CN111718288A - 一种叶黄素酯和水溶型叶黄素酯微胶囊及其制备方法 - Google Patents
一种叶黄素酯和水溶型叶黄素酯微胶囊及其制备方法 Download PDFInfo
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- CN111718288A CN111718288A CN202010603864.8A CN202010603864A CN111718288A CN 111718288 A CN111718288 A CN 111718288A CN 202010603864 A CN202010603864 A CN 202010603864A CN 111718288 A CN111718288 A CN 111718288A
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- Prior art keywords
- lutein ester
- lutein
- oil
- water
- 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.)
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- KBPHJBAIARWVSC-RGZFRNHPSA-N lutein Chemical compound C([C@H](O)CC=1C)C(C)(C)C=1\C=C\C(\C)=C\C=C\C(\C)=C\C=C\C=C(/C)\C=C\C=C(/C)\C=C\[C@H]1C(C)=C[C@H](O)CC1(C)C KBPHJBAIARWVSC-RGZFRNHPSA-N 0.000 title claims abstract description 118
- 239000003094 microcapsule Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000002245 particle Substances 0.000 claims abstract description 35
- 235000005881 Calendula officinalis Nutrition 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 24
- 238000005406 washing Methods 0.000 claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 claims abstract description 6
- 230000008569 process Effects 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 5
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 45
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 34
- 239000003921 oil Substances 0.000 claims description 22
- 235000019198 oils Nutrition 0.000 claims description 22
- 239000000839 emulsion Substances 0.000 claims description 21
- 239000000463 material Substances 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- 239000003963 antioxidant agent Substances 0.000 claims description 14
- 230000003078 antioxidant effect Effects 0.000 claims description 14
- 235000006708 antioxidants Nutrition 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 239000003995 emulsifying agent Substances 0.000 claims description 10
- 239000000047 product Substances 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- 239000003599 detergent Substances 0.000 claims description 9
- 238000010008 shearing Methods 0.000 claims description 9
- GVJHHUAWPYXKBD-UHFFFAOYSA-N (±)-α-Tocopherol Chemical compound OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 claims description 8
- 239000000287 crude extract Substances 0.000 claims description 8
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 8
- 229930195729 fatty acid Natural products 0.000 claims description 8
- 239000000194 fatty acid Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- 229940107604 lutein esters Drugs 0.000 claims description 7
- 150000002658 luteins Chemical class 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- 235000015112 vegetable and seed oil Nutrition 0.000 claims description 7
- 239000008158 vegetable oil Substances 0.000 claims description 7
- 240000000785 Tagetes erecta Species 0.000 claims description 6
- 239000000945 filler Substances 0.000 claims description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 6
