WO2012047098A1 - Encapsulated fat-soluble vitamin - Google Patents
Encapsulated fat-soluble vitamin Download PDFInfo
- Publication number
- WO2012047098A1 WO2012047098A1 PCT/NL2011/050668 NL2011050668W WO2012047098A1 WO 2012047098 A1 WO2012047098 A1 WO 2012047098A1 NL 2011050668 W NL2011050668 W NL 2011050668W WO 2012047098 A1 WO2012047098 A1 WO 2012047098A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- vitamin
- fat
- encapsulated
- process according
- fatty phase
- Prior art date
Links
- 229940088594 vitamin Drugs 0.000 title claims abstract description 86
- 229930003231 vitamin Natural products 0.000 title claims abstract description 86
- 235000013343 vitamin Nutrition 0.000 title claims abstract description 86
- 239000011782 vitamin Substances 0.000 title claims abstract description 86
- 150000003722 vitamin derivatives Chemical class 0.000 title claims abstract description 67
- 238000000034 method Methods 0.000 claims abstract description 30
- 238000001816 cooling Methods 0.000 claims abstract description 14
- 238000004519 manufacturing process Methods 0.000 claims abstract description 11
- 238000002844 melting Methods 0.000 claims abstract description 11
- 230000008018 melting Effects 0.000 claims abstract description 11
- 239000012456 homogeneous solution Substances 0.000 claims abstract description 7
- 241001465754 Metazoa Species 0.000 claims abstract description 6
- QYSXJUFSXHHAJI-XFEUOLMDSA-N Vitamin D3 Natural products 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-XFEUOLMDSA-N 0.000 claims description 29
- 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 claims description 19
- 235000005282 vitamin D3 Nutrition 0.000 claims description 18
- 239000011647 vitamin D3 Substances 0.000 claims description 18
- 229940021056 vitamin d3 Drugs 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 16
- 235000013305 food Nutrition 0.000 claims description 13
- 229930003316 Vitamin D Natural products 0.000 claims description 11
- 235000019166 vitamin D Nutrition 0.000 claims description 11
- 239000011710 vitamin D Substances 0.000 claims description 11
- 150000003710 vitamin D derivatives Chemical class 0.000 claims description 11
- 229940046008 vitamin d Drugs 0.000 claims description 11
- 239000000843 powder Substances 0.000 claims description 10
- 239000004615 ingredient Substances 0.000 claims description 9
- 239000003963 antioxidant agent Substances 0.000 claims description 6
- 235000006708 antioxidants Nutrition 0.000 claims description 6
- 239000008172 hydrogenated vegetable oil Substances 0.000 claims description 6
- 230000003078 antioxidant effect Effects 0.000 claims description 5
- JWUBBDSIWDLEOM-UHFFFAOYSA-N 25-Hydroxycholecalciferol Natural products C1CCC2(C)C(C(CCCC(C)(C)O)C)CCC2C1=CC=C1CC(O)CCC1=C JWUBBDSIWDLEOM-UHFFFAOYSA-N 0.000 claims description 3
- JWUBBDSIWDLEOM-DCHLRESJSA-N 25-Hydroxyvitamin D3 Natural products C1(/[C@@H]2CC[C@@H]([C@]2(CCC1)C)[C@@H](CCCC(C)(C)O)C)=C/C=C1\C[C@@H](O)CCC1=C JWUBBDSIWDLEOM-DCHLRESJSA-N 0.000 claims description 3
- JWUBBDSIWDLEOM-NQZHSCJISA-N 25-hydroxy-3 epi cholecalciferol Chemical compound C1([C@@H]2CC[C@@H]([C@]2(CCC1)C)[C@@H](CCCC(C)(C)O)C)=CC=C1C[C@H](O)CCC1=C JWUBBDSIWDLEOM-NQZHSCJISA-N 0.000 claims description 3
- OVGORFFCBUIFIA-UHFFFAOYSA-N Fenipentol Chemical compound CCCCC(O)C1=CC=CC=C1 OVGORFFCBUIFIA-UHFFFAOYSA-N 0.000 claims description 2
- GVJHHUAWPYXKBD-UHFFFAOYSA-N d-alpha-tocopherol Natural products OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 claims description 2
- 229960001295 tocopherol Drugs 0.000 claims description 2
- 229930003799 tocopherol Natural products 0.000 claims description 2
- 235000010384 tocopherol Nutrition 0.000 claims description 2
- 239000011732 tocopherol Substances 0.000 claims description 2
- GVJHHUAWPYXKBD-IEOSBIPESA-N α-tocopherol Chemical compound OC1=C(C)C(C)=C2O[C@@](CCC[C@H](C)CCC[C@H](C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-IEOSBIPESA-N 0.000 claims description 2
- 238000005538 encapsulation Methods 0.000 description 10
- 239000003921 oil Substances 0.000 description 9
- 235000019198 oils Nutrition 0.000 description 9
- 230000003647 oxidation Effects 0.000 description 9
- 238000007254 oxidation reaction Methods 0.000 description 9
- 235000019197 fats Nutrition 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 238000003860 storage Methods 0.000 description 7
- 239000011159 matrix material Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 239000001993 wax Substances 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 5
- 235000019484 Rapeseed oil Nutrition 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical compound O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 description 4
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 4
- 229940072056 alginate Drugs 0.000 description 4
- 235000010443 alginic acid Nutrition 0.000 description 4
- 229920000615 alginic acid Polymers 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 235000019482 Palm oil Nutrition 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000000839 emulsion Substances 0.000 description 3
