DE10049137A1 - 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
- DE10049137A1 DE10049137A1 DE10049137A DE10049137A DE10049137A1 DE 10049137 A1 DE10049137 A1 DE 10049137A1 DE 10049137 A DE10049137 A DE 10049137A DE 10049137 A DE10049137 A DE 10049137A DE 10049137 A1 DE10049137 A1 DE 10049137A1
- Authority
- DE
- Germany
- Prior art keywords
- oil
- grinding
- water
- oily suspensions
- vitamin
- 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- Withdrawn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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- 235000013365 dairy product Nutrition 0.000 description 1
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- 235000019425 dextrin Nutrition 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
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- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical compound [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 description 1
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- 238000009826 distribution Methods 0.000 description 1
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- 229940093500 ethoxyquin Drugs 0.000 description 1
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- 230000001815 facial effect Effects 0.000 description 1
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- 150000002224 folic acids Chemical class 0.000 description 1
- VVIAGPKUTFNRDU-ABLWVSNPSA-N folinic acid Chemical compound C1NC=2NC(N)=NC(=O)C=2N(C=O)C1CNC1=CC=C(C(=O)N[C@@H](CCC(O)=O)C(O)=O)C=C1 VVIAGPKUTFNRDU-ABLWVSNPSA-N 0.000 description 1
- 235000010382 gamma-tocopherol Nutrition 0.000 description 1
- FOYKKGHVWRFIBD-UHFFFAOYSA-N gamma-tocopherol acetate Natural products CC(=O)OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1 FOYKKGHVWRFIBD-UHFFFAOYSA-N 0.000 description 1
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- 239000008187 granular material Substances 0.000 description 1
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- 238000006460 hydrolysis reaction Methods 0.000 description 1
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- 239000001863 hydroxypropyl cellulose Substances 0.000 description 1
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 description 1
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- 229910052742 iron Inorganic materials 0.000 description 1
- 229910000398 iron phosphate Inorganic materials 0.000 description 1
- 229910000358 iron sulfate Inorganic materials 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 description 1
- 229960000310 isoleucine Drugs 0.000 description 1
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- 229940067606 lecithin Drugs 0.000 description 1
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- ZNOVTXRBGFNYRX-ABLWVSNPSA-N levomefolic acid Chemical compound C1NC=2NC(N)=NC(=O)C=2N(C)C1CNC1=CC=C(C(=O)N[C@@H](CCC(O)=O)C(O)=O)C=C1 ZNOVTXRBGFNYRX-ABLWVSNPSA-N 0.000 description 1
- 229960004488 linolenic acid Drugs 0.000 description 1
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- 235000019136 lipoic acid Nutrition 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 235000020640 mackerel Nutrition 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 229910000157 magnesium phosphate Inorganic materials 0.000 description 1
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 1
- 235000019341 magnesium sulphate Nutrition 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 229940099596 manganese sulfate Drugs 0.000 description 1
- 239000011702 manganese sulphate Substances 0.000 description 1
- 235000007079 manganese sulphate Nutrition 0.000 description 1
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229960005173 methiosulfonium chloride Drugs 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 235000010981 methylcellulose Nutrition 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000011785 micronutrient Substances 0.000 description 1
- 235000013369 micronutrients Nutrition 0.000 description 1
- 235000005152 nicotinamide Nutrition 0.000 description 1
- 239000011570 nicotinamide Substances 0.000 description 1
- 229960003512 nicotinic acid Drugs 0.000 description 1
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- 230000035764 nutrition Effects 0.000 description 1
- 239000010461 other edible oil Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000010525 oxidative degradation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002540 palm oil Substances 0.000 description 1
- 229940101267 panthenol Drugs 0.000 description 1
- 235000020957 pantothenol Nutrition 0.000 description 1
- 239000011619 pantothenol Substances 0.000 description 1
- 239000001814 pectin Substances 0.000 description 1
- 235000010987 pectin Nutrition 0.000 description 1
- 229920001277 pectin Polymers 0.000 description 1
- 239000000825 pharmaceutical preparation Substances 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 229960005190 phenylalanine Drugs 0.000 description 1
- COLNVLDHVKWLRT-UHFFFAOYSA-N phenylalanine Natural products OC(=O)C(N)CC1=CC=CC=C1 COLNVLDHVKWLRT-UHFFFAOYSA-N 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 239000000467 phytic acid Chemical class 0.000 description 1
- 235000002949 phytic acid Nutrition 0.000 description 1
- 229940068041 phytic acid Drugs 0.000 description 1
- 235000021118 plant-derived protein Nutrition 0.000 description 1
- 229920000223 polyglycerol Polymers 0.000 description 1
- 239000001205 polyphosphate Substances 0.000 description 1
- 235000020777 polyunsaturated fatty acids Nutrition 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