- -1 sucrose fatty acid ester Chemical class 0.000 claims description 6
- 229930006000 Sucrose Natural products 0.000 claims description 5
- 240000008042 Zea mays Species 0.000 claims description 5
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 claims description 5
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims description 5
- 235000005822 corn Nutrition 0.000 claims description 5
- 239000005720 sucrose Substances 0.000 claims description 5
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- 229920000881 Modified starch Polymers 0.000 claims description 4
- 239000004368 Modified starch Substances 0.000 claims description 4
- 235000004347 Perilla Nutrition 0.000 claims description 4
- 244000124853 Perilla frutescens Species 0.000 claims description 4
- 229920001938 Vegetable gum Polymers 0.000 claims description 4
- 229930003427 Vitamin E Natural products 0.000 claims description 4
- WIGCFUFOHFEKBI-UHFFFAOYSA-N gamma-tocopherol Natural products CC(C)CCCC(C)CCCC(C)CCCC1CCC2C(C)C(O)C(C)C(C)C2O1 WIGCFUFOHFEKBI-UHFFFAOYSA-N 0.000 claims description 4
- 235000021552 granulated sugar Nutrition 0.000 claims description 4
- 235000019426 modified starch Nutrition 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims description 4
- 239000011265 semifinished product Substances 0.000 claims description 4
- 235000019165 vitamin E Nutrition 0.000 claims description 4
- 229940046009 vitamin E Drugs 0.000 claims description 4
- 239000011709 vitamin E Substances 0.000 claims description 4
- JLPULHDHAOZNQI-ZTIMHPMXSA-N 1-hexadecanoyl-2-(9Z,12Z-octadecadienoyl)-sn-glycero-3-phosphocholine Chemical class CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCCCCCC\C=C/C\C=C/CCCCC JLPULHDHAOZNQI-ZTIMHPMXSA-N 0.000 claims description 3
- 229920000858 Cyclodextrin Polymers 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
- 229920002907 Guar gum Polymers 0.000 claims description 3
- 229920002774 Maltodextrin Polymers 0.000 claims description 3
- 239000005913 Maltodextrin Substances 0.000 claims description 3
- 244000275012 Sesbania cannabina Species 0.000 claims description 3
- 230000009471 action Effects 0.000 claims description 3
- FYGDTMLNYKFZSV-DZOUCCHMSA-N alpha-D-Glcp-(1->4)-alpha-D-Glcp-(1->4)-D-Glcp 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]2[C@H](OC(O)[C@H](O)[C@H]2O)CO)[C@H](O)[C@H]1O FYGDTMLNYKFZSV-DZOUCCHMSA-N 0.000 claims description 3
- 239000008103 glucose Substances 0.000 claims description 3
- 239000000665 guar gum Substances 0.000 claims description 3
- 235000010417 guar gum Nutrition 0.000 claims description 3
- 229960002154 guar gum Drugs 0.000 claims description 3
- 229940035034 maltodextrin Drugs 0.000 claims description 3
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 claims description 3
- 235000012424 soybean oil Nutrition 0.000 claims description 3
- 239000003549 soybean oil Substances 0.000 claims description 3
- 239000006188 syrup Substances 0.000 claims description 3
- 235000020357 syrup Nutrition 0.000 claims description 3