- 238000000265 homogenisation Methods 0.000 description 3
- 239000002540 palm oil Substances 0.000 description 3
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 description 2
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 description 2
- 239000001692 EU approved anti-caking agent Substances 0.000 description 2
- 229920002774 Maltodextrin Polymers 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 2
- 244000299461 Theobroma cacao Species 0.000 description 2
- 229930003268 Vitamin C Natural products 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 150000001720 carbohydrates Chemical class 0.000 description 2
- 239000004203 carnauba wax Substances 0.000 description 2
- 235000013869 carnauba wax Nutrition 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 150000004665 fatty acids Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 235000018102 proteins Nutrition 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 235000012424 soybean oil Nutrition 0.000 description 2
- 239000003549 soybean oil Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 235000019698 starch Nutrition 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- DCXXMTOCNZCJGO-UHFFFAOYSA-N tristearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(OC(=O)CCCCCCCCCCCCCCCCC)COC(=O)CCCCCCCCCCCCCCCCC DCXXMTOCNZCJGO-UHFFFAOYSA-N 0.000 description 2
- 235000015112 vegetable and seed oil Nutrition 0.000 description 2
- 235000019154 vitamin C Nutrition 0.000 description 2
- 239000011718 vitamin C Substances 0.000 description 2
- 244000215068 Acacia senegal Species 0.000 description 1
- 229920001817 Agar Polymers 0.000 description 1
- GUBGYTABKSRVRQ-XLOQQCSPSA-N Alpha-Lactose Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@H](O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-XLOQQCSPSA-N 0.000 description 1
- 239000005995 Aluminium silicate Substances 0.000 description 1
- 235000019737 Animal fat Nutrition 0.000 description 1
- 102000011632 Caseins Human genes 0.000 description 1
- 108010076119 Caseins Proteins 0.000 description 1
- 108010010803 Gelatin Proteins 0.000 description 1
- 235000010469 Glycine max Nutrition 0.000 description 1
- 229920000084 Gum arabic Polymers 0.000 description 1
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 description 1
- 229920001732 Lignosulfonate Polymers 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 239000005913 Maltodextrin Substances 0.000 description 1
- 229920000881 Modified starch Polymers 0.000 description 1
- 239000004368 Modified starch Substances 0.000 description 1
- 235000019483 Peanut oil Nutrition 0.000 description 1
- 235000004443 Ricinus communis Nutrition 0.000 description 1
- 235000019485 Safflower oil Nutrition 0.000 description 1
- 235000003434 Sesamum indicum Nutrition 0.000 description 1
- 244000000231 Sesamum indicum Species 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- 235000019486 Sunflower oil Nutrition 0.000 description 1
- 235000005764 Theobroma cacao ssp. cacao Nutrition 0.000 description 1
- 235000005767 Theobroma cacao ssp. sphaerocarpum Nutrition 0.000 description 1
- 239000000205 acacia gum Substances 0.000 description 1
- 235000010489 acacia gum Nutrition 0.000 description 1
- 239000008272 agar Substances 0.000 description 1
- 235000010419 agar Nutrition 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- PZZYQPZGQPZBDN-UHFFFAOYSA-N aluminium silicate Chemical compound O=[Al]O[Si](=O)O[Al]=O PZZYQPZGQPZBDN-UHFFFAOYSA-N 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 235000013871 bee wax Nutrition 0.000 description 1
- 239000012166 beeswax Substances 0.000 description 1
- 229940092738 beeswax Drugs 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 235000001046 cacaotero Nutrition 0.000 description 1
- 239000001506 calcium phosphate Substances 0.000 description 1
- 235000014633 carbohydrates Nutrition 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 235000019219 chocolate Nutrition 0.000 description 1
- 238000005354 coacervation Methods 0.000 description 1
- 229940110456 cocoa butter Drugs 0.000 description 1
- 235000019868 cocoa butter Nutrition 0.000 description 1
- 239000003240 coconut oil Substances 0.000 description 1
- 235000019864 coconut oil Nutrition 0.000 description 1
- 235000005687 corn oil Nutrition 0.000 description 1
- 239000002285 corn oil Substances 0.000 description 1
- 239000002385 cottonseed oil Substances 0.000 description 1
- 235000012343 cottonseed oil Nutrition 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 235000013376 functional food Nutrition 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 235000019866 hydrogenated palm kernel oil Nutrition 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000008101 lactose Substances 0.000 description 1
- 239000000944 linseed oil Substances 0.000 description 1
- 235000021388 linseed oil Nutrition 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 235000001055 magnesium Nutrition 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 229940035034 maltodextrin Drugs 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 235000019426 modified starch Nutrition 0.000 description 1
