CN112107555A - Vitamin A acetate microcapsule and preparation method thereof - Google Patents
Vitamin A acetate microcapsule and preparation method thereof Download PDFInfo
- Publication number
- CN112107555A CN112107555A CN202010988872.9A CN202010988872A CN112107555A CN 112107555 A CN112107555 A CN 112107555A CN 202010988872 A CN202010988872 A CN 202010988872A CN 112107555 A CN112107555 A CN 112107555A
- Authority
- CN
- China
- Prior art keywords
- vitamin
- acetate
- emulsion
- gelatin
- microcapsule
- 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.)
- Granted
Links
- 239000003094 microcapsule Substances 0.000 title claims abstract description 96
- 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 title claims abstract description 92
- 229960000342 retinol acetate Drugs 0.000 title claims abstract description 90
- 235000019173 retinyl acetate Nutrition 0.000 title claims abstract description 90
- 239000011770 retinyl acetate Substances 0.000 title claims abstract description 90
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000002245 particle Substances 0.000 claims abstract description 122
- 239000000839 emulsion Substances 0.000 claims abstract description 102
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 56
- 108010010803 Gelatin Proteins 0.000 claims abstract description 45
- 229920000159 gelatin Polymers 0.000 claims abstract description 45
- 239000008273 gelatin Substances 0.000 claims abstract description 45
- 235000019322 gelatine Nutrition 0.000 claims abstract description 45
- 235000011852 gelatine desserts Nutrition 0.000 claims abstract description 45
- 238000004132 cross linking Methods 0.000 claims abstract description 42
- 229920002472 Starch Polymers 0.000 claims abstract description 40
- 239000008107 starch Substances 0.000 claims abstract description 40
- 235000019698 starch Nutrition 0.000 claims abstract description 40
- 238000001694 spray drying Methods 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 28
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 26
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 26
- 235000006708 antioxidants Nutrition 0.000 claims abstract description 26
- 238000010008 shearing Methods 0.000 claims abstract description 26
- 235000000346 sugar Nutrition 0.000 claims abstract description 21
- 238000002156 mixing Methods 0.000 claims abstract description 20
- 238000004945 emulsification Methods 0.000 claims abstract description 18
- 238000001914 filtration Methods 0.000 claims abstract description 17
- 229910052751 metal Inorganic materials 0.000 claims abstract description 16
- 239000002184 metal Substances 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 15
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract description 14
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 13
- 230000008569 process Effects 0.000 claims abstract description 13
- 239000002562 thickening agent Substances 0.000 claims abstract description 8
- 238000012216 screening Methods 0.000 claims abstract description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 32
- 239000003921 oil Substances 0.000 claims description 19
- 229910052757 nitrogen Inorganic materials 0.000 claims description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- 238000002844 melting Methods 0.000 claims description 12
- 230000008018 melting Effects 0.000 claims description 12
- 229930006000 Sucrose Natural products 0.000 claims description 11
- 230000001804 emulsifying effect Effects 0.000 claims description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 10
- 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 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000005720 sucrose Substances 0.000 claims description 10
- 239000011790 ferrous sulphate Substances 0.000 claims description 9
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 9
- 238000007710 freezing Methods 0.000 claims description 9
- 230000008014 freezing Effects 0.000 claims description 9
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 9
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 9
- 241000283690 Bos taurus Species 0.000 claims description 8
- 210000000988 bone and bone Anatomy 0.000 claims description 8
- 239000005543 nano-size silicon particle Substances 0.000 claims description 8
- AZJQQNWSSLCLJN-UHFFFAOYSA-N 2-ethoxyquinoline Chemical compound C1=CC=CC2=NC(OCC)=CC=C21 AZJQQNWSSLCLJN-UHFFFAOYSA-N 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 229920005610 lignin Polymers 0.000 claims description 7
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 6
- 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 claims description 5
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- CZBZUDVBLSSABA-UHFFFAOYSA-N butylated hydroxyanisole Chemical compound COC1=CC=C(O)C(C(C)(C)C)=C1.COC1=CC=C(O)C=C1C(C)(C)C CZBZUDVBLSSABA-UHFFFAOYSA-N 0.000 claims description 5
- 235000010354 butylated hydroxytoluene Nutrition 0.000 claims description 5
- 229910052791 calcium Inorganic materials 0.000 claims description 5
- 239000011575 calcium Substances 0.000 claims description 5
- 239000002131 composite material Substances 0.000 claims description 5
- 239000010949 copper Substances 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 5
- 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 5
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 229910052749 magnesium Inorganic materials 0.000 claims description 5
- 239000011777 magnesium Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims 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 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 229920001046 Nanocellulose Polymers 0.000 claims description 4
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L sulfate group Chemical group S(=O)(=O)([O-])[O-] QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 3
- 229930091371 Fructose Natural products 0.000 claims description 3
- 239000005715 Fructose Substances 0.000 claims description 3
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 claims description 3
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 3
- 239000001110 calcium chloride Substances 0.000 claims description 3
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 3
- ONCZQWJXONKSMM-UHFFFAOYSA-N dialuminum;disodium;oxygen(2-);silicon(4+);hydrate Chemical compound O.[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Na+].[Na+].[Al+3].[Al+3].[Si+4].[Si+4].[Si+4].[Si+4] ONCZQWJXONKSMM-UHFFFAOYSA-N 0.000 claims description 3
- 229960002089 ferrous chloride Drugs 0.000 claims description 3
- 239000008103 glucose Substances 0.000 claims description 3
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 3
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 3
- 239000011347 resin Substances 0.000 claims description 3
- 229920005989 resin Polymers 0.000 claims description 3
- 229940080314 sodium bentonite Drugs 0.000 claims description 3
- 229910000280 sodium bentonite Inorganic materials 0.000 claims description 3
- 229920005552 sodium lignosulfonate Polymers 0.000 claims description 3
- 229920001864 tannin Polymers 0.000 claims description 3
- 235000018553 tannin Nutrition 0.000 claims description 3
- 239000001648 tannin Substances 0.000 claims description 3
- 235000010384 tocopherol Nutrition 0.000 claims description 3
- 229930003799 tocopherol Natural products 0.000 claims description 3
- 229960001295 tocopherol Drugs 0.000 claims description 3
- 239000011732 tocopherol Substances 0.000 claims description 3
- 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 3
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 2
- OWEGMIWEEQEYGQ-UHFFFAOYSA-N 100676-05-9 Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC2C(OC(O)C(O)C2O)CO)O1 OWEGMIWEEQEYGQ-UHFFFAOYSA-N 0.000 claims description 2
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims description 2
- 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 claims description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 2
- 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 claims description 2
- 229920001732 Lignosulfonate Polymers 0.000 claims description 2
- GUBGYTABKSRVRQ-PICCSMPSSA-N Maltose Natural products O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@@H](CO)OC(O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-PICCSMPSSA-N 0.000 claims description 2
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 claims description 2
- WQZGKKKJIJFFOK-PHYPRBDBSA-N alpha-D-galactose Chemical compound OC[C@H]1O[C@H](O)[C@H](O)[C@@H](O)[C@H]1O WQZGKKKJIJFFOK-PHYPRBDBSA-N 0.000 claims description 2