- 150000001720 carbohydrates Chemical class 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- YKYONYBAUNKHLG-UHFFFAOYSA-N n-Propyl acetate Natural products CCCOC(C)=O YKYONYBAUNKHLG-UHFFFAOYSA-N 0.000 claims description 2
- 229940090181 propyl acetate Drugs 0.000 claims description 2
- 235000000346 sugar Nutrition 0.000 claims description 2
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 claims description 2
- 240000007472 Leucaena leucocephala Species 0.000 claims 1
- 235000010643 Leucaena leucocephala Nutrition 0.000 claims 1
- 235000010956 sodium stearoyl-2-lactylate Nutrition 0.000 claims 1
- KNYAZNABVSEZDS-UHFFFAOYSA-M sodium;2-octadecanoyloxypropanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC(=O)OC(C)C([O-])=O KNYAZNABVSEZDS-UHFFFAOYSA-M 0.000 claims 1
- 241000736851 Tagetes Species 0.000 abstract description 21
- 230000000694 effects Effects 0.000 abstract description 6
- 235000013305 food Nutrition 0.000 abstract description 4
- 239000002775 capsule Substances 0.000 abstract description 3
- 239000003814 drug Substances 0.000 abstract description 3
- 238000000605 extraction Methods 0.000 abstract description 2
- 238000000746 purification Methods 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 239000011162 core material Substances 0.000 description 8
- 239000010696 ester oil Substances 0.000 description 8
- 239000000843 powder Substances 0.000 description 6
- 229930003231 vitamin Natural products 0.000 description 6
- 239000011782 vitamin Substances 0.000 description 6
- 235000013343 vitamin Nutrition 0.000 description 6
- 229940088594 vitamin Drugs 0.000 description 6
- 150000003722 vitamin derivatives Chemical class 0.000 description 6
- 235000012680 lutein Nutrition 0.000 description 5
- 239000001656 lutein Substances 0.000 description 5
- 229960005375 lutein Drugs 0.000 description 5
- ORAKUVXRZWMARG-WZLJTJAWSA-N lutein Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C1=C(C)CCCC1(C)C)C=CC=C(/C)C=CC2C(=CC(O)CC2(C)C)C ORAKUVXRZWMARG-WZLJTJAWSA-N 0.000 description 5
- 238000003860 storage Methods 0.000 description 5
- KBPHJBAIARWVSC-XQIHNALSSA-N trans-lutein Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C1=C(C)CC(O)CC1(C)C)C=CC=C(/C)C=CC2C(=CC(O)CC2(C)C)C KBPHJBAIARWVSC-XQIHNALSSA-N 0.000 description 5
- FJHBOVDFOQMZRV-XQIHNALSSA-N xanthophyll Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C1=C(C)CC(O)CC1(C)C)C=CC=C(/C)C=CC2C=C(C)C(O)CC2(C)C FJHBOVDFOQMZRV-XQIHNALSSA-N 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 238000001694 spray drying Methods 0.000 description 4
- 235000010489 acacia gum Nutrition 0.000 description 3
- 230000036541 health Effects 0.000 description 3
- 229940080352 sodium stearoyl lactylate Drugs 0.000 description 3
- ODFAPIRLUPAQCQ-UHFFFAOYSA-M sodium stearoyl lactylate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC(=O)OC(C)C(=O)OC(C)C([O-])=O ODFAPIRLUPAQCQ-UHFFFAOYSA-M 0.000 description 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- 239000004366 Glucose oxidase Substances 0.000 description 2
- 235000012311 Tagetes erecta Nutrition 0.000 description 2
- 239000001785 acacia senegal l. willd gum Substances 0.000 description 2