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- 229910000160 potassium phosphate Inorganic materials 0.000 description 1
- 235000010409 propane-1,2-diol alginate Nutrition 0.000 description 1
- 235000018102 proteins Nutrition 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 235000011962 puddings Nutrition 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 229960000342 retinol acetate Drugs 0.000 description 1
- 235000019173 retinyl acetate Nutrition 0.000 description 1
- 239000011770 retinyl acetate Substances 0.000 description 1
- QGNJRVVDBSJHIZ-QHLGVNSISA-N retinyl acetate Chemical compound CC(=O)OC\C=C(/C)\C=C\C=C(/C)\C=C\C1=C(C)CCCC1(C)C QGNJRVVDBSJHIZ-QHLGVNSISA-N 0.000 description 1
- 235000019172 retinyl palmitate Nutrition 0.000 description 1
- 229940108325 retinyl palmitate Drugs 0.000 description 1
- 239000011769 retinyl palmitate Substances 0.000 description 1
- 235000019192 riboflavin Nutrition 0.000 description 1
- 239000002151 riboflavin Substances 0.000 description 1
- 229960002477 riboflavin Drugs 0.000 description 1
- 229940119224 salmon oil Drugs 0.000 description 1
- 239000008159 sesame oil Substances 0.000 description 1
- 235000011803 sesame oil Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- PPASLZSBLFJQEF-RKJRWTFHSA-M sodium ascorbate Substances [Na+].OC[C@@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RKJRWTFHSA-M 0.000 description 1
- 235000010378 sodium ascorbate Nutrition 0.000 description 1
- 229960005055 sodium ascorbate Drugs 0.000 description 1
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 description 1
- 229910000162 sodium phosphate Inorganic materials 0.000 description 1
- 239000011655 sodium selenate Substances 0.000 description 1
- 235000018716 sodium selenate Nutrition 0.000 description 1
- 229960001881 sodium selenate Drugs 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- PPASLZSBLFJQEF-RXSVEWSESA-M sodium-L-ascorbate Chemical compound [Na+].OC[C@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RXSVEWSESA-M 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000003549 soybean oil Substances 0.000 description 1
- 235000012424 soybean oil Nutrition 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 229960003080 taurine Drugs 0.000 description 1
- 235000019157 thiamine Nutrition 0.000 description 1
- 229960003495 thiamine Drugs 0.000 description 1
- 239000011721 thiamine Substances 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 229960002663 thioctic acid Drugs 0.000 description 1
- 229930003802 tocotrienol Natural products 0.000 description 1
- 239000011731 tocotrienol Substances 0.000 description 1
- 235000019148 tocotrienols Nutrition 0.000 description 1
- 150000003669 ubiquinones Chemical class 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 235000019155 vitamin A Nutrition 0.000 description 1
- 239000011719 vitamin A Substances 0.000 description 1
- 235000019154 vitamin C Nutrition 0.000 description 1
- 239000011718 vitamin C 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
- QYSXJUFSXHHAJI-YRZJJWOYSA-N vitamin D3 Chemical compound C1(/[C@@H]2CC[C@@H]([C@]2(CCC1)C)[C@H](C)CCCC(C)C)=C\C=C1\C[C@@H](O)CCC1=C QYSXJUFSXHHAJI-YRZJJWOYSA-N 0.000 description 1
- 235000012711 vitamin K3 Nutrition 0.000 description 1
- 239000011652 vitamin K3 Substances 0.000 description 1
- 229940045997 vitamin a Drugs 0.000 description 1
- 229940041603 vitamin k 3 Drugs 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- 235000013618 yogurt Nutrition 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
- 235000007680 β-tocopherol Nutrition 0.000 description 1
- 239000011590 β-tocopherol Substances 0.000 description 1
- 239000002478 γ-tocopherol Substances 0.000 description 1
- 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
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/33—Heterocyclic compounds
- A61K31/395—Heterocyclic compounds having nitrogen as a ring hetero atom, e.g. guanethidine or rifamycins
- 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
- A61K31/525—Isoalloxazines, e.g. riboflavins, vitamin B2
-
- 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
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- 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
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- 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
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/59—Compounds containing 9, 10- seco- cyclopenta[a]hydrophenanthrene ring systems
- A61K31/593—9,10-Secocholestane derivatives, e.g. cholecalciferol, i.e. vitamin D3
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/70—Carbohydrates; Sugars; Derivatives thereof
- A61K31/7135—Compounds containing heavy metals
- A61K31/714—Cobalamins, e.g. cyanocobalamin, i.e. vitamin B12
-
- 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
- A61K9/10—Dispersions; Emulsions
-
- 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
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Public Health (AREA)
- Epidemiology (AREA)
- Pharmacology & Pharmacy (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Veterinary Medicine (AREA)
- Mycology (AREA)
- Nutrition Science (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Dispersion Chemistry (AREA)
- Molecular Biology (AREA)
- Medicinal Preparation (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
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 Zubereitungen.The invention relates to oily suspensions of at least one water-soluble vitamins and a process for their preparation these suspensions and their use as an additive to life animal feed, pharmaceuticals and cosmetics Preparations.