- 239000000728 ammonium alginate Substances 0.000 claims description 2
- 235000010407 ammonium alginate Nutrition 0.000 claims description 2
- KPGABFJTMYCRHJ-YZOKENDUSA-N ammonium alginate Chemical compound [NH4+].[NH4+].O1[C@@H](C([O-])=O)[C@@H](OC)[C@H](O)[C@H](O)[C@@H]1O[C@@H]1[C@@H](C([O-])=O)O[C@@H](O)[C@@H](O)[C@H]1O KPGABFJTMYCRHJ-YZOKENDUSA-N 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 235000010323 ascorbic acid Nutrition 0.000 claims description 2
- 229960005070 ascorbic acid Drugs 0.000 claims description 2
- 239000011668 ascorbic acid Substances 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- GUBGYTABKSRVRQ-QUYVBRFLSA-N beta-maltose Chemical compound OC[C@H]1O[C@H](O[C@H]2[C@H](O)[C@@H](O)[C@H](O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@@H]1O GUBGYTABKSRVRQ-QUYVBRFLSA-N 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 2
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 2
- 229910021485 fumed silica Inorganic materials 0.000 claims description 2
- 229930182830 galactose Natural products 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 2
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 2
- 239000008101 lactose Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000000661 sodium alginate Substances 0.000 claims description 2
- 235000010413 sodium alginate Nutrition 0.000 claims description 2
- 229940005550 sodium alginate Drugs 0.000 claims description 2
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 claims description 2
- FPIPGXGPPPQFEQ-OVSJKPMPSA-N all-trans-retinol Chemical compound OC\C=C(/C)\C=C\C=C(/C)\C=C\C1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-OVSJKPMPSA-N 0.000 abstract description 52
- 229940045997 vitamin a Drugs 0.000 abstract description 50
- FPIPGXGPPPQFEQ-UHFFFAOYSA-N 13-cis retinol Natural products OCC=C(C)C=CC=C(C)C=CC1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-UHFFFAOYSA-N 0.000 abstract description 49
- FPIPGXGPPPQFEQ-BOOMUCAASA-N Vitamin A Natural products OC/C=C(/C)\C=C\C=C(\C)/C=C/C1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-BOOMUCAASA-N 0.000 abstract description 48
- 235000019155 vitamin A Nutrition 0.000 abstract description 48
- 239000011719 vitamin A Substances 0.000 abstract description 48
- 238000009826 distribution Methods 0.000 abstract description 31
- 230000000694 effects Effects 0.000 abstract description 10
- 238000003860 storage Methods 0.000 abstract description 5
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 42
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- 238000009835 boiling Methods 0.000 description 20
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- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
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- KCYQMQGPYWZZNJ-BQYQJAHWSA-N hydron;2-[(e)-oct-1-enyl]butanedioate Chemical compound CCCCCC\C=C\C(C(O)=O)CC(O)=O KCYQMQGPYWZZNJ-BQYQJAHWSA-N 0.000 description 1
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- 229960003471 retinol Drugs 0.000 description 1
- 235000020944 retinol Nutrition 0.000 description 1
- 239000011607 retinol Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 229940080313 sodium starch Drugs 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- KDYFGRWQOYBRFD-UHFFFAOYSA-L succinate(2-) Chemical compound [O-]C(=O)CCC([O-])=O KDYFGRWQOYBRFD-UHFFFAOYSA-L 0.000 description 1
- -1 sucrose fatty acid ester Chemical group 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000004614 tumor growth Effects 0.000 description 1
- 229940046009 vitamin E Drugs 0.000 description 1
- 235000019165 vitamin E Nutrition 0.000 description 1
- 239000011709 vitamin E Substances 0.000 description 1
- 208000005494 xerophthalmia Diseases 0.000 description 1
Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
- A61K9/5005—Wall or coating material
- A61K9/5021—Organic macromolecular compounds
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- A61K31/22—Esters, e.g. nitroglycerine, selenocyanates of carboxylic acids of acyclic acids, e.g. pravastatin
- A61K31/23—Esters, e.g. nitroglycerine, selenocyanates of carboxylic acids of acyclic acids, e.g. pravastatin of acids having a carboxyl group bound to a chain of seven or more carbon atoms
- A61K31/232—Esters, e.g. nitroglycerine, selenocyanates of carboxylic acids of acyclic acids, e.g. pravastatin of acids having a carboxyl group bound to a chain of seven or more carbon atoms having three or more double bonds, e.g. etretinate
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/11—Encapsulated compositions
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/64—Proteins; Peptides; Derivatives or degradation products thereof
- A61K8/65—Collagen; Gelatin; Keratin; Derivatives or degradation products thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/67—Vitamins
- A61K8/671—Vitamin A; Derivatives thereof, e.g. ester of vitamin A acid, ester of retinol, retinol, retinal
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
- A61K8/732—Starch; Amylose; Amylopectin; Derivatives thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
- A61K9/5005—Wall or coating material
- A61K9/5021—Organic macromolecular compounds
- A61K9/5052—Proteins, e.g. albumin
- A61K9/5057—Gelatin
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- A61K9/00—Medicinal preparations characterised by special physical form
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- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
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Abstract
The invention discloses a vitamin A acetate microcapsule and a preparation method thereof. The method comprises the following steps: uniformly mixing gelatin, sugar, an emulsifier, a thickener, metal inorganic salt and water, adding vitamin A acetate molten oil containing an antioxidant, performing high-speed shearing, high-pressure homogenizing emulsification and micron filtration to obtain emulsion, performing spray drying, and embedding emulsion droplets in starch to obtain microcapsule particles; and then drying, screening and crosslinking to obtain the vitamin A acetate microcapsule. The preparation method of the invention mainly aims at the preparation of the emulsion to be improved, so that the particle size distribution of the emulsion is more uniform, the embedding effect on the vitamin A is better, the loss rate of the vitamin A acetate is low in the spray drying process, the particle uniformity is good, the embedding effect is good, and the storage stability of the product is high; particularly, the metal inorganic salt added in the formula can promote the crosslinking, effectively reduce the crosslinking temperature and shorten the crosslinking time.
Description
Technical Field
The invention belongs to the technical field of vitamin A, and relates to a vitamin A acetate microcapsule and a preparation method thereof.
Background
Vitamin A (vitamin A), also known as retinol (its aldehyde derivative, retinal) or anti-xerophthalmia agent, is an unsaturated monohydric alcohol having an alicyclic ring. The vitamin A can enhance the sensitivity of human eyes to weak light, so that objects can be seen in a dark place with certain illumination; can maintain the health of epithelial tissue cells and promote the synthesis of immunoglobulin; promoting the biosynthesis of protein and the differentiation of osteocyte, and maintaining the normal growth and development of skeleton; the cell proliferation and growth are facilitated, and the growth and reproduction are promoted; and has the functions of delaying or preventing precancerous lesion, preventing chemical carcinogenic agent, inhibiting tumor growth and delaying senility; it can also be used as nutritional supplement, and can prevent pachylosis and promote normal growth, and can be used in cosmetics and health products.
Vitamin A is easily dissolved in organic solvents and fats, is insoluble in water, and is easily deteriorated by heat, light, acid and alkali, oxygen, heavy metals and the like. Therefore, in order to improve the storage stability and transportation requirements of vitamin A, microcapsule technology is adopted in the market, and vitamin A is embedded in colloid with relatively low chemical activity and high stability, so that the activity of the vitamin A is protected. The preparation method of the vitamin A microcapsule particle comprises the steps of firstly emulsifying the vitamin A oil, the emulsifier, water and other auxiliary agents into emulsion, and then carrying out spray drying and granulation to obtain the vitamin A microcapsule product.