- 239000000812 cholinergic antagonist Substances 0.000 description 2
- 239000000625 cyclamic acid and its Na and Ca salt Substances 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000004945 emulsification Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000004665 fatty acids Chemical class 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002674 ointment Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 210000001525 retina Anatomy 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 240000007124 Brassica oleracea Species 0.000 description 1
- 235000003899 Brassica oleracea var acephala Nutrition 0.000 description 1
- 235000011301 Brassica oleracea var capitata Nutrition 0.000 description 1
- 235000001169 Brassica oleracea var oleracea Nutrition 0.000 description 1
- 208000002177 Cataract Diseases 0.000 description 1
- 206010011224 Cough Diseases 0.000 description 1
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 description 1
- 229920000084 Gum arabic Polymers 0.000 description 1
- YHGJHDJZIOYZIR-URPSFYETSA-N Helenien Chemical compound CC1(C)C[C@H](OC(=O)CCCCCCCCCCCCCCC)CC(C)=C1\C=C\C(\C)=C\C=C\C(\C)=C\C=C\C=C(/C)\C=C\C=C(/C)\C=C\[C@@H]1C(C)(C)C[C@@H](OC(=O)CCCCCCCCCCCCCCC)C=C1C YHGJHDJZIOYZIR-URPSFYETSA-N 0.000 description 1
- YHGJHDJZIOYZIR-KFTCWRDFSA-N Helenien Natural products O=C(O[C@H]1C=C(C)[C@H](/C=C/C(=C\C=C\C(=C/C=C/C=C(\C=C\C=C(/C=C/C=2C(C)(C)C[C@H](OC(=O)CCCCCCCCCCCCCCC)CC=2C)\C)/C)\C)/C)C(C)(C)C1)CCCCCCCCCCCCCCC YHGJHDJZIOYZIR-KFTCWRDFSA-N 0.000 description 1
- 206010062717 Increased upper airway secretion Diseases 0.000 description 1
- 235000019483 Peanut oil Nutrition 0.000 description 1
- 229930003268 Vitamin C Natural products 0.000 description 1
- 239000000205 acacia gum Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- YHGJHDJZIOYZIR-UHFFFAOYSA-N all-trans-lutein dipalmitate Natural products CC1(C)CC(OC(=O)CCCCCCCCCCCCCCC)CC(C)=C1C=CC(C)=CC=CC(C)=CC=CC=C(C)C=CC=C(C)C=CC1C(C)(C)CC(OC(=O)CCCCCCCCCCCCCCC)C=C1C YHGJHDJZIOYZIR-UHFFFAOYSA-N 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 230000002921 anti-spasmodic effect Effects 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000003385 bacteriostatic effect Effects 0.000 description 1
- 230000000975 bioactive effect Effects 0.000 description 1
- 230000036772 blood pressure Effects 0.000 description 1
- 210000000621 bronchi Anatomy 0.000 description 1
- 235000021466 carotenoid Nutrition 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000916 dilatatory effect Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- CCGKOQOJPYTBIH-UHFFFAOYSA-N ethenone Chemical compound C=C=O CCGKOQOJPYTBIH-UHFFFAOYSA-N 0.000 description 1
- 125000005313 fatty acid group Chemical group 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 229930182470 glycoside Natural products 0.000 description 1
- 150000002338 glycosides Chemical class 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 210000002189 macula lutea Anatomy 0.000 description 1
- 230000004089 microcirculation Effects 0.000 description 1