Die Verwendung von Vitaminen als Futtermittelzusatzstoffe in der Tierernährung erfolgt mehr und mehr in Form flüssiger Zubereitungen. Dies hat u. a. den Vorteil, daß die Dosierung einfacher und genauer erfolgen kann. Ferner ist es möglich, bei der sogenannten "post-pellet-application" beispielsweise Futter mittelpellets erst nach deren Herstellung mit einer flüssigen Zubereitung von Futtermittelzusatzstoffen zu beladen. Dies hat zur Folge, daß selbst oxidations- und temperaturempfindliche Zusatzstoffe wie Vitamine oder Carotinoide ohne größere Verluste eingesetzt werden können.The use of vitamins as feed additives in animal nutrition takes place more and more in the form of liquid Preparations. This has u. a. the advantage that the dosage can be done more easily and precisely. It is also possible to the so-called "post-pellet application" for example feed medium pellets only after their production with a liquid Preparation of feed additives. this has the consequence that even oxidation and temperature sensitive Additives like vitamins or carotenoids without major losses can be used.
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) can be found 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 flüssiger Formulierungen von wasserlöslichen Vitaminen in Kombination mit Mineralien und fettlöslichen Vitaminen. Hier kann es durch gegenseitige Wechselwirkungen zu unerwünschten Wirkstoffverlusten kommen.Administration has so far been a critical application liquid formulations of water soluble vitamins in Combination with minerals and fat-soluble vitamins. Here can become undesirable through mutual interactions 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, where the vitamins and minerals are kept separately and only be mixed shortly before application. A disadvantage of this The procedure is to match the required deployment the storage container, combined with complex logistics.
Vitamin-Emulsionen - als spezielle Form einer flüssigen Formu lierung - 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 Konta mination auftreten kann. Vitamin emulsions - as a special form of a liquid formulation lation - often have the disadvantage that they are physical (Occurrence of phase separation) and chemical (occurrence of unwanted hydrolysis and / or redox reactions, chemical Incompatibility of individual dissolved components) are unstable and in addition often the risk of microbiological contact mination can occur.
Ferner sind Systeme bekannt, bei denen u. a. wasserlösliche Vitamine in Ölen oder Fetten dispergiert vorliegen.Systems are also known in which u. a. water-soluble Vitamins are 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 verfahrensstechnisch aufwendig ist und bei der Verwendung von Vitaminen häufig mit der Gefahr uner wünschter Wirkstoffverluste verbunden ist.This is how 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 melted hard fats are under Stirring finely divided assimilable iron-containing substances give. The homogeneous dispersion then becomes hard fat Spray cooled pellets. Micronutrients can also be used as an option and vitamins are incorporated. An application in liquid Shape is only higher with the hard fats mentioned here Temperature possible, which is technically complex and when using vitamins often with the danger un desired loss of active ingredient 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 be stable to provide liquid formulations of water-soluble vitamins, which do not have the above-mentioned disadvantages of the prior art exhibit.
Diese Aufgabe wurde erfindungsgemäß gelöst durch ein Verfahren
zur Herstellung öliger Suspensionen wasserlöslicher Vitamine,
dadurch gekennzeichnet, daß man
This object was achieved according to the invention by a process for the preparation of oily suspensions of water-soluble vitamins, characterized in that
- a) mindestens ein wasserlösliches Vitamin in mindestens einem eßbaren Öl bis auf eine mittlere Partikelgröße von 0,1 bis 100 µm mahlt odera) at least one water-soluble vitamin in at least one edible oil down to an average particle size of 0.1 to 100 µm grinds or
- b) mindestens ein wasserlösliches Vitamin ohne Verwendung einer kontinuierlichen Phase bis auf eine mittlere Partikelgröße von 0,1 bis 100 µm mahlt und die gemahlenen Partikel an schließend in mindestens einem eßbaren Öl suspendiert.b) at least one water-soluble vitamin without using one continuous phase down to a medium particle size from 0.1 to 100 µm and the ground particles finally suspended in at least one edible oil.
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-monophosphate or calcium ascorbyl-2-polyphosphate, calcium panto thenate, panthenol , Vitamin B 1 (thiamine) - as hydrochloride, nitrate or pyrophosphate, vitamin B 2 (riboflavin) and their 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 Vitamin K3 (Menadion) als Natriumbisulfit genannt. Vitamin K 3 (menadione) may also be mentioned as sodium bisulfite as water-soluble vitamin.
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 sprühgetrocknetes Pulver eingesetzt werden. Bevorzugt sind die o. g. Vitamine in ihrer kristallinen Form.The above water soluble vitamins can be found in both crystalline form with a purity greater than 90%, preferred greater than 95%, particularly preferably greater than 98%, as well as in formulated form, for example as granules, beadlet or can be used as spray-dried powder. Are preferred the above 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 diesem Zusammenhang Sonnenblumenöl, Palmöl, Sesamöl, Maiskei möl, Baumwollsaatöl, Sojabohnenöl oder Erdnußöl, Ester mittel kettiger Triglyceride sowie außerdem Fischöle wie beispiels weise Makrelen-, 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.Edible oils are usually all physiologically safe oils - both of vegetable and animal origin - in particular oils that are liquid at 20 ° C or those in the suspension at 20 ° C alone or together with others Oils form the liquid phase. Preferred to be mentioned in In this connection, sunflower oil, palm oil, sesame oil, corn turkey oil, cottonseed oil, soybean oil or peanut oil, medium ester chain triglycerides as well as fish oils such as wise mackerel, sprat or salmon oil. For animal nutrition fish oils, corn oil, sunflower oil and Peanut oil. Are also advantageous for the food / pharmaceutical sector the esters of medium chain triglycerides.