Patent CN101214219 describes a process for preparing vitamin a, vitamin E microcapsules by emulsifying by high-speed shearing and high-pressure homogenization, followed by spray drying. Patent CN1965657 introduces a method for preparing a vitamin A microcapsule flour nutrition enhancer, which takes octenyl succinic acid powder as a wall material and vitamin A oil as a core material, and prepares microcapsules by spraying and drying after emulsification, wherein the average particle size of the prepared microcapsules is 85.6 microns. The two preparation methods are easy to cause the deterioration of the vitamin A due to the high emulsification temperature and the operation in an open environment; meanwhile, the emulsion system is unstable, so that the emulsion is easily layered in the spray drying process after emulsification is finished, and aggregated oil drops are easy to form large particles, thereby influencing the embedding effect and bioavailability of final products.
Patent CN104186976 reports a process for the preparation of vitamin a acetate microcapsules by mixing vitamin a with an antioxidant, emulsifying with an aqueous phase with sodium starch octenyl succinate and white sugar, and then preparing cold water dispersible vitamin a acetate microparticles by fluidized bed and starch mixing. The product obtained by the method has poor fluidity and large transportation difficulty, can be dispersed in cold water, and is easy to absorb moisture to cause dissolution and deterioration of vitamin A.
Patent CN102198116 describes a method for preparing vitamin A microcapsules by a spray drying granulation method, which is to mix and emulsify vitamin A acetate and starch neoalkenyl succinate and then prepare vitamin A acetate particles by a hot air spray drying technology.
Patent CN110250521 describes a method for preparing vitamin a acetate microcapsules, which comprises preparing vitamin a acetate, gelatin and sugar into uniform emulsion, and then spray-drying the emulsion by a pressure atomizer to obtain vitamin a acetate microcapsules capable of being stored for one year at normal temperature. However, the emulsion prepared by the method is not added with an emulsifier, so that the emulsion has large particle size, poor fluidity and high viscosity, a high-pressure metering pump is required when a pressure type atomizer is used, and the emulsion needs to be strictly filtered because the aperture of a nozzle is small, otherwise the nozzle is easily blocked, the nozzle is abraded greatly, and the method is not suitable for high-viscosity materials and large-scale production.
The methods have corresponding defects, the attention on emulsion preparation is low, the temperature required by crosslinking is too high, the loss of VA acetic ester in the crosslinking process is high, and a new preparation process needs to be found.
Disclosure of Invention
In view of the above problems in the prior art, the present invention aims to provide a novel vitamin a acetate microcapsule and a preparation method thereof. The preparation method of the invention is mainly improved aiming at the preparation of the emulsion, so that the particle size distribution of the emulsion is more uniform, the embedding effect on the vitamin A is better, the loss rate of the vitamin A acetate is low in the spray drying process, the particle uniformity is good, the embedding effect is good, and the storage stability of the product is high; particularly, the metal inorganic salt (sulfate or hydrochloride of iron/calcium/magnesium/copper) added in the formula can promote the crosslinking, effectively reduce the crosslinking temperature, shorten the crosslinking time, effectively reduce the loss of VA acetate in the crosslinking process, and simultaneously reduce the load and maintenance cost of spray drying equipment and crosslinking equipment.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a preparation method of vitamin A acetate microcapsules comprises the following steps:
(1) mixing vitamin A acetate with an antioxidant in an inert gas environment, and melting to obtain vitamin A acetate molten oil containing the antioxidant;
(2) uniformly mixing gelatin, sugar, an emulsifier, a thickener, metal inorganic salt and water, heating for dissolving, then shearing at a high speed, and removing oxygen in vacuum to obtain a composite aqueous solution containing the gelatin and the sugar;
(3) in an inert gas environment, adding the vitamin A acetate molten oil containing the antioxidant in the step (1) into the compound aqueous solution containing the gelatin and the sugar in the step (2), and then carrying out high-speed shearing, high-pressure homogenizing emulsification and micron filtration to obtain uniform and stable emulsion;
(4) spray drying the prepared emulsion by using a rotary atomizer, simultaneously adding starch, enabling the rotation direction of emulsion droplets to be opposite to the rotation direction of the starch in the spray drying process, controlling the centrifugal rotation speed, the feeding amount, the air inlet temperature and the starch flow rate, and embedding the emulsion droplets in the starch to obtain microcapsule particles;
(5) and (4) drying and screening the microcapsule particles obtained in the step (4), and then transferring the microcapsule particles into a fluidized bed dryer for crosslinking to obtain the vitamin A acetate microcapsule.
In the step (1) of the invention, the vitamin A acetate and the antioxidant are mixed according to a mass ratio of 100: 0.1-5, preferably 100: 1-5;
in step (1) of the present invention, the antioxidant is selected from one or more of EMQ (ethoxyquinoline), BHA (butylhydroxyanisole), BHT (2, 6-di-tert-butyl-4-methylphenol), tocopherol, ascorbic acid, preferably EMQ;
in step (1) of the present invention, the inert gas is selected from one or more of nitrogen, helium and argon, and is preferably nitrogen.
In the step (1), the melting temperature is 55-75 ℃, and preferably 60-70 ℃; the melting time is 20-120 min, preferably 30-60 min.
In the step (2), the gelatin is selected from one or more of pigskin gelatin, pig bone gelatin, cow skin gelatin and cow bone gelatin, and preferably is cow bone gelatin; the isoelectric point of the gelatin is 3.5-6.5, preferably 4.5-5.5; the freezing strength of the gelatin is 20-180 bloom, and preferably 20-60 bloom.
In step (2) of the present invention, the sugar is selected from one or more of glucose, fructose, sucrose, lactose, maltose and galactose, and is preferably sucrose.
In step (2) of the present invention, the metal inorganic salt is selected from one or more of sulfate or hydrochloride of metal, and the metal is selected from iron, calcium, magnesium, copper;
preferably, the metal inorganic salt is one or more of ferrous sulfate, ferric sulfate, calcium sulfate, ferric chloride, ferrous chloride, calcium chloride, magnesium chloride and copper sulfate, and is more preferably ferrous sulfate.
In the step (2), the emulsifier is selected from one or more of lignosulfonate, nano-silicon dioxide, nano-aluminum oxide, nano-talcum powder, nano-cellulose, ammonium alginate, sodium alginate and the like, and is preferably nano-cellulose and/or nano-silicon dioxide;
the thickener is selected from one or more of fumed silica, sodium bentonite, sodium lignosulfonate, lignin, tannin resin, rosin and the like, and is preferably lignin.
In the step (2), the mass ratio of the water, the gelatin, the sugar, the emulsifier, the thickener and the metal inorganic salt is 1: 0.3-0.5: 0.15-0.45: 0.01-0.05: 0.005-0.02: 0.005-0.02, preferably 1: 0.3-0.4: 0.2-0.4: 0.02-0.04: 0.01-0.02: 0.01 to 0.02.
In the step (2), the heating and dissolving are carried out at the temperature of 55-75 ℃, and preferably at the temperature of 60-70 ℃; the time is 20-120 min, preferably 20-60 min.
In the step (2), the high-speed shearing is carried out at a rotating speed of 5000-15000 rpm, preferably 6000-8000 rpm; the time is 5-60 min, preferably 10-15 min.
In the step (2) of the invention, the vacuum oxygen removal pressure is-0.05 to-0.1 Mpa, preferably-0.07 to-0.08 Mpa; the time is 0.5 to 3 hours, preferably 1 to 2 hours.
In the step (3), the mass ratio of the antioxidant-containing vitamin A acetate molten oil to the gelatin-sugar-containing composite aqueous solution is 1: 3-10, and preferably 1: 3.5-6.