- YZNWXXJZEDHRKB-UHFFFAOYSA-N octadecyl 2-hydroxypropanoate;sodium Chemical compound [Na].CCCCCCCCCCCCCCCCCCOC(=O)C(C)O YZNWXXJZEDHRKB-UHFFFAOYSA-N 0.000 description 1
- 208000001749 optic atrophy Diseases 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
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- 239000000312 peanut oil Substances 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 208000026435 phlegm Diseases 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
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- 239000000932 sedative agent Substances 0.000 description 1
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- 201000008525 senile cataract Diseases 0.000 description 1
- 230000002048 spasmolytic effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- 230000002936 tranquilizing effect Effects 0.000 description 1
- 238000009461 vacuum packaging Methods 0.000 description 1
- 230000017260 vegetative to reproductive phase transition of meristem Effects 0.000 description 1
- 235000019154 vitamin C Nutrition 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C403/00—Derivatives of cyclohexane or of a cyclohexene or of cyclohexadiene, having a side-chain containing an acyclic unsaturated part of at least four carbon atoms, this part being directly attached to the cyclohexane or cyclohexene or cyclohexadiene rings, e.g. vitamin A, beta-carotene, beta-ionone
- C07C403/24—Derivatives of cyclohexane or of a cyclohexene or of cyclohexadiene, having a side-chain containing an acyclic unsaturated part of at least four carbon atoms, this part being directly attached to the cyclohexane or cyclohexene or cyclohexadiene rings, e.g. vitamin A, beta-carotene, beta-ionone having side-chains substituted by six-membered non-aromatic rings, e.g. beta-carotene
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
- A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
- A61K9/1605—Excipients; Inactive ingredients
- A61K9/1617—Organic compounds, e.g. phospholipids, fats
- A61K9/1623—Sugars or sugar alcohols, e.g. lactose; Derivatives thereof; Homeopathic globules
-
- 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
- A61K9/5089—Processes
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
-
- 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
-
- 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
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/21—Esters, e.g. nitroglycerine, selenocyanates
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/21—Esters, e.g. nitroglycerine, selenocyanates
- A61K31/215—Esters, e.g. nitroglycerine, selenocyanates of carboxylic acids
- 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
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/28—Asteraceae or Compositae (Aster or Sunflower family), e.g. chamomile, feverfew, yarrow or echinacea
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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
- A61K9/0012—Galenical forms characterised by the site of application
- A61K9/0053—Mouth and digestive tract, i.e. intraoral and peroral administration
