeding antibiotics for medicated feed and microorganisms to improve digestion.
In manchen Fällen kann es erforderlich sein, daß die öligen Suspensionen außerdem Hilfsstoffe, wie z. B. Schutzkolloide, Antioxidantien, Verdicker, Chelatbildner, wie z. B. Alkali- oder Erdalkalisalze der Citronensäure, Phytinsäure oder Phosphorsäure enthalten und/oder Emulgatoren enthalten.In some cases, it may be necessary that the oily Suspensions also excipients, such as. B. protective colloids, Antioxidants, thickeners, chelating agents, such as. B. alkali or Alkaline earth salts of citric acid, phytic acid or phosphoric acid contain and / or contain emulsifiers.
Als Schutzkolloide können beispielsweise Gelatine, Fischgelatine, Stärke, Dextrin, Pflanzenproteine, Pektin, Gummi-Arabikum, Kasein, Kaseinat oder Mischungen davon verwendet. Es können aber auch Polyvinylalkohol, Polyvinylpyrrolidon, Methylcellulose, Carboxymethylcellulose, Hydroxypropylcellulose und Alginate ein gesetzt werden. Bezüglich näherer Einzelheiten wird auf R. A. Morton, Fat Soluble Vitamins, Intern. Encyclopedia of Food and Nutrition, Bd. 9, Pergamon Press 1970, S. 128-131, verwiesen.As protective colloids, for example, gelatin, fish gelatin, Starch, dextrin, vegetable proteins, pectin, gum arabic, Casein, caseinate or mixtures thereof. But it can also polyvinyl alcohol, polyvinyl pyrrolidone, methyl cellulose, Carboxymethylcellulose, hydroxypropylcellulose and alginates be set. For more details will be on R.A. Morton, Fat Soluble Vitamins, Intern. Encyclopedia of Food and Nutrition, Vol. 9, Pergamon Press 1970, pp. 128-131.
Zur Erhöhung der Stabilität des Wirkstoffes gegen oxidativen Abbau ist es vorteilhaft, Stabilisatoren wie α-Tocopherol, t-Butyl-hydroxy-toluol, t-Butylhydroxyanisol, Ascorbinsäure oder Ethoxyguin zuzusetzen.To increase the stability of the active ingredient against oxidative Degradation, it is advantageous to use stabilizers such as α-tocopherol, t-butyl-hydroxy-toluene, t-butylhydroxyanisole, ascorbic acid or To add ethoxyguin.
Als Emulgatoren bzw. Solubilisatoren können beispielsweise Ascorbylpalmitat, Polyglycerin-Fettsäureester, Sorbitan-Fett säureester, Propylenglycol-Fettsäureester oder Lecithin verwendet werden.As emulsifiers or solubilizers, for example Ascorbyl palmitate, polyglycerol fatty acid ester, sorbitan fat acid ester, propylene glycol fatty acid ester or lecithin used become.
Die erfindungsgemäßen öligen Suspensionen haben u. a. den Vorteil, daß die Vitamine durch das Öl gegen Sauerstoff und Feuchtigkeit geschützt sind. Die wasserlöslichen Vitamine und die Mineralien sind nahezu ölunlöslich und können dadurch auch keine Reaktionen untereinander eingehen (Kompatibilität). Zudem sind mikrobiologi sche Probleme in öligen, wasserfreien Systemen nicht zu erwarten.The oily suspensions according to the invention have u. a. the advantage, that the vitamins are protected by the oil against oxygen and moisture are protected. The water-soluble vitamins and minerals are almost insoluble in oil and therefore can not react enter into each other (compatibility). In addition, microbiological not expected problems in oily, anhydrous systems.
Die Suspensionen eignen sich u. a. als Zusatzstoff für Lebens mittel- und Tierfuttermittelzubereitungen bzw. Mischfutter, als Mittel für die Herstellung pharmazeutischer und kosmetischer Zubereitungen sowie für die Herstellung von Nahrungsergänzungs präparaten im Human- und Tierbereich.The suspensions are u. a. as an additive for life medium and animal feed preparations or compound feed, as Means for the preparation of pharmaceutical and cosmetic Preparations and for the preparation of dietary supplements preparations in the human and animal sector.
Bevorzugt lassen sich die Suspensionen als Futtermittelzusatz in der Tierernährung einsetzen, insbesondere zum Auftragen bzw. Auf sprühen auf Futtermittelpellets.Preferably, the suspensions can be used as a feed additive use the animal nutrition, especially for application or on spray on feed pellets.