In the step (3), the high-speed shearing is carried out at a speed of 6000-20000 rpm, preferably 8000-15000 rpm; the time is 5 to 50min, preferably 10 to 30 min.
In the step (3), the high-pressure homogenizing and emulsifying is carried out, wherein the pressure is 20-60 MpaG, and preferably 30-50 MpaG; the number of times is 2-6, preferably 2-3, and the number of times refers to the number of times of passing through the high-pressure homogenizer cavity.
In the step (3), the micron filtration is carried out, and the filtration precision is 0.5-5 μm, preferably 0.5-2.5 μm; the micron filtration operation means that the prepared emulsion is filtered by a micron filter bag, so that large-particle emulsion which cannot pass through the micron filter bag is removed, a proper particle size range is obtained, and the particle embedding rate is improved; the average particle size of the emulsion passing through the micron filter bag is 0.2-2.0 μm, and preferably 0.2-1.0 μm.
In step (4) of the present invention, the rotary atomizer is selected from a smooth disc atomizer, a wheel atomizer, a rotary-airflow cup atomizer, preferably a wheel atomizer; the emulsion enters a rotary atomizer, rotary liquid drops are formed through the centrifugal action of the atomizer, meanwhile, starch enters from a side pipe beside the rotary atomizer through the wind power action, and the entering direction is opposite to the rotating direction of the rotary atomizer;
the centrifugal rotating speed of the rotary atomizer is 4000-12000 rpm, and preferably 4000-6000 rpm.
In the step (4), the feeding mass ratio of the emulsion to the starch in the rotary atomizer is 1: 1-8, preferably 1: 2-3; the starch flow is 3-12 kg/h (50-200 g/min), preferably 3.5-5 kg/h; the air inlet temperature is 20-70 ℃, and preferably 30-50 ℃.
In the step (5), the drying temperature is 80-130 ℃, and preferably 80-105 ℃; drying until the water content is 2-10 wt%, preferably 5-7 wt%. The drying is preferably carried out by a boiling fluidized bed dryer, and hot air can be used for heat exchange to avoid particle accumulation and local overheating.
In the step (5), the particle size range of the sieved particles is 180-400 μm, preferably 210-350 μm.
In the step (5), the crosslinking is carried out at the temperature of 60-130 ℃, preferably 80-90 ℃; the time is 10 to 240min, preferably 30 to 60 min.
According to the preparation method of the vitamin A acetate microcapsule, the embedding rate of the vitamin A acetate microcapsule is more than 95%, and preferably, the embedding rate is more than 97%; the loss of vitamin a acetate is less than 5%, preferably less than 3%.
The invention also provides a vitamin A acetate microcapsule prepared by the method, wherein the particle size of the vitamin A acetate microcapsule is 180-400 mu m, preferably 210-350 mu m, and the moisture content is 0.5-1.5 wt%. The microcapsule can be stably stored for 1-1.5 years at room temperature, and the loss rate of the vitamin A acetate is lower than 3%.
The technical scheme of the invention has the beneficial effects that:
according to the invention, metal inorganic salt (sulfate or hydrochloride of iron/calcium/magnesium/copper) is added into a raw material system containing gelatin and sugar to promote the progress of a crosslinking reaction, and iron, calcium, magnesium and copper metal ions provided by the inorganic salt can promote the amino group of protein and the carbonyl group of reducing sugar through forming a complex, so that the progress of the crosslinking reaction is promoted, the time required by the crosslinking reaction is effectively reduced, the crosslinking temperature is reduced, the decomposition and deterioration of heat-sensitive components such as gelatin and sugar and the loss of vitamin A acetate in a long-time high-temperature process are avoided, and meanwhile, the load and the maintenance cost of crosslinking equipment can be reduced.
According to the invention, the emulsifier and the thickener are added in the preparation stage of the emulsion, so that the emulsion has better dispersibility and stability, and particularly, when the nano-cellulose and the nano-silicon dioxide are added as the emulsifier, the interface tension of an oil-water two-phase interface can be reduced through the adsorption effect of the nano-particles on the oil-water two-phase interface, and the stability of the emulsion is obviously enhanced. The particle size of the emulsion is further reduced by the cooperation of the high-pressure homogenization effect, the particle size distribution of the emulsion is more uniform by micron filtration, the vitamin A acetate can be more uniformly coated on the wall materials such as gelatin, sugar and the like in the liquid drops, the stability of the emulsion is further improved, the loss rate of the vitamin A acetate in the spray granulation process is reduced, the uniformity of the obtained microcapsule particles is good, the embedding effect is good, and the storage stability of the product is high.
Detailed Description
The following detailed description of embodiments of the invention is intended to be illustrative of the invention and is not to be construed as limiting the invention. The examples do not specify particular techniques or conditions, and are performed according to the techniques or conditions described in the literature in the art or according to the product specifications.
< raw Material information >
EMQ (ethoxyquinoline): michelin reagent Ltd
Gelatin: luosilou Co Ltd
Nano silicon dioxide: particle size of 5-10 μm, Dojindo chemical Co., Ltd
Other raw materials are all common commercial products and the reagents are all analytically pure, unless otherwise specified.
< analytical test method >
Vitamin A microcapsule unit is detected according to the national standard GB/T7292-;
the particle size testing instrument is a Dandong Baite laser dynamics instrument Bettersize 2600E;
the moisture test adopts a WKT-A8 Karl Fischer moisture tester;
the embedding rate test method comprises the following steps:
loss rate test method:
example 1
(1) Weighing 42.8g of vitamin A acetate crystal and 2g of EMQ (ethoxyquinoline) in a nitrogen environment, uniformly mixing, and melting at 60 ℃ for 60min to obtain antioxidant-containing vitamin A acetate molten oil;
(2) weighing 35g of gelatin (bovine bone gelatin, freezing power: 60bloom, isoelectric point of 4.5), 30g of sucrose, 3g of nano-silica, 1.5g of lignin and 1.2g of ferrous sulfate, uniformly mixing the gelatin (bovine bone gelatin, freezing power: 60bloom, isoelectric point of 4.5) with 100g of deionized water, heating and dissolving at 60 ℃ for 60min, then shearing at a high speed of 6000rpm for 15min by using a high-speed shearing machine to obtain a uniformly mixed water phase, and deoxidizing for 1.5h under the vacuum condition of-0.07 MPa to obtain a composite water solution containing the gelatin and sugar;
(3) adding vitamin A acetate molten oil containing antioxidant into complex water solution containing gelatin and sugar in nitrogen environment, continuing shearing at 8000rpm for 30min, homogenizing and emulsifying for 3 times with high pressure homogenizer with homogenization pressure of 30MpaG, and filtering with 1.0 μm precision micrometer filter bag to obtain uniform and stable emulsion; the average grain diameter of the emulsion after high-pressure homogenizing emulsification is 0.9 mu m, the grain diameter distribution coefficient PDI is 2.314, after passing through a 1.0 mu m precision micron filter bag, the average grain diameter of the emulsion is 0.8 mu m, the grain diameter distribution coefficient PDI is 1.915, and the average grain diameter of the emulsion is unchanged after standing and storing for 30 min;
(4) carrying out spray drying on the prepared emulsion by using a wheel type atomizer, enabling the emulsion to enter the rotary atomizer, forming rotary liquid drops through the centrifugal action of the atomizer, and enabling starch to enter from a side pipe beside the rotary atomizer through the wind power action, wherein the entering direction is opposite to the rotating direction of the rotary atomizer; the rotation speed of an atomizer is 4000rpm, the feeding speed is 20g/min, the air inlet temperature is 30 ℃ and the starch flow is 60g/min, and emulsion droplets are embedded in starch to obtain microcapsule particles;
(5) and (3) starting a fluidized bed dryer, setting the drying temperature to be 90 ℃ until the moisture content of the microcapsule particles is reduced to 6 +/-1 wt%, sieving the crude product by using 30-mesh and 100-mesh sieves respectively, removing large particles which cannot pass through the 30-mesh sieve and starch particles which can pass through the 100-mesh sieve, and crosslinking the crude product on a boiling fluidized bed at the crosslinking temperature of 90 ℃ for 30min to obtain the vitamin A acetate microcapsule.