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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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Abstract
本申请公开了一种叶黄素酯和水溶型叶黄素酯微胶囊及其制备方法。本发明从万寿菊颗粒中提取叶黄素酯,经过浓缩、洗涤、脱残后得到叶黄素酯,再将叶黄素酯通过采用二次包埋法工艺,制备得到叶黄素酯微胶囊。本发明中叶黄素酯为从万寿菊颗粒中提取,原材料经济易得,没有经过分离提纯,保留了万寿菊颗粒的部分药用价值,增加了叶黄素酯的保健功效,同时采用二次包埋法还可以使得制备得到的胶囊更稳定、易存放,适用在于食品、医药等领域。并且有效解决了现有技术中对于提取设备要求较高的技术问题,进而实现了设备要求低,工艺简单,生产成本大幅度降低的技术效果。
Description
技术领域
本发明属于生物活性物质深加工技术领域,具体涉及一种叶黄素酯的提取方法及水溶型叶黄素酯微胶囊的制备方法。
背景技术
万寿菊(Tagetes erecta L)原产墨西哥。中国各地均有分布,可生长在海拔1150米至1480米的地区,其花大、花期长,也常用于花坛布景,其花的药用价值有:清热解毒,化痰止咳;有香味,可作芳香剂;以前曾用作抑菌、镇静、解痉剂。其同属植物Tagetesminuta(T.glanduliflora)含挥发油,有镇静、降压、扩张支气管、解痉及抗炎作用。
叶黄素酯是类胡萝卜素脂肪酸酯,化学名称是叶黄素二棕榈酸酯,易溶于有机溶剂,广泛存在于玉米、甘蓝、万寿菊等植物,其中在万寿菊中含量最为丰富。叶黄素酯是人眼视网膜、黄斑区域的主要组成物质,其抗氧化能力强,防止自由基对眼部的氧化损伤,改善眼部微循环,预防老年白内障、保护视网膜、预防视神经萎缩等多重功效,叶黄素酯必须从食物中摄取。
叶黄素酯是叶黄素和一分子或两分子的脂肪酸形成的化合物,其稳定性强于叶黄素,只有在高温、强酸、氧等因素对其破坏性大;叶黄素酯含有脂肪酸基团,可以在人体内自然水解为游离态叶黄素,易于吸收,生物利用率远高于叶黄素晶体,2008年5月26(卫生部公告2008年第12号)文件:国家卫生部确立批准叶黄素酯为新资源食品功效原料,目前市场上的叶黄素保健制品也多以叶黄素酯为主要功效原料。
微囊化技术是一种有效改善药物稳定性及溶解性的药剂学手段,将芯材包裹在微小的壁材构成的囊中,保留芯材的活性成分不受外界不良因素的影响,延长芯材的保存时间,控制芯材的释放,而二次包埋法是在一次包埋(乳化)的基础上在干燥过程中对芯材进行二次包埋,其干燥温度需求低,避免芯材高温破坏,得到的颗粒比传统喷雾干燥的颗粒更稳定,存放期更长,芯材释放性更可控。
但本申请发明人在实现本申请实施例中发现上述技术至少存在如下技术问题:
(1)现有技术中利用高纯度叶黄素酯晶体进行微胶囊化的工艺,对于设备的要求过高,需要特别复杂的精炼设备,从而带来生产成本的大幅度提高;
(2)现有技术中由于需要利用高纯度叶黄素酯晶体,但是叶黄素酯晶体纯度越高,那么对于运输、储存的条件要求就越高,进一步提高生产的成本。
如何降低生产成本,成为本领域技术人员研究的热点。
发明内容
为了克服在规模化量产不同规格的叶黄素酯微囊粉时成本过高的不足,本申请实施例提供了一种叶黄素酯提取及叶黄素酯微胶囊制备的方法,该制备方法首先通过在万寿菊颗粒中提取得到叶黄素酯,然后通过一系列方法制备叶黄素酯微胶囊的工艺。本发明中,叶黄素酯从万寿菊颗粒中提取得到,之后经过浓缩、洗涤、脱残后得到叶黄素酯,将叶黄素酯通过一系列工艺,制备得到叶黄素酯微胶囊。其中,叶黄素酯为从万寿菊颗粒中提取,原材料经济易得,且没有经过分离提纯,保留了万寿菊颗粒的部分药用价值,增加了叶黄素酯的保健功效,同时采用二次包埋法还可以使得制备得到的胶囊更稳定、易存放,适用在于食品、医药等领域。
本申请实施例解决其技术问题所采用的技术方案是:
一种叶黄素酯的提取方法,所述的方法包括:取万寿菊颗粒,之后采用溶剂对干燥后的万寿菊颗粒进行提取,直至提取的溶剂无颜色为止,取回收的溶剂浓缩,然后用洗涤剂洗涤,分离洗涤剂,即可制备得到叶黄素酯。
优选的,所述的溶剂为正己烷、丙酮、丁酮、乙酸乙酯、乙酸丙酯中的一种,该部分溶剂对叶黄素酯溶解度大,并且方便易得;所述的洗涤剂为乙醇、乙二醇、丙二醇、异丙醇中的一种或两种以任意比例组成,提取的混合物中有脂肪酸、酮、烯酮、甙和其他极性小分子,该部分洗涤剂用极性良性溶剂,能够满足较好的洗涤,操作方便等要求。洗涤的次数为2-9次;制备得到的叶黄素酯的浓度为45-70%。
由上述叶黄素酯制备水溶型叶黄素酯微胶囊的方法,所述的制备方法中包含如下组分:叶黄素酯1份、油相抗氧化剂0.03-0.8份、植物油1-8份、壁材1-30份、乳化剂0.1-8份、水相抗氧化剂0.02-0.8份、水相填充剂0.2-30份、水10-200份。
优选的,所述的方法包括以下步骤:
(1)将叶黄素酯与植物油、油相抗氧化剂混合油浴加热溶解均匀制得油相,将壁材、乳化剂、水相抗氧化剂、水相填充剂加入水中,加热充分溶解制得水相;
(2)油相缓慢加入到高速剪切作用下的水相中,混合均匀,经过高压均质机均质,制得叶黄素酯乳液;
(3)对均质后的叶黄素酯乳液进行二次包埋干燥,得到叶黄素酯微胶囊半成品;
(4)对叶黄素酯微胶囊半成品进行固化,得到叶黄素酯微胶囊成品。
优选的,步骤(1)中,油相溶解温度是70℃~135℃,壁材的溶解温度是60℃~85℃,温度过低叶黄素酯无法完全溶解(分子化),在乳化时无法被壁材包埋,会以油状浮于液面,影响产品品质,温度越高,叶黄素酯损失越快,产品含量不够,经过申请人的研究发现,在该温度条件下,能够达到较好的效果。
步骤(2)中,剪切速度是4000~10000转每分钟,均质压力为20~60Mpa;溶解后的芯材与水相壁材快速结合,在高剪切力作用下使壁材包裹芯材,得到均匀的微胶囊形态,达到稳定的水包油乳化体系。速度低时芯材和壁材会以半包埋态存在,速度高,会破坏已形成的微囊颗粒,芯材可能被剥离壁材,乳液破乳,经过申请人的研究发现,在该剪切速度下,能够达到较好的效果。
步骤(3)中,二次包埋干燥法进风温度是60-120℃,进料速度为是10~90ml每分钟;
步骤(4)中,叶黄素酯微胶囊固化温度是-18℃-120℃,固化时间是30分钟-24小时。
优选的,所述的油相抗氧化剂是天然维生素E,天然维生素E可以减缓叶黄素酯的氧化,减少热损失,延长货架期。
优选的,所述的植物油为大豆油、玉米胚芽油、紫苏油中的任意一种或任意两种组成的混合物,植物油的使用使得溶解的叶黄素酯使其更容易。
优选的,所述的壁材为糖类或植物胶,壁材是微胶囊必须的膜衣;其中,糖类包括变性淀粉、麦芽糊精或环糊精,植物胶为阿拉伯胶、田菁胶或瓜尔胶。
优选的,所述的乳化剂为蔗糖脂肪酸酯、改性大豆磷脂、单棕榈酸酯、硬脂酰乳酸钠中的任意两种或任意三种组成的混合物,乳化剂可以使得乳液更加稳定,增强壁材的乳化(包埋)能力,
优选的,所述的水相填充剂是白砂糖、葡萄糖浆、低聚麦芽糖中的一种或任意两种组成的混合物,可以增强乳液的稳定性,降低乳液破乳风险。
本发明与现有技术相比的优点在于:
1、由于采用了直接从万寿菊颗粒中提取叶黄素酯的技术手段,所以,有效解决了现有技术中对于提取设备要求较高的技术问题,进而实现了设备要求低,工艺简单的技术效果。
2、由于采用了直接从万寿菊颗粒中提取叶黄素酯的技术手段,所以,有效解决了现有技术中制备叶黄素酯成本较高的技术问题,进而实现万寿菊颗粒易贮存,并且生产后的叶黄素酯检测合格后经由管道可直接进入制剂工段,得到微囊化颗粒,产能不受影响,产品品质与用叶黄素酯纯品做的没有显著差异,成本却能大幅降低的技术效果。
3、由于采用了直接从万寿菊颗粒中提取叶黄素酯的技术手段,所以,有效解决了现有技术中纯度较高的叶黄素酯对运输和储存的条件要求较高的问题,通过本方法可控制得到的叶黄素酯的含量,在开发低含量(0.5%-5%)叶黄素酯微胶囊产品时不需要对叶黄素酯进一步纯化,只需要控制在一个合适的范围便于制剂化操作即可。
具体实施方式
本申请实施例通过提供一种叶黄素酯提取及叶黄素酯微胶囊制备的方法,解决现有技术中规模化量产不同规格的叶黄素酯微囊粉时成本过高的问题,在制备方法首先通过在万寿菊颗粒中提取得到叶黄素酯,然后通过一系列方法制备叶黄素酯微胶囊的工艺,在提取叶黄素酯中运用了直接从万寿菊颗粒中提取出来的技术,实现保留万寿菊颗粒的部分药用价值,增加了叶黄素酯的保健功效,同时采用二次包埋法还可以使得制备得到的胶囊更稳定、易存放,适用于食品、医药等领域,极大的降低了叶黄素酯微囊粉的生产成本。
一、制备叶黄素酯:
实施例1
称取100g万寿菊花颗粒,加入2L圆底烧瓶,加入1.5L乙酸乙酯,85℃水浴搅拌保温回流,乙酸乙酯与万寿菊花颗粒混合将叶黄素酯及其他脂溶性物质提取出来,直到回流的乙酸乙酯变为无色即为提取完全,回收乙酸乙酯得到叶黄素酯粗提物,用乙二醇:丙二醇=1:1的混合物冲洗粗提物3次,真空加热回收洗涤剂,加入少量抗氧化剂混合得到含量48%的叶黄素酯。
实施例2
称取100g万寿菊花颗粒,加入2L圆底烧瓶,加入1.5L正己烷,80℃水浴搅拌保温回流,乙酸乙酯与万寿菊花颗粒混合将叶黄素酯及其他脂溶性物质提取出来,直到回流的乙酸乙酯变为无色即为提取完全,回收乙酸乙酯得到叶黄素酯粗提物,用乙醇:丙二醇=5:1的混合物冲洗粗提物7次,真空加热回收洗涤剂,加入少量抗氧化剂混合得到含量59.5%的叶黄素酯。
实施例3
称取100g万寿菊花颗粒,加入2L圆底烧瓶,加入1.5L丙酮,65℃水浴搅拌保温回流,纯净的乙酸乙酯与万寿菊花颗粒混合将叶黄素酯及其他脂溶性物质提取出来,直到回流的乙酸乙酯变为无色即为提取完全,回收乙酸乙酯得到叶黄素酯粗提物,用乙醇冲洗粗提物9次,真空加热回收洗涤剂,加入少量抗氧化剂混合得到含量69%的叶黄素酯(E1102)。
二、由上述叶黄素酯制备水溶型叶黄素酯微胶囊
实施例1
称取48%的叶黄素酯(E768)20g和混合天然维生素E1g置于烧杯中,向其中加入40g大豆油,置于90℃搅拌加热20min完全溶解,得到叶黄素酯油相。称取变性淀粉100g、麦芽糊精70g、维生素C2g、白砂糖25g加入500ml去离子水中,60℃搅拌溶解15min得到水相,将叶黄素酯油相加入水相中,加入2g乳化剂(蔗糖脂肪酸酯:硬脂酰乳酸钠=2:1),6000r/min剪切10min形成初乳,在30MPa压力下均质2次,得到均匀乳液,对乳液进行二次包埋干燥,干燥条件为:进风60-70℃,进料速度10ml每分钟,得到的颗粒通过不同目数的标准筛,可以得到不同粒径的球状叶黄素酯微胶囊,对叶黄素酯微胶囊进行固化,固化温度-16℃,时间12小时,得到水溶性叶黄素酯微胶囊。
实施例2
称取59.5%的叶黄素酯(E952)50g和混合天然维生素E2.3g置于烧杯中,向其中加入80g玉米胚芽油,置于90℃搅拌加热20min完全溶解,得到叶黄素酯油相。称取瓜儿胶300g、环糊精200g、维生素C3g、葡萄糖浆55g,加入800ml去离子水中,60℃搅拌溶解25min得到水相,将叶黄素酯油相加入水相中,加入5.6g乳化剂(蔗糖脂肪酸酯:改性大豆磷脂=0.5:1),7800r/min高速剪切10min形成初乳,在30MPa压力下均质3次,得到均匀乳液,对乳液进行二次包埋干燥,干燥条件为:进风60-70℃,进料速度15ml每分钟,得到的颗粒通过不同目数的标准筛,可以得到不同粒径的球状叶黄素酯微胶囊,对叶黄素酯微胶囊进行固化,固化温度-8℃,时间18小时,得到水溶性叶黄素酯微胶囊。
实施例3
称取59.5%叶黄素酯油膏(E952)50g和混合天然维生素E4g置于烧杯中,向其中加入120g(紫苏油:花生油=1:2),置于100℃搅拌加热10min完全溶解,得到叶黄素酯油相。称取阿拉伯胶400g、田菁胶110g、维生素C3g、白砂糖35g加入800ml蒸馏水中,70℃搅拌溶解15min得到水相,将叶黄素酯油相加入水相中,加入5.5g乳化剂(单棕榈酸酯:硬脂酰乳酸钠=1:1),7800r/min高速剪切10min形成初乳,在55MPa压力下均质2次,得到均匀乳液,对乳液进行二次包埋干燥,干燥条件为:进风80-90℃,进料速度10ml每分钟,得到的颗粒通过不同目数的标准筛,可以得到不同粒径的球状叶黄素酯微胶囊,对叶黄素酯微胶囊进行固化,固化温度56℃,时间9小时,得到水溶性叶黄素酯微胶囊。
实施例4
称取69%的叶黄素酯(E1102)100g和混合天然维生素E4g置于烧杯中,向其中加入180g(玉米胚芽油:紫苏油=3:1),置于110℃油浴搅拌加热8min完全溶解,得到叶黄素酯油相。称取变性淀粉500g、阿拉伯胶200g、维生素C3g、低聚麦芽糖65g加入1100ml蒸馏水中,80℃搅拌溶解30min得到水相,将叶黄素酯油相加入水相中,加入7.5g乳化剂(蔗糖脂肪酸酯:硬脂酰乳酸钠:单棕榈酸酯=1:1:1),10000r/min高速剪切13min形成初乳,在45MPa压力下均质4次,得到均匀乳液,对乳液进行二次包埋干燥,干燥条件为:进风95-105℃,进料速度35ml每分钟,得到的颗粒通过不同目数的标准筛,可以得到不同粒径的球状叶黄素酯微胶囊对叶黄素酯微胶囊进行固化,固化温度115℃,时间2小时,得到水溶性叶黄素酯微胶囊。
在稳定性应用测试中,在环境温度55℃,非真空包装密封、避光存储的条件下,将二次包埋干燥颗粒和常规喷雾干燥粉末分别存放24小时、48小时、72小时,二次包埋干燥颗粒含量损失比例分别是0%、0.03%、0.18%,常规喷雾干燥粉末含量损失比例分别是0.53%、2.97%、7.29%,且常规喷雾干燥粉末有轻微油脂渗出现象,由此可见二次包埋干燥的产品稳定性比常规喷雾干燥粉有很大提高,对运输、存储的条件要求低,在实际应用中能增加产品的保质期。
最后应说明的是:显然,上述实施例仅仅是为清楚地说明本发明所作的举例,而并非对实施方式的限定。对于所属领域的普通技术人员来说,在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无需也无法对所有的实施方式予以穷举。而由此所引申出的显而易见的变化或变动仍处于本发明的保护范围之中。
Claims (10)
1.一种叶黄素酯的制备方法,其特征在于,所述的方法为:
取万寿菊颗粒,之后采用溶剂对干燥后的万寿菊颗粒进行提取,直至提取的溶剂无颜色为止,取回收的溶剂浓缩,然后用洗涤剂洗涤,分离洗涤剂,即可制备得到叶黄素酯。