Als eßbares Öl im Sinne der Erfindung sind auch Vitamin E, Vitamin E-Derivate oder Mischungen davon zu verstehen. Die Be zeichnung Vitamin E steht in diesem Zusammenhang für natürliches oder synthetisches α-, β-, γ- oder δ-Tocopherol, bevorzugt für natürliches oder synthetisches α-Tocopherol sowie für Toco trienol. Vitamin E-Derivate sind z. B. Tocopheryl-C1-C20-Alkyl ester wie Tocopherylacetat oder Tocopherylpalmitat.Vitamin E, vitamin E derivatives or mixtures thereof are also to be understood as edible oil in the sense of the invention. The term vitamin E in this context stands for natural or synthetic α-, β-, γ- or δ-tocopherol, preferably for natural or synthetic α-tocopherol and for tocotrienol. Vitamin E derivatives are e.g. B. tocopheryl-C 1 -C 20 alkyl esters such as tocopheryl acetate or tocopheryl palmitate.
Vitamin E und/oder deren Derivate können dabei allein oder zusammen mit den anderen eßbaren Ölen als Dispergiermedium verwendet werden.Vitamin E and / or their derivatives can be used alone or together with the other edible oils as a dispersing medium be used.
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 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 µm, insbesondere 1,0 bis 10 µm aufweisen. Der Begriff D[4,3] bezeichnet den volumengewichteten mittleren Durchmesser (siehe Handbuch zu Malvern Mastersizer S, Malvern Instruments Ltd., UK).The grinding can be carried out in a manner known per se, for. B. with a ball mill done. Depending on the type of mill used, this is the case long ground until the particles have a Fraunhofer diffraction determined average particle size D [4,3] from 0.1 to 100 µm, preferably 0.2 to 50 μm, particularly preferably 0.5 to 30 μm, entirely particularly preferably 0.8 to 20 μm, in particular 1.0 to 10 μm exhibit. The term D [4,3] denotes the volume-weighted medium diameter (see manual for Malvern Mastersizer S, Malvern Instruments Ltd., UK).
Nähere Einzelheiten zur Mahlung und den dafür eingesetzten Apparaturen finden sich u. a. in Ullmann's Encyclopedia of Industrial Chemistry, Sixth Edition, 1999, Electronic Release, Size Reduction, Kapitel 3.6.: Wet Grinding. More details about the grinding and the used for it Apparatus can be found u. a. in Ullmann's Encyclopedia of Industrial Chemistry, Sixth Edition, 1999, Electronic Release, Size Reduction, 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 process according to the invention it is possible to use all 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 ground in high concentration be ground in the oil to be used. The final preparation then results from a mixture of the 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 can be used before Ver greases or oils to the respective use concentration become thin.
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 special embodiment of the method according to the invention is characterized in that the grinding in the absence of a Emulsifier takes place. Surprisingly, it was found that fine-particle, homogeneous even without the addition of a surfactant Have suspensions of water-soluble vitamins produced in oils, which are stable to sedimentation even in high concentrations.
Eine weitere vorteilhafte Ausführungsform des erfindungsgemäßen Verfahrens ist dadurch gekennzeichnet, daß die Mahlung in Abwesenheit eines Schutzkolloids erfolgt.Another advantageous embodiment of the invention The method is characterized in that the grinding in Absence of a protective colloid occurs.
Trotz Fehlen der o. g. Dispergier- bzw. Formulierhilfsmittel konnten die an sich hydrophilen Vitamine - für den Fachmann unerwartet - ohne Benetzungsprobleme und Agglomeratbildung in den o. g. hydrophoben Dispergiermedien feinstgemahlen werden.Despite the absence of the above Dispersing or formulation aids the hydrophilic vitamins themselves - for the specialist unexpectedly - without wetting problems and agglomerate formation in the above hydrophobic dispersing media are finely ground.
Neben der oben beschriebenen Naßmahlung, lassen sich die erfindungsgemäßen öligen Suspensionen auch dadurch Trockenmahlung der wasserlöslichen Vitamine und anschließendes Suspendieren der gemahlenen Partikel in mindestens einem eßbaren Öl herstellen. Als Trockenmahlung versteht man in diesem Zusammenhang eine Mahlung ohne Verwendung einer kontinuierlichen Phase.In addition to the wet grinding described above, the oily suspensions according to the invention also thereby dry grinding of the water-soluble vitamins and subsequent suspension of the Make ground particles in at least one edible oil. In this context, dry grinding means one Grinding without using a continuous phase.