The loss rate of vitamin A acetate in the spray drying stage is 2.8%, the embedding rate of vitamin A acetate microcapsules is 97.6%, and the microcapsule particles are insoluble in boiling water within 15 min.
The vitamin A acetate unit in the microcapsule is 104.4 ten thousand IU/g, the water content is 1.2 wt%, and the particle size range is 160-200 mu m. After being placed at normal temperature for one year, the content of the vitamin A acetic ester is detected to be reduced to 103.6 ten thousand IU/g.
Example 2
(1) Weighing 20.5g of vitamin A acetate and 1.0g of EMQ (ethoxyquinoline) in a nitrogen environment, uniformly mixing, and melting at 60 ℃ for 60min to obtain antioxidant-containing vitamin A acetate molten oil;
(2) weighing 40g of gelatin (freezing force: 50bloom, isoelectric point of 5.5), 35g of sucrose, 4g of nanocellulose, 2g of lignin and 1.5g of ferrous chloride, uniformly mixing with 100g of deionized water, heating and dissolving at 60 ℃, wherein the dissolving time is 60min, then shearing at high speed of 6000rpm for 15min by using a high-speed shearing machine to obtain a uniformly mixed water phase, and deoxidizing for 1.5h under the vacuum condition of-0.07 MPaG to obtain a composite aqueous solution containing gelatin and sugar;
(3) adding vitamin A acetate molten oil containing antioxidant into complex water solution containing gelatin and sugar in nitrogen environment, continuing shearing at 8000rpm for 30min, homogenizing and emulsifying for 2 times with high pressure homogenizer with homogenization pressure of 50MpaG, and filtering with 1.2 μm precision micrometer filter bag to obtain uniform and stable emulsion; the average grain diameter of the emulsion after high-pressure homogenizing emulsification is 1.0 mu m, the grain diameter distribution coefficient PDI is 2.564, after passing through a 1.2 mu m precision micron filter bag, the average grain diameter of the emulsion is 0.9 mu m, the grain diameter distribution coefficient PDI is 1.865, and the emulsion is kept stand and stored for 45min without changing the average grain diameter;
(4) carrying out spray drying on the prepared emulsion by using a wheel type atomizer, enabling the emulsion to enter the rotary atomizer, forming rotary liquid drops through the centrifugal action of the atomizer, and enabling starch to enter from a side pipe beside the rotary atomizer through the wind power action, wherein the entering direction is opposite to the rotating direction of the rotary atomizer; the rotational speed of the atomizer is 6000rpm, the feeding speed is 45g/min, the air inlet temperature is 50 ℃ and the starch flow is 120g/min, and emulsion droplets are embedded in the starch to obtain microcapsule particles;
(5) starting a fluidized bed dryer, setting the drying temperature to be 100 ℃, until the moisture content of the microcapsule particles is reduced to 6 +/-1 wt%, respectively screening the crude product by using 40-mesh and 100-mesh screens, removing large particles which cannot pass through the 40-mesh screen and starch particles which can pass through the 100-mesh screen, and crosslinking the crude product on a boiling fluidized bed, wherein the crosslinking temperature is 85 ℃, and the crosslinking time is 45min, so as to obtain the vitamin A acetate microcapsule.
The loss rate of vitamin A acetate in spray drying stage is 2.9%, the embedding rate of vitamin A acetate microcapsule is 98.2%, and microcapsule granule is insoluble in boiling water within 22 min.
The vitamin A acetate unit in the microcapsule is 55.5 ten thousand IU/g, the water content is 0.8 wt%, and the particle size range is 150-180 mu m. After being placed at normal temperature for one year, the content of the vitamin A acetic ester is detected to be reduced to 53.6 ten thousand IU/g.
Example 3
(1) Weighing 40g of vitamin A acetate crystal and 1.5g of EMQ (ethoxyquinoline) in a nitrogen environment, uniformly mixing, and melting at 70 ℃ for 30min to obtain antioxidant-containing vitamin A acetate molten oil;
(2) weighing 55g of gelatin (freezing force: 50bloom, isoelectric point of 3.5), 45g of glucose, 5g of nano silicon dioxide, 2g of sodium bentonite, 1.6g of copper chloride and 150g of deionized water, uniformly mixing, heating and dissolving at 65 ℃ for 50min, then shearing at high speed of 5000rpm for 20min by using a high-speed shearing machine to obtain a uniformly mixed water phase, and deoxidizing for 1h under the vacuum condition of-0.08 MPa;
(3) adding vitamin A acetate molten oil containing antioxidant into the prepared gelatin-sugar-water solution in nitrogen environment, continuing to shear at high speed of 12000rpm for 20min, homogenizing and emulsifying for 3 times with a high-pressure homogenizer at homogenizing pressure of 40Mpa, and filtering with 1.5 μm precision micrometer filter bag to obtain uniform and stable emulsion; the average grain diameter of the emulsion after high-pressure homogenizing emulsification is 1.4 mu m, the grain diameter distribution coefficient PDI is 3.265, after passing through a 1.5 mu m precision micron filter bag, the average grain diameter of the emulsion is 1.2 mu m, the grain diameter distribution coefficient PDI is 2.132, and the emulsion is kept still for storage within 25min and is unchanged;
(4) carrying out spray drying on the prepared emulsion by using a wheel type atomizer, wherein the rotating speed of the atomizer is 5000rpm, the feeding speed is 30g/min, the air inlet temperature is 40 ℃, the starch flow is 210g/min, and the rotating direction of liquid drops in the spray dryer is opposite to the rotating direction of starch, so that the starch effectively embeds the liquid drops;
(5) and (3) starting a fluidized bed dryer, setting the drying temperature to be 105 ℃, until the moisture content of the microcapsule particles is reduced to 6 +/-1 w%, sieving the crude product by using 30-mesh and 100-mesh sieves respectively, removing large particles which cannot pass through the 30-mesh sieve and starch particles which can pass through the 100-mesh sieve, and crosslinking the crude product on a boiling fluidized bed at the crosslinking temperature of 85 ℃ for 50min to obtain the vitamin A acetate microcapsule particles.
The loss rate of vitamin A acetate in the spray drying stage is 2.8%, the embedding rate of vitamin A acetate microcapsules is 98.6%, and the microcapsule particles are insoluble in boiling water within 25 min.
The vitamin A microcapsule unit detected according to the national standard GB/T7292-. After being placed at normal temperature for one year, the content of the vitamin A acetic ester is detected to be reduced to 73.2 ten thousand IU/g.