Die Anwendung als Futtermittelzusatzstoff erfolgt insbesondere durch direktes Aufsprühen der erfindungsgemäßen Suspensionen, gegebenenfalls nach Verdünnung mit Ölen, beispielsweise auf Tier futterpellets als sogenannte "post-pelleting-application".The application as a feed additive takes place in particular by direct spraying of the suspensions according to the invention, optionally after dilution with oils, for example on animal feed pellets as a so-called "post-pelleting-application".
Eine bevorzugte Ausführungsform des Sprühverfahrens besteht darin, daß man die Futtermittelpellets unter vermindertem Druck mit der öligen Suspension belädt.A preferred embodiment of the spraying method is in that the feed pellets under reduced pressure loaded with the oily suspension.
Beispiele hierfür finden sich u. a. in GB-A-2 232 573 sowie in EP-A-0 556 883. Examples of this can be found u. a. in GB-A-2 232 573 and in EP-A-0 556 883.
Typische Einsatzgebiete im Lebensmittelbereich sind beispiels weise die Vitaminierung von Getränken, Milchprodukten wie Joghurt, Milchmixgetränken oder Milchspeiseeis sowie von Pudding pulvern, Eiprodukten, Backmischungen und Süßwaren.Typical applications in the food industry are, for example wise the vitaminization of drinks, dairy products like Yoghurt, milk-based drinks or milk ice cream and pudding powders, egg products, baking mixes and sweets.
Im Kosmetikbereich können die öligen Suspensionen beispielsweise für Vitamin-haltige Körperpflegemittel beispielsweise in Form einer Creme, einer Lotion, als Lippenstifte oder Make-up ver wendet werden.In the cosmetics industry, for example, the oily suspensions for vitamin-containing personal care products, for example in the form a cream, a lotion, as lipsticks or make-up ver be used.
Gegenstand der Erfindung sind ferner Nahrungsergänzungsmittel, Tierfuttermittel, Lebensmittel sowie pharmazeutische und kosmeti sche Zubereitungen, enthaltend die eingangs beschriebenen öligen Suspensionen wasserlöslicher Vitamine.The invention furthermore relates to dietary supplements, Animal feed, food and pharmaceutical and cosmetic cal preparations containing the oily described above Suspensions of water-soluble vitamins.
Bevorzugt richtet sich die Erfindung auf Tierfuttermittel, insbesondere auf Futtermittelpellets, die mit den Suspensionen beladen werden.Preferably, the invention is directed to animal feed, especially on feed pellets containing the suspensions be loaded.
Unter Nahrungsergänzungspräparate sowie pharmazeutische Zuberei tungen, die die erfindungsgemäße Suspension enthalten, sind u. a. Tabletten, Dragees sowie bevorzugt Hart- und Weichgelatinekapseln zu verstehen.Among dietary supplements and pharmaceutical preparations tions containing the suspension according to the invention are u. a. Tablets, dragées and preferably hard and soft gelatine capsules to understand.
Kosmetische Zubereitungen, die die erfindungsgemäßen Suspensionen enthalten können, sind beispielsweise topisch anwendbare Zuberei tungen, insbesondere dekorative Körperpflegemittel wie Lippen stifte, Gesichts-Make-up in Form einer Creme sowie Lotionen.Cosmetic preparations containing the suspensions according to the invention may include, for example, topically applicable Zuberei tions, in particular decorative body care products such as lips pens, face make-up in the form of a cream and lotions.
In den folgenden Beispielen wird die Herstellung der erfindungs gemäßen öligen Suspensionen wasserlöslicher Vitamine näher erläu tert.In the following examples, the preparation of the invention appropriate oily suspensions of water-soluble vitamins closer erläu tert.