Nähere Einzelheiten zur Trockenmahlung finden sich u. a. in Ullmann's Encyclopedia of Industrial Chemistry, Sixth Edition, 1999, Electronic Release, Size Reduction, Kapitel 3.4.Further details on dry grinding can be found u. a. in Ullmann's Encyclopedia of Industrial Chemistry, Sixth Edition, 1999, Electronic Release, Size Reduction, Chapter 3.4.
Als besonderen Vorteil hinsichtlich der Stabilität der erfindungsgemäßen öligen Dispersionen hat sich herausgestellt, wenn man die Mahlung in den Verfahrensvarianten a) oder b) in Gegenwart von Trockenmitteln, ausgewählt aus der Gruppe, bestehend aus Alkali- und Erdalkalisulfaten wie Natrium-, Calcium- und Magnesiumsulfat, Alkali- und Erdalkalichloriden wie Natrium-, Calcium- und Magnesiumchlorid und Kieselgel durchführt. Als ganz besonders bevorzugtes Trockenmittel ist CaCl2 zu nennen.A particular advantage with regard to the stability of the oily dispersions according to the invention has been found when grinding in process variants a) or b) in the presence of drying agents selected from the group consisting of alkali and alkaline earth metal sulfates such as sodium, calcium and magnesium sulfate , Alkali and alkaline earth chlorides such as sodium, calcium and magnesium chloride and silica gel. CaCl 2 should be mentioned as a particularly preferred desiccant.
Die Menge an eingesetztem Trockenmittel liegt im allgemeinen zwischen 0,1 und 20 Gew.-%, bevorzugt zwischen 0,5 und 15 Gew.-%, besonders bevorzugt zwischen 1,0 und 10 Gew.-%, bezogen auf die Gesamtmenge der öligen Suspension.The amount of desiccant used is generally between 0.1 and 20% by weight, preferably between 0.5 and 15% by weight, particularly preferably between 1.0 and 10% by weight, based on the Total amount of the oily suspension.
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 fine distribution of the dispersed water Soluble vitamins excel according to the invention Process produced oily suspensions through a high bio availability of the active ingredients contained in the suspension.
Neben den eingangs genannten wasserlöslichen Vitaminen können vor, während oder nach der Mahlung zusätzliche fettlösliche Vitamine, 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 at the beginning, additional fat-soluble vitamins such as, for example, B. 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 entered and dissolved in the oily suspension. Grinding is preferably carried out 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 wasser lösliches Vitamin in mindestens einem eßbaren Öl bis auf eine mittlere Partikelgröße von 0,1 bis 100 µm mahlt.The invention also relates to at least oily suspensions a water-soluble vitamin, obtainable by a process, which is characterized in that at least one water soluble vitamin in at least one edible oil except for one average particle size of 0.1 to 100 µm grinds.
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 according to the invention contain 5 to 70% by weight, preferably 5 to 60% by weight, particularly preferably 10 to 55% by weight very particularly preferably at least 15 to 50% by weight one of the water-soluble vitamins mentioned in fine ground 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 can additionally 0.5 to 60% by weight, preferably 5 to 50% by weight, particularly preferably 10 to 45% by weight, very particularly preferably at least 15 to 40% by weight one of the fat-soluble vitamins mentioned in the solution Form included.
Darüberhinaus können die öligen Zubereitungen zusätzlich mindestens ein weiteres Carotinoid enthalten.In addition, the oily preparations can also 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,
Lycopin, Lutein, Astaxanthin, Zeaxanthin, Citranaxanthin und
Canthaxanthin.Among carotenoids are e.g. B. understand the following connections:
β-carotene, lycopene, lutein, astaxanthin, zeaxanthin, cryptoxanthine, citranaxanthin, canthaxanthin, bixin, β-apo-4-carotinal, β-apo-8-carotinal, β-apo-8-carotinic acid esters, individually or as a mixture. Carotenoids which are preferably used are β-carotene, lycopene, lutein, astaxanthin, zeaxanthin, citranaxanthin and canthaxanthin.
Die Carotinoide können dabei in kristalliner Form oder als Formulierung - beispielsweise als Trockenpulver, gemäß EP-A-0 065 193 eingesetzt werden.The carotenoids can be in crystalline form or as a formulation - for example as dry powder, according to EP-A-0 065 193 can be used.
Vorteilhafterweise werden die Carotinoide in der Regel in kristalliner Form zusammen mit den wasserlöslichen Vitaminen in dem Öl gemahlen. Im Falle von Astaxanthin und Canthaxanthin werden bevorzugt Astaxanthin- bzw. Canthaxanthin-haltige Trocken pulver, beispielsweise Lucantin® Pink bzw. Lucantin® Rot (ein 10%iges Astaxanthin- bzw. Canthaxanthin-Trockenpulver, Fa. BASF Aktiengesellschaft, Ludwigshafen, Deutschland) zusammen mit den wasserlöslichen Vitaminen eingesetzt.Advantageously, the carotenoids are usually in crystalline form together with the water soluble vitamins in ground the oil. In the case of astaxanthin and canthaxanthin are preferred astaxanthin or canthaxanthin-containing dry powder, for example Lucantin® Pink or Lucantin® Red (a 10% astaxanthin or canthaxanthin dry powder, from BASF Aktiengesellschaft, Ludwigshafen, Germany) together with the water-soluble vitamins.