- 239000004006 olive oil Substances 0.000 description 1
- 235000008390 olive oil Nutrition 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 239000000312 peanut oil 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
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 235000005713 safflower oil Nutrition 0.000 description 1
- 239000003813 safflower oil Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229940080237 sodium caseinate Drugs 0.000 description 1
- 235000010356 sorbitol Nutrition 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 235000000346 sugar Nutrition 0.000 description 1
- 150000008163 sugars Chemical class 0.000 description 1
- 239000002600 sunflower oil Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 150000003626 triacylglycerols Chemical class 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
- 229940078499 tricalcium phosphate Drugs 0.000 description 1
- 229910000391 tricalcium phosphate Inorganic materials 0.000 description 1
- 235000019731 tricalcium phosphate Nutrition 0.000 description 1
- -1 vitamin AD Chemical class 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/10—Organic substances
- A23K20/174—Vitamins
-
- 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
- A23K40/30—Shaping or working-up of animal feeding-stuffs by encapsulating; by coating
-
- 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
- A23L33/155—Vitamins A or D
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
- A23P10/00—Shaping or working of foodstuffs characterised by the products
- A23P10/30—Encapsulation of particles, e.g. foodstuff additives
- A23P10/35—Encapsulation of particles, e.g. foodstuff additives with oils, lipids, monoglycerides or diglycerides
-
- 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
Definitions
- the present invention relates to a process for manufacturing an encapsulated fat-soluble vitamin, to an encapsulated fat-soluble vitamin obtainable by such process and to the use of such encapsulated fat-soluble vitamin.
- One of the techniques often used for encapsulation of water-soluble vitamins such as vitamin C is dispersion of the water-soluble vitamin in molten fat or wax followed by spray-cooling or spray-chilling of the dispersion.
- coating of water-soluble vitamin with a mixture of saturated C14-C18 fatty acids having a melting point of at least 45 °C is disclosed.
- the coating process involves suspension of the vitamin in the molten fatty material followed by the production of solid spheroidal particles by means of spray-chilling of the suspension.
- GB 340,580 is disclosed the preparation of vitamin D, a fat-soluble vitamin, in a form that is suitable for household purposes, in particular for providing the daily dosage of vitamin D to children in an attractive and easy way.
- the vitamin D is dissolved in cocoa butter and subsequently processed into chocolate or cacao products.
- fat-soluble vitamins are encapsulated by spray-drying of an emulsion of the fat-soluble vitamin, optionally dissolved in an oil phase, in a matrix material.
- the matrix material is optionally coated with starch or modified starch.
- the matrix material typically is a protein, for example gum arabic, sodium caseinate or gelatin, in combination with a carbohydrate, for example maltodextrin, sucrose or lactose.
- US 4,389,419 for example is disclosed a process for encapsulation of oil soluble vitamins in a shape-retaining water-insoluble alginate matrix.
- a process for encapsulation of oil soluble vitamins in a shape-retaining water-insoluble alginate matrix first an emulsion consisting of a continuous phase comprising an aqueous solution of an alginate and optionally a water-soluble filler such as a polysaccharide and a dispersed phase comprising the vitamin dissolved in oil is formed.
- the emulsion is then formed into droplets that are immersed in an alcoholic solution of multivalent cations in order to produce the shape-retaining alginate matrix enclosing the oil droplets.
- microencapsulation of 25-hydroxy vitamin D3 is disclosed.
- the vitamin D3 is first dissolved in oil and the resulting oil composition is then encapsulated in an encapsulation agent selected from starches, protein, pectin, alginate, agar, maltodextrins, lignin sulfonates, cellulose derivatives, saccharides, sugars, sorbitols, or gums.
- an encapsulation agent selected from starches, protein, pectin, alginate, agar, maltodextrins, lignin sulfonates, cellulose derivatives, saccharides, sugars, sorbitols, or gums.
- the present invention relates to a process for manufacturing an encapsulated fat- soluble vitamin comprising: (a) preparing a homogeneous solution of a fat-soluble vitamin in a molten fatty phase; and
- the invention relates to an encapsulated fat-soluble vitamin obtainable by a process as defined hereinbefore.
- the invention relates to the use of the encapsulated fat-soluble vitamin defined hereinbefore as ingredient in animal feed.