Example 4
(1) Weighing 40g of vitamin A acetate crystals and 1.5g of tocopherol in a nitrogen environment, uniformly mixing, and melting at 70 ℃ for 30min to obtain vitamin A acetate molten oil containing an antioxidant;
(2) weighing 35g of gelatin (freezing force: 20bloom, isoelectric point of 6), 25g of fructose, 5g of nano talcum powder, 2g of sodium lignosulfonate and 1.5g of calcium chloride, uniformly mixing with 100g of deionized water, heating and dissolving at 65 ℃ for 50min, then shearing at high speed of 6000rpm for 15min by using a high-speed shearing machine to obtain a uniformly mixed water phase, and deoxidizing for 2h under the vacuum condition of-0.07 MPaG;
(3) adding vitamin A acetate molten oil containing antioxidant into the prepared gelatin-sugar-water solution in nitrogen environment, continuously shearing at high speed of 15000rpm for 10min, homogenizing and emulsifying for 3 times with a high pressure homogenizer at 50Mpa, and filtering with 1.0 μm precision micrometer filter bag to obtain uniform and stable emulsion; the average grain diameter of the emulsion after high-pressure homogenizing emulsification is 0.8 mu m, the grain diameter distribution coefficient PDI is 2.132, after passing through a 1.0 mu m micron filter bag, the average grain diameter of the emulsion is 0.7 mu m, the grain diameter distribution coefficient PDI is 1.535, and the average grain diameter of the emulsion is not changed after standing and storing within 50 min;
(4) carrying out spray drying on the prepared emulsion by using a wheel type atomizer, wherein the rotating speed of the atomizer is 5000rpm, the feeding speed is 25g/min, the air inlet temperature is 40 ℃, the starch flow is 60g/min, and the rotating direction of liquid drops in the spray dryer is opposite to the rotating direction of starch, so that the starch effectively embeds the liquid drops;
(5) and (3) starting a fluidized bed dryer, setting the drying temperature to be 95 ℃ until the moisture content of the microcapsule particles is reduced to 6 +/-1 w%, sieving the crude product by using 30-mesh and 100-mesh sieves respectively, removing large particles which cannot pass through the 30-mesh sieve and starch particles which can pass through the 100-mesh sieve, and crosslinking the crude product on a boiling fluidized bed at the crosslinking temperature of 85 ℃ for 35min to obtain the vitamin A acetate microcapsule particles.
The loss rate of vitamin A acetate in the spray drying stage is 2.6%, the embedding rate of vitamin A acetate microcapsules is 99.5%, and the microcapsule particles are insoluble in boiling water within 18 min.
The vitamin A microcapsule unit detected according to the national standard GB/T7292-. After being placed at normal temperature for one year, the content of the vitamin A acetic ester is detected to be reduced to 100.5 ten thousand IU/g.
Example 5
(1) Weighing 55g of vitamin A acetate crystal and 2g of BHT (2, 6-di-tert-butyl-4-methylphenol) in a nitrogen environment, uniformly mixing the crystals together, and melting the mixture at 65 ℃ for 40min to obtain vitamin A acetate molten oil containing an antioxidant;
(2) weighing 100g of gelatin (freezing force: 60bloom, isoelectric point of 4.5), 70g of sucrose, 10g of nano-alumina, 4g of tannin resin and 5g of magnesium chloride, uniformly mixing with 250g of deionized water, heating and dissolving at 70 ℃ for 50min, then shearing at a high speed of 8000rpm for 20min by using a high-speed shearing machine to obtain a uniformly mixed water phase, and deoxidizing for 2h under the vacuum condition of-0.08 MPa;
(3) adding vitamin A acetate molten oil containing antioxidant into the prepared gelatin-sugar-water solution in nitrogen environment, continuing to shear at high speed of 12000rpm for 20min, homogenizing and emulsifying for 3 times with a high-pressure homogenizer at homogenizing pressure of 35Mpa, and filtering with 1.2 μm precision micrometer filter bag to obtain uniform and stable emulsion; the average particle size of the emulsion after high-pressure homogeneous emulsification is 1.0 mu m, the particle size distribution coefficient PDI is 2.896, after passing through a 1.2 mu m micron filter bag, the average particle size of the emulsion is 0.8 mu m, the particle size distribution coefficient PDI is 1.473, and the emulsion is kept stand for 35min without changing the average particle size;
(4) carrying out spray drying on the prepared emulsion by using a wheel type atomizer, wherein the rotating speed of the atomizer is 6000rpm, the feeding speed is 50g/min, the air inlet temperature is 50 ℃, the starch flow is 165g/min, and the rotating direction of liquid drops in the spray dryer is opposite to the rotating direction of starch, so that the starch effectively embeds the liquid drops;
(5) starting a fluidized bed dryer, setting the drying temperature to be 100 ℃, until the moisture content of the microcapsule particles is reduced to 6 +/-1 w%, respectively screening the crude product by using 30-mesh and 100-mesh screens, removing large particles which cannot pass through the 30-mesh screen and starch particles which can pass through the 100-mesh screen, and crosslinking the crude product on a boiling fluidized bed, wherein the crosslinking temperature is 115 ℃, and the crosslinking time is 20min, so as to obtain the vitamin A acetate microcapsule particles.
The loss rate of vitamin A acetate in spray drying stage is 3.0%, the embedding rate of vitamin A acetate microcapsule is 97.6%, and microcapsule granule is insoluble in boiling water within 25 min.
The vitamin A microcapsule unit detected according to the national standard GB/T7292-. After being placed at normal temperature for one year, the content of the vitamin A acetic ester is detected to be reduced to 60.5 ten thousand IU/g.
Example 6
(1) Weighing 50g of vitamin A acetate crystals and 2.2g of BHA (butylated hydroxyanisole) in a nitrogen environment, uniformly mixing, and melting at 70 ℃ for 40min to obtain antioxidant-containing vitamin A acetate molten oil;
(2) weighing 40g of gelatin (with freezing power of 40bloom and isoelectric point of 5.5), 32g of sucrose, 4g of nanocellulose, 1.2g of lignin and 3g of ferrous sulfate, uniformly mixing the gelatin, the sucrose and the deionized water with 100g of deionized water, heating and dissolving at 65 ℃ for 40min, then shearing at 7000rpm for 20min by using a high-speed shearing machine to obtain a uniformly mixed water phase, and deoxidizing for 1.5h under the vacuum condition of-0.08 MPa;
(3) adding vitamin A acetate molten oil containing antioxidant into the prepared gelatin-sugar-water solution in nitrogen environment, continuing to shear at high speed of 10000rpm for 20min, homogenizing and emulsifying for 3 times by using a high-pressure homogenizer with the homogenizing pressure of 45MpaG, and filtering by a 0.5-micrometer precision micrometer filter bag to obtain uniform and stable emulsion; the average grain diameter of the emulsion after high-pressure homogenizing emulsification is 0.9 mu m, the grain diameter distribution coefficient PDI is 1.832, after passing through a 1.0 mu m micron filter bag, the average grain diameter of the emulsion is 0.83 mu m, the grain diameter distribution coefficient PDI is 1.135, and the emulsion is kept still for 50min without changing the average grain diameter;
(4) carrying out spray drying on the prepared emulsion by using a wheel type atomizer, wherein the rotating speed of the atomizer is 5000rpm, the feeding speed is 35g/min, the air inlet temperature is 45 ℃, the starch flow is 40g/min, and the rotating direction of liquid drops in the spray dryer is opposite to the rotating direction of starch, so that the starch effectively embeds the liquid drops;
(5) starting a fluidized bed dryer, setting the drying temperature to be 80 ℃ until the moisture content of the microcapsule particles is reduced to 6 +/-1 wt%, sieving the crude product by using 30-mesh and 120-mesh sieves respectively, removing large particles which cannot pass through the 30-mesh sieve and starch particles which can pass through the 120-mesh sieve, and crosslinking the crude product on a boiling fluidized bed at the crosslinking temperature of 90 ℃ for 70min to obtain the vitamin A acetate microcapsule particles.