2.如权利要求1所述的一种叶黄素酯制备方法,其特征在于,所述的溶剂为正己烷、丙酮、丁酮、乙酸乙酯、乙酸丙酯中的一种;所述的洗涤剂为乙醇、乙二醇、丙二醇、异丙醇中的一种或任意两种任意比例混合组成,洗涤的次数为2-13次。
3.如权利要求1或2所述的一种叶黄素酯的制备方法,其特征在于,制备得到的叶黄素酯的浓度为45-70%。
4.如权利要求1或2所述的一种叶黄素酯的制备方法,其特征在于,包括如下步骤:称取100g万寿菊花颗粒,加入2L圆底烧瓶,加入1.5L丙酮,65℃水浴搅拌保温回流,纯净的乙酸乙酯与万寿菊花颗粒混合将叶黄素酯及其他脂溶性物质提取出来,直到回流的乙酸乙酯变为无色即为提取完全,回收乙酸乙酯得到叶黄素酯粗提物,用乙醇冲洗粗提物13次,真空加热回收洗涤剂,加入少量抗氧化剂混合得到叶黄素酯。
5.一种水溶型叶黄素酯微胶囊,其特征在于,按照重量份数计,制备原料组成为:叶黄素酯1份、油相抗氧化剂0.03-2.0份、植物油1-10份、壁材1-50份、乳化剂0.1-8份、水相抗氧化剂0.02-2.0份、水相填充剂0.2-50份、水10-200份。
6.如权利要求5所述的一种叶黄素酯微胶的囊制备方法,其特征在于,制备方法包括以下步骤:
(1)将叶黄素酯与植物油、油相抗氧化剂混合油浴加热溶解均匀制得油相,将壁材、乳化剂、水相抗氧化剂、水相填充剂加入水中,加热充分溶解制得水相;
(2)油相缓慢加入到高速剪切作用下的水相中,混合均匀,经过高压均质机均质,制得叶黄素酯乳液;
(3)对均质后的叶黄素酯乳液进行二次包埋干燥,得到叶黄素酯微胶囊半成品;
(4)对叶黄素酯微胶囊半成品进行固化,得到叶黄素酯微胶囊成品。
7.如权利要求6所述的一种叶黄素酯微胶囊的制备方法,其特征在于,
步骤(1)中,油相溶解温度是70℃~135℃,壁材的溶解温度是60℃~85℃;
步骤(2)中,剪切速度是4000~10000转每分钟,均质压力为20~60Mpa;
步骤(3)中,二次包埋干燥法进风温度是60-120℃,进料速度为10~90ml每分钟;
步骤(4)中,叶黄素酯微胶囊固化温度是-18℃-120℃,固化时间是30分钟-24小时。
8.如权利要求7所述的一种叶黄素酯微胶囊的制备方法,其特征在于,所述的油相抗氧化剂是天然维生素E。
9.如权利要求7所述的一种叶黄素酯微胶囊制备的方法,其特征在于,所述的植物油为大豆油、玉米胚芽油、紫苏油中的任意一种或任意两种组成的混合物。
10.如权利要求7所述的一种叶黄素酯微胶囊的制备方法,其特征在于,所述的壁材为糖类或植物胶;其中,糖类包括变性淀粉、麦芽糊精或环糊精,植物胶为阿拉伯胶、田菁胶或瓜尔胶;所述的乳化剂为蔗糖脂肪酸酯、改性大豆磷脂、单棕榈酸酯、硬脂酰乳酸钠中的任意两种或任意三种组成的混合物;所述的水相填充剂是白砂糖、葡萄糖浆、低聚麦芽糖中的一种或任意两种组成的混合物。
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CN113115945A (zh) * | 2021-03-29 | 2021-07-16 | 湖南万象生物科技有限公司 | 一种叶黄素复方微囊粉及其制备方法与应用 |
CN114957073A (zh) * | 2021-02-25 | 2022-08-30 | 内蒙古昶辉生物科技股份有限公司 | 利用万寿菊油膏制备叶黄素酯的方法与叶黄素酯 |
CN115160822A (zh) * | 2022-07-26 | 2022-10-11 | 武汉星辰现代生物工程有限公司 | 一种叶黄素酯的生产工艺 |
CN115251376A (zh) * | 2022-07-28 | 2022-11-01 | 青岛康小鹿生物科技有限公司 | 一种叶黄素酯纳米微囊及其制备方法 |
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101288662A (zh) * | 2008-05-09 | 2008-10-22 | 济南大学 | 一种叶黄素微胶囊及其制备方法 |
CN103735532A (zh) * | 2014-01-15 | 2014-04-23 | 山东星光生物科技有限公司 | 叶黄素酯微胶囊及其制备方法 |
CN109305931A (zh) * | 2018-10-15 | 2019-02-05 | 河南中大恒源生物科技股份有限公司 | 一种叶黄素酯提取及叶黄素酯微胶囊制备的方法 |
CN106262926B (zh) * | 2016-08-11 | 2019-12-10 | 晨光生物科技集团股份有限公司 | 一种叶黄素酯微囊制剂及其制备方法和用途 |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DK546289D0 (da) * | 1989-11-02 | 1989-11-02 | Danochemo As | Carotenoidpulvere |
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Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101288662A (zh) * | 2008-05-09 | 2008-10-22 | 济南大学 | 一种叶黄素微胶囊及其制备方法 |
CN103735532A (zh) * | 2014-01-15 | 2014-04-23 | 山东星光生物科技有限公司 | 叶黄素酯微胶囊及其制备方法 |
CN106262926B (zh) * | 2016-08-11 | 2019-12-10 | 晨光生物科技集团股份有限公司 | 一种叶黄素酯微囊制剂及其制备方法和用途 |
CN109305931A (zh) * | 2018-10-15 | 2019-02-05 | 河南中大恒源生物科技股份有限公司 | 一种叶黄素酯提取及叶黄素酯微胶囊制备的方法 |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114957073A (zh) * | 2021-02-25 | 2022-08-30 | 内蒙古昶辉生物科技股份有限公司 | 利用万寿菊油膏制备叶黄素酯的方法与叶黄素酯 |
CN113115945A (zh) * | 2021-03-29 | 2021-07-16 | 湖南万象生物科技有限公司 | 一种叶黄素复方微囊粉及其制备方法与应用 |
CN115160822A (zh) * | 2022-07-26 | 2022-10-11 | 武汉星辰现代生物工程有限公司 | 一种叶黄素酯的生产工艺 |
CN115160822B (zh) * | 2022-07-26 | 2023-08-15 | 武汉星辰现代生物工程有限公司 | 一种叶黄素酯的生产工艺 |
CN115251376A (zh) * | 2022-07-28 | 2022-11-01 | 青岛康小鹿生物科技有限公司 | 一种叶黄素酯纳米微囊及其制备方法 |
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