- an encapsulated fat-soluble vitamin is manufactured by first preparing a homogeneous solution of a fat-soluble vitamin in a molten fatty phase (step (a)) and subsequently cooling the homogeneous solution thus prepared to solidify the fatty phase such that fat-encapsulated vitamin is formed (step (b))-
- the fatty phase used has a melting temperature of at least 45 °C, preferably at least 55 °C, more preferably at least 58 °C.
- a too high processing temperature in step (a) is preferably avoided. Therefore, the fatty phase has a melting temperature of at most 90 °C, preferably at most 80 °C, more preferably at most 72 °C, even more preferably at most 68 °C.
- a fatty phase with a melting temperature in the range of from 58 to 68 °C is particularly preferred.
- a fat-soluble vitamin is homogeneously solved in the molten fatty phase.
- Such homogenization is carried out at a temperature above the melting temperature of the fatty phase.
- the homogenization is carried out at a temperature below 100 °C, more preferably at a temperature in the range of from 80 to 95 °C.
- the preparation of the homogenous solution may be carried out in any suitable way known in the art.
- a molten fatty phase will first be provided and then the fat-soluble vitamin will be added to the molten fatty phase.
- further ingredients such as anti-oxidants or anti-caking agents may be added to the molten fatty phase.
- the fat-soluble vitamin may be added in any suitable form, for example in crystalline form, in the form of a vitamin resin or dissolved in an oil or fat. After or during addition of the fat-soluble vitamin and the optional further ingredients, mixing is applied to form a homogeneous solution of the vitamin in the molten fatty phase.
- Subsequent cooling step (b) may be any suitable cooling step known in the art. Cooling techniques that enable formation of the encapsulated vitamin in powder form are preferred. Preferably, the cooling is spray-cooling or spray-chilling. Spray-cooling and spray-chilling are techniques well-known in the art.
- the fatty phase may comprise any food grade or feed grade fatty compound such as for example triglycerides, other esters of fatty acids, waxes or combination of two or more thereof.
- the fatty phase preferably comprises a hydrogenated animal fat or oil, a hydrogenated vegetable oil, a feed grade or food grade wax or a combination of two or more thereof.
- the fatty phase essentially consists of one or more hydrogenated vegetable oils such as hydrogenated palm kernel oil, palm oil, rape seed oil, soy oil, sunflower oil, safflower oil, coconut oil, peanut oil, corn oil, cotton seed oil, sesame seed oil, olive oil, linseed oil or castor seed oil or of a feed grade or food grade wax such as for example carnauba wax, bees wax or edible paraffin wax.
- the fatty phase is a hydrogenated vegetable oil or a food grade wax, still more preferably a hydrogenated vegetable oil.
- the process according to the invention is suitable for encapsulation of any fat- soluble vitamin.
- the vitamin may thus be any fat-soluble vitamin such as vitamin AD, E or K, including any of its analogues.
- the vitamin is vitamin D or any of its analogues.
- Reference to vitamin D is to any one of vitamin Dl, D2, D3, D4 or D5. More preferably, the vitamin is vitamin D3 or any of its analogues.
- a particularly preferred vitamin is 25 -hydroxy vitamin D3, an analogue of vitamin D3.
- the vitamin may be added to the molten fatty phase in any suitable amount.
- the vitamin is preferably added in such amount that a concentration in the range of from 0.1 to 0.8 million international units (IU) per gram of the resulting encapsulated vitamin is obtained, more preferably of from 0.2 to 0.6 million IU per gram.
- IU international units
- One million IU of vitamin D3 corresponds to 25 mg of vitamin D3.
- an anti-oxidant is added to the fatty phase in step (a).
- Any suitable anti-oxidant may be used.
- the anti-oxidant is selected from the group consisting of butyl hydroxyl toluene, tocopherol, and etoxyquin.
- the encapsulated fat-soluble vitamin obtainable by the process according to the invention is preferably in powder form.
- Powder with an average particle size in the range of from 100 to 850 ⁇ is preferred.
- An advantage of an average particle size of at least 100 ⁇ is that oxidation stability is improved as compared to particles with a smaller diameter.
- the average particle size is preferably at most 850 ⁇ , more preferably at most 750 ⁇ , even more preferably at most 500 ⁇ .
- An average particle size of at most 300 ⁇ is particularly preferred.
- the particle size can be controlled by adjusting the spray-chilling or spray-cooling conditions, in particular the flow rate of the solution through the spray-chilling or spray-cooling nozzle and the flow rate of the atomizing gas.
- Reference herein to the average particle size is to the average particle diameter.
- an anti-caking agent is optionally added to the powder formed in step b). Any suitable anti-caking agent may be used.
- Preferred anti-caking agents are silicon dioxide, tri calcium phosphate and magnesium aluminium silicate.