The loss rate of vitamin A acetate in the spray drying stage is 2.8%, the embedding rate of vitamin A acetate microcapsules is 98.3%, and the microcapsule particles are insoluble in boiling water within 24 min.
The vitamin A microcapsule unit detected according to the national standard GB/T7292-. After being placed at normal temperature for one year, the content of the vitamin A acetic ester is detected to be reduced to 104.6 ten thousand IU/g.
Example 7
The experimental procedure was as in example 1, except that in step (2) the ferrous sulfate was replaced with a homogenous mass of sodium chloride.
The average grain diameter of the emulsion after the high-pressure homogenizing emulsification in the step (3) is 1.16 mu m, the grain diameter distribution coefficient PDI is 2.315, after the emulsion passes through a 1.0-micron filter bag, the average grain diameter of the emulsion is 0.84 mu m, the grain diameter distribution coefficient PDI is 1.562, and the emulsion is kept still for 30min and is unchanged;
in the step (5), the temperature required by crosslinking is 105 ℃, and the crosslinking time is 4.5h, so that the vitamin A acetate microcapsule particles are obtained.
In the spray drying stage, the loss rate of vitamin A acetate is 3.8%, the embedding rate of vitamin A microcapsules is 95.1%, and the microcapsule particles are insoluble in boiling water within 10 min.
The vitamin A unit in the microcapsule is 103.4 ten thousand IU/g, the water content is 0.6 percent, and the particle size range of the particles is 140-180 mu m. After being placed at normal temperature for one year, the content of the vitamin A acetic ester is detected to be reduced to 97.8 ten thousand IU/g.
Example 8
The experimental procedure was as in example 1, except that the emulsifier nanosilicon dioxide was replaced with sucrose fatty acid ester of the same mass in step (2).
The average particle size of the emulsion after high-pressure homogenizing emulsification in the step (3) is 1.17 mu m, the particle size distribution coefficient PDI is 2.862, and after passing through a 1.0-micron filter bag, the average particle size of the emulsion is 0.86 mu m, and the particle size distribution coefficient PDI is 1.642; after the emulsion is kept stand for 30min, the average particle size of the emulsion is increased to 0.92 mu m, and the particle size distribution coefficient PDI is 1.925;
in the step (5), the temperature required by crosslinking is 85 ℃, and the crosslinking time is 2 hours, so that the vitamin A acetate microcapsule particles are obtained.
In the spray drying stage, the loss rate of vitamin A acetate is 3.6%, the embedding rate of vitamin A microcapsules is 97.8%, and the microcapsule particles are insoluble in boiling water within 15 min.
The vitamin A unit in the microcapsule is 103.6 ten thousand IU/g, the water content is 1.1 wt%, and the particle size range is 140-170 mu m. After being placed at normal temperature for one year, the content of the vitamin A acetic ester is detected to be reduced to 101.9 ten thousand IU/g.
Comparative example 1
The experimental procedure was as in example 1 except that no metallic inorganic salt (ferrous sulfate) was used in step (2).
And (3) after the high-pressure homogenizing emulsification in the step (3), the average particle size of the emulsion is 1.15 microns, the particle size distribution coefficient PDI is 2.963, after the emulsion passes through a 1.2-micron filter bag, the average particle size of the emulsion is 0.94 microns, the particle size distribution coefficient PDI is 1.632, and the emulsion is kept standing for 30min without changing the average particle size of the emulsion.
In the step (5), the temperature required by crosslinking is 120 ℃, and the crosslinking time is 3.5h, so that the vitamin A acetate microcapsule particles are obtained.
In the spray drying stage, the loss rate of vitamin A acetate is 4.9%, the embedding rate of vitamin A microcapsules is 96.1%, and the microcapsule particles are insoluble in boiling water within 10 min.
The vitamin A unit in the microcapsule is 103.3 ten thousand IU/g, the water content is 0.5 wt%, and the particle size range of the particles is 150-200 mu m. After being placed at normal temperature for one year, the content of the vitamin A acetic ester is detected to be reduced to 98.5 ten thousand IU/g.
Comparative example 2
The experimental procedure was as in example 1, except that in step (2) the ferrous sulfate was replaced with a homogeneous mass of sodium sulfonate.
And (3) after the high-pressure homogenizing emulsification in the step (3), the average particle size of the emulsion is 1.15 mu m, the particle size distribution coefficient PDI is 2.865, after the emulsion passes through a 1.2-micron filter bag, the average particle size of the emulsion is 0.94 mu m, the particle size distribution coefficient PDI is 1.598, and the emulsion is kept stand for 40min without changing the average particle size.
In the step (5), the temperature required by crosslinking is 125 ℃, and the crosslinking time is 2.5h, so that the vitamin A acetate microcapsule particles are obtained.
In the spray drying stage, the loss rate of vitamin A acetate is 4.6%, the embedding rate of vitamin A microcapsules is 96.7%, and the microcapsule particles are insoluble in boiling water within 8 min.
The vitamin A unit in the microcapsule is 102.5 ten thousand IU/g, the water content is 0.45 wt%, and the particle size range is 140-200 mu m. After being placed at normal temperature for one year, the content of the vitamin A acetic ester is detected to be reduced to 96.1 ten thousand IU/g.
Comparative example 3
The experimental procedure was as in example 1, except that no emulsifier nanosilica was used in step (2).
The average particle size of the emulsion after the high-pressure homogenizing emulsification in the step (3) is 2.1 mu m, the particle size distribution coefficient of the emulsion is 5.623, the average particle size of the emulsion is 1.9 mu m after the emulsion passes through a 2.5-micron filter bag, the particle size distribution coefficient of the emulsion is 3.256, the average particle size of the emulsion is 2.0 mu m after the emulsion is placed for 20min, and the particle size distribution coefficient PDI is 3.565.
In the spray drying stage, the loss rate of vitamin A acetate is 7.6%, the embedding rate of vitamin A microcapsules is 95.6%, and the microcapsule particles are insoluble in boiling water within 10 min.
The vitamin A unit in the microcapsule is 99.3 ten thousand IU/g, the water content is 1.8 wt%, and the particle size range of the particles is 150-180 mu m. After being placed at normal temperature for one year, the content of the vitamin A acetic ester is detected to be reduced to 93.2 ten thousand IU/g.
Comparative example 4
The experimental procedure was as in example 1, except that the high-pressure homogenization operation was omitted in step (3).
The average particle size of the solution after high-speed shearing in the step (3) is 2.3 microns, the particle size distribution coefficient of the emulsion is 6.756, after the solution passes through a micron filter bag (the filtering precision of the micron filter bag is 2.5 microns), the average particle size of the emulsion is 1.8 microns, the particle size distribution coefficient of the emulsion is 4.632, after the emulsion is kept still for 30min, the particle size of the emulsion is 1.95 microns, and the particle size distribution coefficient PDI is 5.065.
In the spray drying stage, the loss rate of vitamin A acetate is 8.4%, the embedding rate of vitamin A microcapsules is 93.8%, and the microcapsule particles are insoluble in boiling water within 5 min.
The vitamin A unit in the microcapsule is 98.4 ten thousand IU/g, the water content is 1.1 wt%, and the particle size range of the particles is 120-220 mu m. After being placed at normal temperature for one year, the content of the vitamin A acetic ester is detected to be reduced to 92.1 ten thousand IU/g.