Zwei Kilogramm einer Mischung aus 25 Gew.-% Vitamin C (99%ig, BASF AG) und 75 Gew.-% eines mittelkettigen Triglycerids (Delios® SK der Fa. Grünau, Deutschland) wurden mit einem Blatt rührer solange gerührt, bis eine homogene Suspension vorlag. Danach wurde die Mischung in eine rührbare Vorlage umgefüllt, aus der die Suspension mittels Schlauchpumpe durch eine kontinuier lich betriebene Kugelmühle (Dyno Mill KDL Spezial) gefördert wurde. Der Mahlbehälter der Kugelmühle war mit 400 g Glaskugeln (Durchmesser 800-1200 µm) gefüllt. Die aus der Mühle austretende feinteilige Suspension wurde aufgefangen und mittels eines Parti kelgrößenmeßgerätes (Malvern Mastersizer) vermessen. Der Mahlvor gang wurde so oft wiederholt bis 90% der suspendierten Teilchen eine Teilchengröße kleiner 10 gin [D(0.9) < 10 µm] hatten. Dies entsprach einer mittleren Partikelgröße D[4,3] von 5,2 µm.Two kilograms of a mixture of 25% by weight of vitamin C (99% pure, BASF AG) and 75% by weight of a medium-chain triglyceride (Delios® SK Fa. Grünau, Germany) were with a leaf Stirred until a homogeneous suspension was present. Thereafter, the mixture was transferred to a stirrable template, from the suspension by means of peristaltic pump through a continuous supported ball mill (Dyno Mill KDL Spezial) has been. The grinding container of the ball mill was with 400 g of glass beads (Diameter 800-1200 microns) filled. The exiting from the mill finely divided suspension was collected and by means of a Parti size measuring device (Malvern Mastersizer). The Mahlvor The procedure was repeated until 90% of the suspended particles had a particle size smaller than 10 g in [D (0.9) <10 μm]. This corresponded to an average particle size D [4,3] of 5.2 μm.
Nach der Abtrennung von den Mahlkörpern wurde ein Teil der Dis persion mit der 10 fachen Menge des verwendeten Öls verdünnt und über 12 h stehengelassen. Weder die unverdünnte noch die ver dünnte Dispersion zeigten über diesen Zeitraum Sedimentationser scheinungen.After separation from the media, a portion of the dis diluted with 10 times the amount of oil used and left over 12 h. Neither the undiluted nor the ver thin dispersion showed over this period sedimentation phenomena.
Eine Mischung aus
A mix of
wurde mit einem Blattrührer solange gerührt, bis eine homogene Suspension vorlag. Die Mischung wurde daraufhin in eine rührbare Vorlage umgefüllt, aus der die Suspension mittels Schlauchpumpe durch die in Beispiel 1 genannte, kontinuierlich betriebene Ku gelmühle gefördert wurde. Der Mahlvorgang wurde so oft wiederholt, bis 90% der suspendierten Teilchen eine Teilchengröße kleiner 20 µm [D(0.9) < 20 µm] hatten. Dies entsprach einer mittleren Partikelgröße D[4,3] von 10,9 µm.was stirred with a paddle stirrer until a homogeneous Suspension was present. The mixture was then into a stirrable Template refilled, from which the suspension by means of peristaltic pump by the continuously operated Ku mentioned in Example 1 gelmühle was promoted. The milling process was repeated so many times, Up to 90% of the suspended particles have a particle size smaller 20 μm [D (0.9) <20 μm]. This corresponded to a middle one Particle size D [4,3] of 10.9 μm.
Nach der Abtrennung von den Mahlkörpern wurde ein Teil der Dis persion mit der 10fachen Menge Maiskeimöl verdünnt und über 12 h stehengelassen. Weder die unverdünnte noch die verdünnte Disper sion zeigten über diesen Zeitraum Sedimentationserscheinungen. After separation from the media, a portion of the dis diluted with 10 times the amount of corn oil and over 12 h ditched. Neither the undiluted nor the diluted Disper sion showed sedimentation phenomena over this period.
Eine Mischung aus
A mix of
wurde analog Beispiel 2 suspendiert und durch eine kontinuierlich betriebene Kugelmühle gemahlen. Der Mahlvorgang wurde so lange durchgeführt, bis 90% der suspendierten Teilchen eine Teilchen größe kleiner 30 µm [D(0.9) < 30 µm] hatten. Dies entsprach einer mittleren Partikelgröße D[4,3] von 15,3 µm.was suspended as in Example 2 and by a continuous ground ball mill. The grinding process was so long carried out until 90% of the suspended particles a particle size smaller than 30 μm [D (0.9) <30 μm]. This corresponded to one average particle size D [4,3] of 15.3 μm.
Nach der Abtrennung von den Mahlkörpern wurde ein Teil der Dis persion mit der 10fachen Menge Maiskeimöl verdünnt und über 12 h stehengelassen. Weder die unverdünnte noch die verdünnte Disper sion zeigten über diesen Zeitraum Sedimentationserscheinungen.After separation from the media, a portion of the dis diluted with 10 times the amount of corn oil and over 12 h ditched. Neither the undiluted nor the diluted Disper sion showed sedimentation phenomena over this period.