- the encapsulated fat-soluble vitamin according to the invention is particularly suitable for use as ingredient in food products or in animal feed, in particular in animal feed. It has been found that the encapsulated vitamin can suitably be processed at a temperature in the order of 80-90 °C, a temperature commonly used in the manufacture of animal feed. Examples
- the thus-obtained homogeneous solution of vitamin D3 in the molten fat phase was spray-chilled by pumping it (40 rpm, approximately 30 g/min) through heated tubing (95 °C) to a two-fluid nozzle (diameter 2.0 mm) and spraying it with nitrogen gas into liquid nitrogen to form particles with a particle size ranging from 100 to 650 ⁇ .
- the pumping rate of the vitamin solution and the nitrogen pressure the particle size could be adjusted.
- the homogeneity and the stability of the encapsulated vitamin was determined. For determining the homogeneity, five samples of 10 grams each were taken from the entire batch and analysed with respect to vitamin D3 content. The average vitamin D3 content appeared to be 0.507 million IU per gram with a standard deviation of 0.003 million IU per gram. After storage for three months at 40 °C and a relative humidity of 75%, the vitamin D3 content of samples appeared to be at the same level as just after manufacture. This shows that no oxidation or other degradation reaction had occurred. EXAMPLE 2 (according to the invention)
- Example 2 the homogeneity and the stability of the encapsulated vitamin was determined.
- the average vitamin D3 content appeared to be 0.504 million IU per gram with a standard deviation of 0.003 million IU per gram.
- the vitamin D3 content of samples appeared to be at the same level as just after manufacture. This shows that no oxidation or other degradation reaction had occurred.
- EXAMPLE 3 (according to the invention) The experiment of EXAMPLE 1 was repeated, but now with carnauba wax (ex Paramelt, Alkmaar, The Netherlands) instead of hydrogenated rape seed oil.
- the vitamin D3 content of the samples was determined and appeared to be at the same level as just after manufacture. This shows that no oxidation or other degradation had occurred.
- the material was sprayed into a large scale spray chiller at a rate of 500 kg/h to form particles with an average particle size of 250 ⁇ . Samples were taken after each 500 kg of product. The average vitamin D3 content was 0.57 MlU/g for all samples with a standard deviation of 0.01 MlU/g.
- Samples of the vitamin powder were stored at three different conditions: 25°C and 60% relative humidity; 30°C and 65% relative humidity; and 40°C and 75% relative humidity.
- the vitamin D3 content of the samples was determined and appeared to be at the same level as just after manufacture. This shows that no oxidation or other degradation had occurred.
Abstract
The present invention relates to a process for manufacturing an encapsulated fat- soluble vitamin comprising: (a) preparing a homogeneous solution of a fat-soluble vitamin in a molten fatty phase; and (b) cooling the solution to solidify the fatty phase and form the encapsulated vitamin, wherein the fatty phase has a melting point in the range of from 45 to 90 °C. The invention further relates to an encapsulated fat-soluble vitamin obtainable by such process and to the use of such encapsulated fat-soluble vitamin in animal feed.
Description
ENCAPSULATED FAT-SOLUBLE VITAMIN
Field of the invention
The present invention relates to a process for manufacturing an encapsulated fat-soluble vitamin, to an encapsulated fat-soluble vitamin obtainable by such process and to the use of such encapsulated fat-soluble vitamin.
Background of the invention
There is an increasing demand for industrially prepared food and feed products that comprise health promoting compounds such as vitamins. In order to avoid that vitamins react too early, i.e. during storage or manufacture of the food or feed product, with other food or feed ingredients, microencapsulation of vitamins is often applied. In this way, a barrier against chemical reactions is provided and vitamin retention is improved. Moreover, vitamins are typically used in low dosages that are difficult to distribute homogeneously throughout the food or feed products. Micro-encapsulation provides an adequate dilution of the vitamins in a form that has good distribution properties. Some vitamins, such as for example vitamin D, are extremely toxic in its undiluted form and handling such undiluted vitamins would required very stringent safety measures. Handling of micro-encapsulated vitamins requires less stringent safety measures.
One of the techniques often used for encapsulation of water-soluble vitamins such as vitamin C is dispersion of the water-soluble vitamin in molten fat or wax followed by spray-cooling or spray-chilling of the dispersion. In GB 922,697 for example, coating of water-soluble vitamin with a mixture of saturated C14-C18 fatty acids having a melting point of at least 45 °C is disclosed. The coating process involves suspension of the vitamin in the molten fatty material followed by the production of solid spheroidal particles by means of spray-chilling of the suspension.
In GB 340,580 is disclosed the preparation of vitamin D, a fat-soluble vitamin, in a form that is suitable for household purposes, in particular for providing the daily dosage of vitamin D to children in an attractive and easy way. The vitamin D is dissolved in cocoa butter and subsequently processed into chocolate or cacao products.