Comparative example 5
The experimental procedure was as in example 1 except that the microfiltration process was omitted in step (3).
The average particle size of the emulsion after high-pressure homogenizing emulsification in the step (3) is 1.2 mu m, the particle size distribution coefficient is 2.315, and the emulsion is kept stand for 30min without obvious change of the average particle size of the emulsion;
in the spray drying stage, the loss rate of vitamin A acetate is 4.8%, the embedding rate of vitamin A microcapsules is 96.6%, and the microcapsule particles are insoluble in boiling water within 12 min.
The vitamin A unit in the microcapsule is 102.3 ten thousand IU/g, the water content is 1.7 wt%, and the particle size range of the particles is 150-200 mu m. After being placed at normal temperature for one year, the content of the vitamin A acetic ester is detected to be reduced to 98.5 ten thousand IU/g.
Claims (9)
1. A preparation method of vitamin A acetate microcapsules is characterized by comprising the following steps:
(1) mixing vitamin A acetate with an antioxidant in an inert gas environment, and melting to obtain vitamin A acetate molten oil containing the antioxidant;
(2) uniformly mixing gelatin, sugar, an emulsifier, a thickener, metal inorganic salt and water, heating for dissolving, then shearing at a high speed, and removing oxygen in vacuum to obtain a composite aqueous solution containing the gelatin and the sugar;
(3) in an inert gas environment, adding the vitamin A acetate molten oil containing the antioxidant in the step (1) into the compound aqueous solution containing the gelatin and the sugar in the step (2), and then carrying out high-speed shearing, high-pressure homogenizing emulsification and micron filtration to obtain uniform and stable emulsion;
(4) spray drying the prepared emulsion by using a rotary atomizer, simultaneously adding starch, enabling the rotation direction of emulsion droplets to be opposite to the rotation direction of the starch in the spray drying process, controlling the centrifugal rotation speed, the feeding amount, the air inlet temperature and the starch flow rate, and embedding the emulsion droplets in the starch to obtain microcapsule particles;
(5) and (4) drying and screening the microcapsule particles obtained in the step (4), and then transferring the microcapsule particles into a fluidized bed dryer for crosslinking to obtain the vitamin A acetate microcapsule.
2. The preparation method according to claim 1, wherein in the step (1), the mixing mass ratio of the vitamin A acetate to the antioxidant is 100: 0.1-5, preferably 100: 1-5;
the antioxidant is selected from one or more of ethoxyquinoline, butyl hydroxy anisole, 2, 6-di-tert-butyl-4-methylphenol, tocopherol and ascorbic acid, and is preferably ethoxyquinoline;
the inert gas is selected from one or more of nitrogen, helium and argon, and is preferably nitrogen;
the melting temperature is 55-75 ℃, and preferably 60-70 ℃; the melting time is 20-120 min, preferably 30-60 min.
3. The preparation method according to claim 1 or 2, wherein in step (2), the gelatin is selected from one or more of porcine skin gelatin, porcine bone gelatin, bovine skin gelatin and bovine bone gelatin, preferably bovine bone gelatin; the isoelectric point of the gelatin is 3.5-6.5, preferably 4.5-5.5; the freezing degree of the gelatin is 20-180 bloom, and preferably 20-60 bloom;
the sugar is selected from one or more of glucose, fructose, sucrose, lactose, maltose and galactose, and is preferably sucrose;
the metal inorganic salt is selected from sulfate or hydrochloride of metal, and the metal is selected from iron, calcium, magnesium and copper; preferably, the metal inorganic salt is one or more of ferrous sulfate, ferric sulfate, calcium sulfate, ferric chloride, ferrous chloride, calcium chloride, magnesium chloride and copper sulfate, and is more preferably ferrous sulfate;
the emulsifier is selected from one or more of lignosulfonate, nano silicon dioxide, nano aluminum oxide, nano talcum powder, nano cellulose, ammonium alginate and sodium alginate, and is preferably nano cellulose and/or nano silicon dioxide;
the thickener is selected from one or more of fumed silica, sodium bentonite, sodium lignosulphonate, lignin, tannin resin and rosin, and is preferably lignin;
the mass ratio of the water, the gelatin, the sugar, the emulsifier, the thickener and the metal inorganic salt is 1: 0.3-0.5: 0.15-0.45: 0.01-0.05: 0.005-0.02: 0.005-0.02, preferably 1: 0.3-0.4: 0.2-0.4: 0.02-0.04: 0.01-0.02: 0.01 to 0.02.
4. The method according to any one of claims 1 to 3, wherein in the step (2), the heating is performed to dissolve the mixture at a temperature of 55 to 75 ℃, preferably 60 to 70 ℃; the time is 20-120 min, preferably 20-60 min;
the high-speed shearing is carried out at the rotating speed of 5000-15000 rpm, preferably at 6000-8000 rpm; the time is 5-60 min, preferably 10-15 min;
the vacuum oxygen removal pressure is-0.05 to-0.1 Mpa, preferably-0.07 to-0.08 Mpa; the time is 0.5 to 3 hours, preferably 1 to 2 hours.
5. The preparation method according to any one of claims 1 to 4, wherein in the step (3), the mass ratio of the antioxidant-containing vitamin A acetate molten oil to the complex aqueous solution containing gelatin and sugar is 1:3 to 10, preferably 1:3.5 to 6;
the high-speed shearing rate is 6000-20000 rpm, preferably 8000-15000 rpm; the time is 5-50 min, preferably 10-30 min;
the high-pressure homogenizing and emulsifying, wherein the pressure is 20-60 MpaG, and preferably 30-50 MpaG; the number of times is 2-6, preferably 2-3;
the micron filtration is carried out, and the filtration precision is 0.5-5 μm, preferably 0.5-2.5 μm; the average particle size of the emulsion after the micron filtration operation is 0.2-2.0 μm, preferably 0.2-1.0 μm.
6. The process according to any one of claims 1 to 5, wherein in step (4), the rotary atomizer is selected from the group consisting of a smooth disk atomizer, a wheel atomizer, a rotary-air cup atomizer, preferably a wheel atomizer;
the centrifugal rotating speed of the rotary atomizer is 4000-12000 rpm, and is preferably 4000-6000 rpm;
the feeding mass ratio of the emulsion to the starch in the rotary atomizer is 1: 1-8, preferably 1: 2-3; the starch flow is 3-12 kg/h, preferably 3.5-5 kg/h; the air inlet temperature is 20-70 ℃, and preferably 30-50 ℃.
7. The method according to any one of claims 1 to 6, wherein in the step (5), the drying temperature is 80 to 130 ℃, preferably 80 to 105 ℃; drying until the water content is 2-10 wt%, preferably 5-7 wt%;
the particle size range of the screened particles is 180-400 mu m, preferably 210-350 mu m;
the temperature of the crosslinking is 60-130 ℃, and preferably 80-90 ℃; the time is 10 to 240min, preferably 30 to 60 min.
8. A vitamin a acetate microcapsule prepared by the process of any one of claims 1 to 9.
9. The vitamin A acetate microcapsule according to claim 8, wherein the particle size of the vitamin A acetate microcapsule is 180 to 400 μm, preferably 210 to 350 μm; the water content is 0.5-1.5 wt%; the microcapsule can be stably stored for 1-1.5 years at room temperature, and the loss rate of the vitamin A acetate is lower than 3%.
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| CN113181157B (en) * | 2021-05-24 | 2023-04-07 | 万华化学集团股份有限公司 | Preparation method of vitamin A acetate micro-capsule |
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