Der Gehalt an Carotinoide liegt in den Formulierungen im all gemeinen zwischen 0,1 und 40 Gew.-%, bevorzugt zwischen 0,3 und 20 Gew.-%, besonders bevorzugt zwischen 0,5 und 10 Gew.-%, ganz 3 besonders bevorzugt zwischen 1 und 5 Gew.-%, bezogen auf die Gesamtmenge der Formulierung.The carotenoid content in the formulations lies in all generally between 0.1 and 40 wt .-%, preferably between 0.3 and 20% by weight, particularly preferably between 0.5 and 10% by weight, entirely 3 particularly preferably between 1 and 5 wt .-%, based on the Total amount of formulation.
Je nach Anwendungszweck können die erfindungsgemäßen öligen Zubereitungen bis zu 10 Gew.-% weiterer Zusatzkomponenten wie beispielsweise Mineralstoffe, Aminosäuren, Proteine oder Enzyme enthalten.Depending on the application, the oily according to the invention Preparations up to 10% by weight of additional components such as for example minerals, amino acids, proteins or enzymes contain.
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 above. fat-soluble vitamins and carotenoids, can be before, during or after the grinding of the suspension according to the invention can be added. To one if possible finely divided homogeneous suspension of all non-oil-soluble stocks To receive parts, it is advantageous to use the above. additives also 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-, Natrium- 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. 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, Sodium or iron phosphate, cobalt carbonate, sodium selenate or Silica and its salts incorporated into the suspension and be co-ground. The amount of minerals used, for example in the area of animal nutrition according to the needs 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, Hippursäure, Serin und Taurin. Besonders bevorzugt sind Lysin, Methionin und Cystein.In general, all known physiological residues come as amino acid residues harmless α-amino acid residues in question. To be preferred 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, Hippuric acid, serine and taurine. Lysine is particularly preferred, Methionine and cysteine.
Als Enzyme kommen in diesem Zusammenhang bevorzugt Phosphatasen Glucanasen und gegebenenfalls Esterasen bzw. Lipasen, letztere in verkapselter Form, in Frage.In this connection, the preferred enzymes are phosphatases Glucanases and optionally esterases or lipases, the latter in encapsulated form, in question.
Weitere Bestandteile der Suspension können sein:
Verbindungen mit Vitamin- oder Coenzymcharakter, z. B. Cholin
chlorid, Carnitin, γ-Butyrobetain, Liponsäure, Kreatin,
Ubichinone, S-Methylmethionin, S-Adenosylmethionin.Other components of the suspension can be:
Compounds with a vitamin or coenzyme character, e.g. B. choline chloride, carnitine, γ-butyrobetaine, lipoic acid, creatine, ubiquinones, S-methylmethionine, S-adenosylmethionine.
Mehrfach ungesättigte Fettsäuren, z. B. Linolsäure, Linolensäure, Arachidonsäure, Eicosapentaensäure, Docosahexaensäure.Polyunsaturated fatty acids, e.g. B. 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, Anti oxidantien, Verdicker, Chelatbildner, wie z. B. Alkali- oder Erd alkalisalze der Citronensäure, Phytinsäure oder Phosphorsäure enthalten und/oder Emulgatoren enthalten.In some cases it may be necessary that the oily Suspensions also auxiliary substances, such as. B. protective colloids, anti oxidants, thickeners, chelating agents, such as. B. alkali or earth alkali 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.Protective colloids that can be used include, for example, gelatin, fish gelatin, Starch, dextrin, plant proteins, pectin, gum arabic, Casein, caseinate or mixtures thereof are used. It can but also polyvinyl alcohol, polyvinyl pyrrolidone, methyl cellulose, Carboxymethyl cellulose, hydroxypropyl cellulose and alginates be set. For more details, see 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 Ethoxyquin 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 add ethoxyquin.
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 mikrobio logische Probleme in öligen, wasserfreien Systemen nicht zu erwarten.The oily suspensions according to the invention have u. a. the advantage, that the vitamins through the oil against oxygen and moisture are protected. The water-soluble vitamins and minerals are almost insoluble in oil and therefore cannot react interact with each other (compatibility). In addition, are microbiological logical problems in oily, water-free systems too expect.
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 animal and animal feed preparations or compound feed, as Agents for the manufacture of pharmaceutical and cosmetic Preparations and for the manufacture of nutritional supplements preparations in the human and animal area.
Bevorzugt lassen sich die Suspensionen als Futtermittelzusatz in der Tierernährung einsetzen, insbesondere zum Auftragen bzw. Auf sprühen auf Futtermittelpellets.The suspensions can preferably be added as feed use animal nutrition, especially for application or application 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 use as a feed additive is particularly important by directly spraying on the suspensions according to the invention, optionally after dilution with oils, for example on animals 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.There is a preferred embodiment of the spraying process 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. 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 areas of application in the food sector are, for example wise the vitaminization of beverages, dairy products like Yogurt, milk mix drinks or milk ice cream and pudding powders, egg products, baking mixes and confectionery.