For fat-soluble vitamins, encapsulation in a solid fat or wax phase, such as typically done for vitamin C, was never applied for the provision of a vitamin
ingredient for the industrial production of functional food or feed products. Such fat encapsulation was not seen as providing a sufficient barrier in view of the solubility of the vitamins in the fatty composition. Also, because of the high sensitivity of vitamin D to oxidation, a fat coating was not seen as sufficient protection in the further processing of vitamin D, since any downstream high temperature processing step would expose the vitamin again to oxidation conditions.
Typically, fat-soluble vitamins are encapsulated by spray-drying of an emulsion of the fat-soluble vitamin, optionally dissolved in an oil phase, in a matrix material. The matrix material is optionally coated with starch or modified starch. The matrix material typically is a protein, for example gum arabic, sodium caseinate or gelatin, in combination with a carbohydrate, for example maltodextrin, sucrose or lactose.
In US 4,389,419 for example is disclosed a process for encapsulation of oil soluble vitamins in a shape-retaining water-insoluble alginate matrix. In the process of US 4,389,419, first an emulsion consisting of a continuous phase comprising an aqueous solution of an alginate and optionally a water-soluble filler such as a polysaccharide and a dispersed phase comprising the vitamin dissolved in oil is formed. The emulsion is then formed into droplets that are immersed in an alcoholic solution of multivalent cations in order to produce the shape-retaining alginate matrix enclosing the oil droplets.
In US 2003/0170324 microencapsulation of 25-hydroxy vitamin D3 is disclosed. The vitamin D3 is first dissolved in oil and the resulting oil composition is then encapsulated in an encapsulation agent selected from starches, protein, pectin, alginate, agar, maltodextrins, lignin sulfonates, cellulose derivatives, saccharides, sugars, sorbitols, or gums.
Also, relatively expensive formulation processes like spray congealing or complex coacervation are used for encapsulation of vitamin D and other fat-soluble vitamins.
Since achieving the droplet size distribution in the matrix material required for a homogenous product is relatively complex, the above-mentioned encapsulation techniques for fat-soluble vitamins are expensive.
Summary of the invention
The present invention relates to a process for manufacturing an encapsulated fat- soluble vitamin comprising:
(a) preparing a homogeneous solution of a fat-soluble vitamin in a molten fatty phase; and
(b) cooling the solution to solidify the fatty phase and form the encapsulated vitamin, wherein the fatty phase has a melting point in the range of from 45 to 90 °C.
It has been found that encapsulation of fat-soluble vitamins in a fatty phase that melts at a temperature of at least 45 °C, preferably at least 55 °C, by the process according to the invention provides fat-encapsulated vitamins that can be suitably used as ingredient in industrially produced food or feed products. The fat coating thus produced appears to be sufficiently stable to protect the encapsulated vitamins against undesired chemical reactions such as oxidation during storage and further processing into food and feed products.
In a further aspect, the invention relates to an encapsulated fat-soluble vitamin obtainable by a process as defined hereinbefore.
In a final aspect, the invention relates to the use of the encapsulated fat-soluble vitamin defined hereinbefore as ingredient in animal feed.
Detailed description of the invention
In the process according to the invention, an encapsulated fat-soluble vitamin is manufactured by first preparing a homogeneous solution of a fat-soluble vitamin in a molten fatty phase (step (a)) and subsequently cooling the homogeneous solution thus prepared to solidify the fatty phase such that fat-encapsulated vitamin is formed (step (b))-
In order to form an encapsulated fat-soluble vitamin that has a coating that is sufficiently stable to protect the vitamin against undesirable chemical reactions, in particular oxidation, during storage and during further processing steps, the fatty phase used has a melting temperature of at least 45 °C, preferably at least 55 °C, more preferably at least 58 °C. In view of the instability of most fat-soluble vitamins, in particular vitamin D, a too high processing temperature in step (a) is preferably avoided. Therefore, the fatty phase has a melting temperature of at most 90 °C, preferably at most 80 °C, more preferably at most 72 °C, even more preferably at most 68 °C. A fatty phase with a melting temperature in the range of from 58 to 68 °C is particularly preferred.
Reference herein to the melting temperature is to the initial melting temperature of the fatty phase.
In step (a) a fat-soluble vitamin is homogeneously solved in the molten fatty phase. Such homogenization is carried out at a temperature above the melting temperature of the fatty phase. Preferably, the homogenization is carried out at a temperature below 100 °C, more preferably at a temperature in the range of from 80 to 95 °C.