Analog Beispiel 2 wurde eine Mischung aus
Analogously to Example 2 was a mixture of
suspendiert und durch eine kontinuierlich betriebene Kugelmühle gemahlen. Der Mahlvorgang wurde so lange durchgeführt, bis 90% der suspendierten Teilchen eine Teilchengröße kleiner 20 µm [D(0.9) < 20 µm] hatten. Dies entsprach einer mittleren Partikel größe D[4,3] von 10,9 µm.suspended and by a continuously operated ball mill ground. The milling process was carried out until 90% the suspended particles have a particle size of less than 20 microns [D (0.9) <20 μm]. This corresponded to a medium particle size D [4.3] of 10.9 μm.
Nach der Abtrennung von den Mahlkörpern wurde ein Teil der Dis persion mit der 10 fachen Menge Maiskeimöl verdünnt und über 12 h stehengelassen. Weder die unverdünnte noch die verdünnte Disper sion zeigten über diesen Zeitraum Sedimentationserscheinungen.After separation from the media, a portion of the dis diluted with 10 times the amount of corn oil and over 12 h ditched. Neither the undiluted nor the diluted Disper sion showed sedimentation phenomena over this period.
Analog Beispiel 2 wurde eine Mischung aus
Analogously to Example 2 was a mixture of
suspendiert und durch eine kontinuierlich betriebene Kugelmühle gemahlen. Der Mahlvorgang wurde so lange durchgeführt, bis 90% der suspendierten Teilchen eine Teilchengröße kleiner 20 µm [D(0.9) < 20 µm] hatten. Dies entsprach einer mittleren Partikel größe D[4,3] von 10,9 µm.suspended and by a continuously operated ball mill ground. The milling process was carried out until 90% the suspended particles have a particle size of less than 20 microns [D (0.9) <20 μm]. This corresponded to a medium particle size D [4.3] of 10.9 μm.
Nach der Abtrennung von den Mahlkörpern wurde ein Teil der Dispersion mit der 10fachen Menge Sonnenblumenöl verdünnt und über 12 h stehengelassen. Weder die unverdünnte noch die ver dünnte Dispersion zeigten über diesen Zeitraum Sedimentations erscheinungen. After separation from the grinding media was part of the Diluted with 10 times the amount of sunflower oil and left over 12 h. Neither the undiluted nor the ver thin dispersion showed sedimentation over this period phenomena.
Analog Beispiel 2 wurde eine Mischung aus
Analogously to Example 2 was a mixture of
suspendiert und durch eine kontinuierlich betriebene Kugelmühle gemahlen. Der Mahlvorgang wurde so lange durchgeführt, bis 90% der suspendierten Teilchen eine Teilchengröße kleiner 20 µm [D(0.9) < 20 µm] hatten. Dies entsprach einer mittleren Partikel größe D[4,3] von 10,9 µm.suspended and by a continuously operated ball mill ground. The milling process was carried out until 90% the suspended particles have a particle size of less than 20 microns [D (0.9) <20 μm]. This corresponded to a medium particle size D [4.3] of 10.9 μm.
Nach der Abtrennung von den Mahlkörpern wurde ein Teil der Dis persion mit der 10fachen Menge Fischöl verdünnt und über 12 h stehengelassen. Weder die unverdünnte noch die verdünnte Disper sion zeigten über diesen Zeitraum Sedimentationserscheinungen.After separation from the media, a portion of the dis diluted with 10 times the amount of fish oil and over 12 h ditched. Neither the undiluted nor the diluted Disper sion showed sedimentation phenomena over this period.
Analog Beispiel 2 wurde eine Mischung aus
Analogously to Example 2 was a mixture of
suspendiert und durch eine kontinuierlich betriebene Kugelmühle gemahlen. Der Mahlvorgang wurde so lange durchgeführt, bis 90% der suspendierten Teilchen eine Teilchengröße kleiner 20 µm [D(0.9) < 20 µm] hatten. Dies entsprach einer mittleren Partikel größe D[4,3] von 10,9 µm.suspended and by a continuously operated ball mill ground. The milling process was carried out until 90% the suspended particles have a particle size of less than 20 microns [D (0.9) <20 μm]. This corresponded to a medium particle size D [4.3] of 10.9 μm.
Nach der Abtrennung von den Mahlkörpern wurde ein Teil der Dis persion mit der 10fachen Menge Maiskaimöl verdünnt und über 12 h stehengelassen. Weder die unverdünnte noch die verdünnte Disper sion zeigten über diesen Zeitraum Sedimentationserscheinungen.After separation from the media, a portion of the dis diluted with 10 times the amount of corn shark oil and over 12 h ditched. Neither the undiluted nor the diluted Disper sion showed sedimentation phenomena over this period.