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 sector, 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 applied.
Gegenstand der Erfindung sind ferner Nahrungsergänzungsmittel, Tierfuttermittel, Lebensmittel sowie pharmazeutische und kosmetische Zubereitungen, enthaltend die eingangs beschriebenen öligen Suspensionen wasserlöslicher Vitamine.The invention further relates to food supplements, Animal feed, food and pharmaceutical and cosmetic preparations containing those described in the introduction oily suspensions of water-soluble vitamins.
Bevorzugt richtet sich die Erfindung auf Tierfuttermittel, insbesondere auf Futtermittelpellets, die mit den Suspensionen beladen werden.The invention is preferably directed to animal feed, especially on feed pellets containing the suspensions be loaded.
Unter Nahrungsergänzungspräparate sowie pharmazeutische Zubereitungen, die die erfindungsgemäße Suspension enthalten, sind u. a. Tabletten, Dragees sowie bevorzugt Hart- und Weich gelatinekapseln zu verstehen.Taking nutritional supplements as well as pharmaceutical Preparations containing the suspension according to the invention, are u. a. Tablets, coated tablets and preferably hard and soft to understand gelatin capsules.
Kosmetische Zubereitungen, die die erfindungsgemäßen Suspensionen enthalten können, sind beispielsweise topisch anwendbare Zubereitungen, insbesondere dekorative Körperpflegemittel wie Lippenstifte, Gesichts-Make-up in Form einer Creme sowie Lotionen.Cosmetic preparations containing the suspensions according to the invention can contain, for example, are topically applicable Preparations, in particular decorative personal care products such as Lipsticks, facial makeup in the form of a cream as well Lotions.
In den folgenden Beispielen wird die Herstellung der erfindungs gemäßen öligen Suspensionen wasserlöslicher Vitamine näher erläutert.In the following examples, the preparation of the Invention according to oily suspensions of water-soluble vitamins explained.
Zwei Kilogramm einer Mischung aus 25 Gew.-% Vitamin C (99%ig, BASF Aktiengesellschaft) und 75 Gew.-% eines mittelkettigen Triglycerids (Delios® SK der Fa. Grünau, Deutschland) wurden mit einem Blattrührer solange gerührt, bis eine homogene Suspension vorlag. Danach wurde die Mischung in eine rührbare Vorlage um gefüllt, aus der die Suspension mittels Schlauchpumpe durch eine kontinuierlich betriebene Kugelmühle (Dyno Mill KDL Spezial) gefördert wurde. Der Mahlbehälter der Kugelmühle war mit 400 g Glaskugeln (Durchmesser 800 bis 1200 µm) gefüllt. Die aus der Mühle austretende feinteilige Suspension wurde aufgefangen und mittels eines Partikelgrößenmeßgerätes (Malvern Mastersizer) vermessen. Der Mahlvorgang wurde so oft wiederholt bis 90% der suspendierten Teilchen eine Teilchengröße kleiner 10 µm [D(0.9) < 10 µm] hatten. Dies entsprach einer mittleren Partikelgröße 0[4,3] von 5,2 µm.Two kilograms of a mixture of 25% by weight of vitamin C (99%, BASF Aktiengesellschaft) and 75% by weight of a medium chain Triglycerides (Delios® SK from Grünau, Germany) were also included a blade stirrer until a homogeneous suspension Template. The mixture was then converted into a stirrable template filled, from which the suspension by means of a peristaltic pump continuously operated ball mill (Dyno Mill KDL special) was promoted. The grinding bowl of the ball mill was 400 g Glass balls (diameter 800 to 1200 µm) filled. The one from the The fine particulate suspension emerging was collected and using a particle size measuring device (Malvern Mastersizer) measured. The grinding process was repeated until 90% of the time suspended particles a particle size smaller than 10 µm [D (0.9) <10 µm]. This corresponded to an average particle size 0 [4.3] of 5.2 µm.
Nach der Abtrennung von den Mahlkörpern wurde ein Teil der Dispersion mit der 10 fachen Menge des verwendeten Öls verdünnt und über 12 h stehengelassen. Weder die unverdünnte noch die verdünnte Dispersion zeigten über diesen Zeitraum Sedimentations erscheinungen. After separation from the grinding media, part of the Dispersion diluted with 10 times the amount of oil used and left over 12 h. Neither the undiluted nor the dilute dispersion showed sedimentation over this period 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 Kugelmühle gefördert wurde. Der Mahlvorgang wurde so oft wieder holt 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 blade stirrer until a homogeneous Suspension was present. The mixture was then turned into a stirrable Transfer the template from which the suspension is pumped using a peristaltic pump by the continuously operated one mentioned in Example 1 Ball mill was promoted. The grinding process was repeated so often catches up to 90% of the suspended particles a particle size less than 20 µm [D (0.9) <20 µm]. This corresponded to one average particle size D [4.3] of 10.9 µm.