The preparation of the homogenous solution may be carried out in any suitable way known in the art. Typically, a molten fatty phase will first be provided and then the fat-soluble vitamin will be added to the molten fatty phase. Optionally, further ingredients such as anti-oxidants or anti-caking agents may be added to the molten fatty phase. The fat-soluble vitamin may be added in any suitable form, for example in crystalline form, in the form of a vitamin resin or dissolved in an oil or fat. After or during addition of the fat-soluble vitamin and the optional further ingredients, mixing is applied to form a homogeneous solution of the vitamin in the molten fatty phase.
Subsequent cooling step (b) may be any suitable cooling step known in the art. Cooling techniques that enable formation of the encapsulated vitamin in powder form are preferred. Preferably, the cooling is spray-cooling or spray-chilling. Spray-cooling and spray-chilling are techniques well-known in the art.
The fatty phase may comprise any food grade or feed grade fatty compound such as for example triglycerides, other esters of fatty acids, waxes or combination of two or more thereof. The fatty phase preferably comprises a hydrogenated animal fat or oil, a hydrogenated vegetable oil, a feed grade or food grade wax or a combination of two or more thereof. More preferably the fatty phase essentially consists of one or more hydrogenated vegetable oils such as hydrogenated palm kernel oil, palm oil, rape seed oil, soy oil, sunflower oil, safflower oil, coconut oil, peanut oil, corn oil, cotton seed oil, sesame seed oil, olive oil, linseed oil or castor seed oil or of a feed grade or food grade wax such as for example carnauba wax, bees wax or edible paraffin wax. Even more preferably the fatty phase is a hydrogenated vegetable oil or a food grade wax, still more preferably a hydrogenated vegetable oil.
The process according to the invention is suitable for encapsulation of any fat- soluble vitamin. The vitamin may thus be any fat-soluble vitamin such as vitamin AD, E or K, including any of its analogues. Preferably the vitamin is vitamin D or any of its analogues. Reference to vitamin D is to any one of vitamin Dl, D2, D3, D4 or D5.
More preferably, the vitamin is vitamin D3 or any of its analogues. A particularly preferred vitamin is 25 -hydroxy vitamin D3, an analogue of vitamin D3.
The vitamin may be added to the molten fatty phase in any suitable amount. For vitamin D3, the vitamin is preferably added in such amount that a concentration in the range of from 0.1 to 0.8 million international units (IU) per gram of the resulting encapsulated vitamin is obtained, more preferably of from 0.2 to 0.6 million IU per gram. One million IU of vitamin D3 corresponds to 25 mg of vitamin D3.
Preferably an anti-oxidant is added to the fatty phase in step (a). Any suitable anti-oxidant may be used. Preferably, the anti-oxidant is selected from the group consisting of butyl hydroxyl toluene, tocopherol, and etoxyquin.
The encapsulated fat-soluble vitamin obtainable by the process according to the invention is preferably in powder form. Powder with an average particle size in the range of from 100 to 850 μιη is preferred. An advantage of an average particle size of at least 100 μιη is that oxidation stability is improved as compared to particles with a smaller diameter. In order to be able to mix the vitamin powder homogeneously with other food or feed ingredients, the average particle size is preferably at most 850 μιη, more preferably at most 750 μιη, even more preferably at most 500 μιη. An average particle size of at most 300 μιη is particularly preferred. It will be appreciated that the particle size can be controlled by adjusting the spray-chilling or spray-cooling conditions, in particular the flow rate of the solution through the spray-chilling or spray-cooling nozzle and the flow rate of the atomizing gas. Reference herein to the average particle size is to the average particle diameter.
In case the encapsulated fat-soluble vitamin manufactured is in the form of a powder, an anti-caking agent is optionally added to the powder formed in step b). Any suitable anti-caking agent may be used. Preferred anti-caking agents are silicon dioxide, tri calcium phosphate and magnesium aluminium silicate.
The encapsulated fat-soluble vitamin according to the invention is particularly suitable for use as ingredient in food products or in animal feed, in particular in animal feed. It has been found that the encapsulated vitamin can suitably be processed at a temperature in the order of 80-90 °C, a temperature commonly used in the manufacture of animal feed.
Examples
The invention will be further illustrated in a non-limiting way by the following examples.
EXAMPLE 1 (according to the invention)
An amount of 480 grams of fully hydrogenated rape seed oil (ex Unimills,
Zwijndrecht, The Netherlands) was melted by heating it to a temperature of 95 °C. To the molten hydrogenated rape seed oil was added 16.7 grams of a solution of vitamin D3 resin in soy bean oil comprising 15 MlU/g vitamin D3, and 3.8 grams of butyl hydroxy toluene. The mixture was homogenized in a laboratory homogenizer at 400 bar. The thus-obtained homogeneous solution of vitamin D3 in the molten fat phase was spray-chilled by pumping it (40 rpm, approximately 30 g/min) through heated tubing (95 °C) to a two-fluid nozzle (diameter 2.0 mm) and spraying it with nitrogen gas into liquid nitrogen to form particles with a particle size ranging from 100 to 650 μιη. By varying the pumping rate of the vitamin solution and the nitrogen pressure the particle size could be adjusted.