Analog Beispiel 2 wurde eine Mischung aus
Analogously to Example 2 was a mixture of
suspendiert und durch eine kontinuierlich betriebene Kugelmühle gemahlen. Der Mahlvorgang wurde so lange durchgeführt, bis 90% der suspendierten Teilchen eine Teilchengröße kleiner 20 µm [D(0.9) < 20 µm] hatten.suspended and by a continuously operated ball mill ground. The milling process was carried out until 90% the suspended particles have a particle size of less than 20 microns [D (0.9) <20 μm].
Nach der Abtrennung von den Mahlkörpern wurde ein Teil der Dis persion mit der 10fachen Menge Fischöl verdünnt und über 12 h stehengelassen. Weder die unverdünnte noch die verdünnte Disper sion zeigten über diesen Zeitraum Sedimentationserscheinungen.After separation from the media, a portion of the dis diluted with 10 times the amount of fish oil and over 12 h ditched. Neither the undiluted nor the diluted Disper sion showed sedimentation phenomena over this period.
Analog Beispiel 2 wurde eine Mischung aus
Analogously to Example 2 was a mixture of
suspendiert und durch eine kontinuierlich betriebene Kugelmühle gemahlen. Der Mahlvorgang wurde so lange durchgeführt, bis 90% der suspendierten Teilchen eine Teilchengröße kleiner 20 µm [D(0.9) < 20 µm] hatten.suspended and by a continuously operated ball mill ground. The milling process was carried out until 90% the suspended particles have a particle size of less than 20 microns [D (0.9) <20 μm].
Nach der Abtrennung von den Mahlkörpern wurde ein Teil der Dis persion mit der 10fachen Menge Maiskeimöl verdünnt und über 12 h stehengelassen. Weder die unverdünnte noch die verdünnte Disper sion zeigten über diesen Zeitraum Sedimentationserscheinungen.After separation from the media, a portion of the dis diluted with 10 times the amount of corn oil and over 12 h ditched. Neither the undiluted nor the diluted Disper sion showed sedimentation phenomena over this period.
Claims (15)
Priority Applications (11)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE10013312A DE10013312A1 (en) | 2000-03-17 | 2000-03-17 | Production of oily suspensions of water soluble vitamins comprises milling of vitamins in oil or dry milling and suspension in oil |
DK01927730T DK1272059T3 (en) | 2000-03-17 | 2001-03-15 | Process for the preparation of oily suspensions of water-soluble vitamins |
ES01927730T ES2252217T3 (en) | 2000-03-17 | 2001-03-15 | PROCEDURE FOR OBTAINING OLEAGINOUS SUSPENSIONS OF HYDROSOLUBABLE VITAMINS. |
US10/221,203 US20030185877A1 (en) | 2000-03-17 | 2001-03-15 | Method of producing oily suspensions of water-soluble vitamins |
JP2001566374A JP2004500392A (en) | 2000-03-17 | 2001-03-15 | Method for producing oil-based suspension of water-soluble vitamin |
CNB01806695XA CN1197483C (en) | 2000-03-17 | 2001-03-15 | Method of producing oily suspensions of water-soluble vitamins |
EP01927730A EP1272059B1 (en) | 2000-03-17 | 2001-03-15 | Method of producing oily suspensions of water-soluble vitamins |
AT01927730T ATE311766T1 (en) | 2000-03-17 | 2001-03-15 | METHOD FOR PRODUCING OIL SUSPENSIONS OF WATER-SOLUBLE VITAMINS |
DE50108311T DE50108311D1 (en) | 2000-03-17 | 2001-03-15 | PROCESS FOR PREPARING OILY SUSPENSIONS OF WATER SOLUBLE VITAMINS |
AU2001254687A AU2001254687A1 (en) | 2000-03-17 | 2001-03-15 | Method of producing oily suspensions of water-soluble vitamins |
PCT/EP2001/002939 WO2001067896A2 (en) | 2000-03-17 | 2001-03-15 | Method of producing oily suspensions of water-soluble vitamins |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE10013312A DE10013312A1 (en) | 2000-03-17 | 2000-03-17 | Production of oily suspensions of water soluble vitamins comprises milling of vitamins in oil or dry milling and suspension in oil |
Publications (1)
Publication Number | Publication Date |
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DE10013312A1 true DE10013312A1 (en) | 2001-09-20 |
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Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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DE10013312A Withdrawn DE10013312A1 (en) | 2000-03-17 | 2000-03-17 | Production of oily suspensions of water soluble vitamins comprises milling of vitamins in oil or dry milling and suspension in oil |
Country Status (1)
Country | Link |
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DE (1) | DE10013312A1 (en) |
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2000
- 2000-03-17 DE DE10013312A patent/DE10013312A1/en not_active Withdrawn
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