Nach der Abtrennung von den Mahlkörpern wurde ein Teil der Dispersion mit der 10 fachen Menge Maiskeimöl 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, part of the Dispersion diluted with 10 times the amount of corn oil and left over 12 h. Neither the undiluted nor the ver thin dispersion showed sedimentation over this period phenomena.
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 analogously to Example 2 and by a continuous operated ball mill ground. The grinding process was so long performed up to 90% of the suspended particles one 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 Dispersion mit der 10 fachen Menge Maiskeimöl 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, part of the Dispersion diluted with 10 times the amount of corn 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
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 grinding process was carried out until 90% the suspended particles have a particle size of less than 20 μm [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 10 fachen Menge Maiskeimöl 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, part of the Dispersion diluted with 10 times the amount of corn 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
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 grinding process was carried out until 90% the suspended particles have a particle size of less than 20 μm [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 10 fachen 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, part of the Dispersion 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
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 grinding process was carried out until 90% the suspended particles have a particle size of less than 20 μm [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 10 fachen Menge Fischöl 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, part of the Dispersion diluted with 10 times the amount of fish 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
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 grinding process was carried out until 90% the suspended particles have a particle size of less than 20 μm [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 10 fachen Menge Maiskaimöl 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, part of the Dispersion diluted with 10 times the amount of corn 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
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 grinding process was carried out until 90% the suspended particles have a particle size of less than 20 μm [D (0.9) <20 µm].
Nach der Abtrennung von den Mahlkörpern wurde ein Teil der Dispersion mit der 10 fachen Menge Fischöl 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, part of the Dispersion diluted with 10 times the amount of fish 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
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 grinding process was carried out until 90% the suspended particles have a particle size of less than 20 μm [D (0.9) <20 µm].
Nach der Abtrennung von den Mahlkörpern würde ein Teil der Dispersion mit der 10 fachen Menge Maiskeimöl 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, part of the Dispersion diluted with 10 times the amount of corn oil and left over 12 h. Neither the undiluted nor the ver thin dispersion showed sedimentation over this period phenomena.
Analog Beispiel 4 wurde eine Mischung aus
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 grinding process was carried out until 90% the suspended particles have a particle size of less than 20 μm [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 10 fachen Menge Maiskeimöl verdünnt und über einen Zeitraum von einem Monat bei 40°C gelagert. Weder die unver dünnte noch die verdünnte Dispersion zeigten über diesen Zeitraum Sedimentationserscheinungen.After separation from the grinding media, part of the Dispersion diluted with 10 times the amount of corn oil and over stored at 40 ° C for a period of one month. Neither the uncorrect thinned the diluted dispersion showed over this period Sedimentation.
Claims (17)
- a) mindestens ein wasserlösliches Vitamin in mindestens einem eßbaren Öl bis auf eine mittlere Partikelgröße von 0,1 bis 100 µm mahlt oder
- b) mindestens ein wasserlösliches Vitamin ohne Verwendung einer kontinuierlichen Phase bis auf eine mittlere Partikelgröße von 0,1 bis 100 µm mahlt und die gemahlenen Partikel anschließend in mindestens einem eßbaren Öl suspendiert.
- a) grinding at least one water-soluble vitamin in at least one edible oil to an average particle size of 0.1 to 100 microns or
- b) grinding at least one water-soluble vitamin without using a continuous phase to an average particle size of 0.1 to 100 μm and then suspending the ground particles in at least one edible oil.
Priority Applications (11)
Application Number | Priority Date | Filing Date | Title |
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DE10049137A DE10049137A1 (en) | 2000-10-04 | 2000-10-04 | Production of oily suspensions of water soluble vitamins comprises milling of vitamins in oil or dry milling and suspension in oil |
AU2001254687A AU2001254687A1 (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 |
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 |
EP01927730A EP1272059B1 (en) | 2000-03-17 | 2001-03-15 | Method of producing oily suspensions of water-soluble vitamins |
CNB01806695XA CN1197483C (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 |
DE50108311T DE50108311D1 (en) | 2000-03-17 | 2001-03-15 | PROCESS FOR PREPARING OILY SUSPENSIONS OF WATER SOLUBLE VITAMINS |
DK01927730T DK1272059T3 (en) | 2000-03-17 | 2001-03-15 | Process for the preparation of oily suspensions of water-soluble vitamins |
AT01927730T ATE311766T1 (en) | 2000-03-17 | 2001-03-15 | METHOD FOR PRODUCING OIL SUSPENSIONS OF WATER-SOLUBLE VITAMINS |
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DE10049137A DE10049137A1 (en) | 2000-10-04 | 2000-10-04 | Production of oily suspensions of water soluble vitamins comprises milling of vitamins in oil or dry milling and suspension in oil |
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Cited By (1)
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DE102004004030A1 (en) * | 2004-01-27 | 2005-08-18 | Mars Inc. | Food product and process for its production |
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2000
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DE102004004030A1 (en) * | 2004-01-27 | 2005-08-18 | Mars Inc. | Food product and process for its production |
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