The homogeneity and the stability of the encapsulated vitamin was determined. For determining the homogeneity, five samples of 10 grams each were taken from the entire batch and analysed with respect to vitamin D3 content. The average vitamin D3 content appeared to be 0.507 million IU per gram with a standard deviation of 0.003 million IU per gram. After storage for three months at 40 °C and a relative humidity of 75%, the vitamin D3 content of samples appeared to be at the same level as just after manufacture. This shows that no oxidation or other degradation reaction had occurred. EXAMPLE 2 (according to the invention)
The experiment of EXAMPLE 1 was repeated, but now with palm stearin (Prifex 300, ex Unimills, Zwijndrecht, The Netherlands) instead of hydrogenated rape seed oil.
As in Example 1, the homogeneity and the stability of the encapsulated vitamin was determined. The average vitamin D3 content appeared to be 0.504 million IU per gram with a standard deviation of 0.003 million IU per gram. After storage for three months at 40 °C and a relative humidity of 75%, the vitamin D3 content of samples appeared to be at the same level as just after manufacture. This shows that no oxidation or other degradation reaction had occurred.
EXAMPLE 3 (according to the invention)
The experiment of EXAMPLE 1 was repeated, but now with carnauba wax (ex Paramelt, Alkmaar, The Netherlands) instead of hydrogenated rape seed oil.
After storage of the vitamin powder for three months and for six months at 40°C and 75% relative humidity, the vitamin D3 content of the samples was determined and appeared to be at the same level as just after manufacture. This shows that no oxidation or other degradation had occurred.
EXAMPLE 4 (according to the invention)
An amount of 1000 kg of fully hardened palm oil (UmFeed®131, ex Unimills, Zwijndrecht, The Netherlands) was melted and kept at 70°C (+/- 5°C). Then 183 kg of butyl hydroxy toluene (ex Merck, Darmstadt, Germany) was added to the molten phase and subsequently 750 kg of a warm solution (60°C) of 15 MlU/g vitamin D3 in soy bean oil. After homogenization, this mixture was added to 18375 kg of molten fully hardened palm oil (UmFeed®131, ex Unimills, Zwijndrecht, The Netherlands) and further homogenized at 70°C (+/- 5°C).
Subsequently the material was sprayed into a large scale spray chiller at a rate of 500 kg/h to form particles with an average particle size of 250 μιη. Samples were taken after each 500 kg of product. The average vitamin D3 content was 0.57 MlU/g for all samples with a standard deviation of 0.01 MlU/g.
Samples of the vitamin powder were stored at three different conditions: 25°C and 60% relative humidity; 30°C and 65% relative humidity; and 40°C and 75% relative humidity.
After storage of the vitamin powder samples for three months and for six months, the vitamin D3 content of the samples was determined and appeared to be at the same level as just after manufacture. This shows that no oxidation or other degradation had occurred.
Claims
1. A process for manufacturing an encapsulated fat-soluble vitamin comprising: (a) preparing a homogeneous solution of a fat-soluble vitamin in a molten fatty phase; and
(b) cooling the solution to solidify the fatty phase and form the encapsulated vitamin, wherein the fatty phase has a melting point in the range of from 45 to 90 °C.
2. A process according to claim 1, wherein the fat-soluble vitamin is vitamin D or one of its analogues.
3. A process according to claim 2, where in the fat-soluble vitamin is vitamin D3 or one of its analogues.
4. A process according to claim 3, where in the fat-soluble vitamin is 25-hydroxy- vitamin D3.
5. A process according to any one of claims 1 to 4, wherein the solution further comprises an anti-oxidant.
6. A process according to claim 5, wherein the anti-oxidant is selected from the group consisting of butyl hydroxyl toluene, tocopherol, etoxyquin.
7. A process according to any one of the preceding claims, wherein the solution is cooled in step (b) by spray-cooling or spray-chilling.
8. A process according to any one of the preceding claims, wherein in step (b) a powder of encapsulated vitamin is formed with an average particle size in the range of from 100 to 850 μιη.
9. A process according to claim 8, wherein the average particle size is in the range of from 100 to 300 μιη.
10. A process according to any one of the preceding claims, wherein the fatty phase has a melting point in the range of from 55 to 80 °C, preferably in the range of from 55 to 72 °C, more preferably of from 58 to 68 °C.
11. A process according the any one of the preceding claims, wherein the fatty phase is a hydrogenated vegetable oil or a food grade wax.
12. A process according to claim 11, wherein the fatty phase is a hydrogenated vegetable oil.
13. An encapsulated fat-soluble vitamin obtainable by a process according to any one of the preceding claims.
14. Use of the encapsulated fat-soluble vitamin according to claim 13 as ingredient in animal feed.
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