CN104490994A - Method for extracting lipid-soluble and water-soluble antioxidant from rosemary - Google Patents
Method for extracting lipid-soluble and water-soluble antioxidant from rosemary Download PDFInfo
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- CN104490994A CN104490994A CN201410786659.4A CN201410786659A CN104490994A CN 104490994 A CN104490994 A CN 104490994A CN 201410786659 A CN201410786659 A CN 201410786659A CN 104490994 A CN104490994 A CN 104490994A
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- rosemary
- lixiviating solution
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- 239000003963 antioxidant agent Substances 0.000 title claims abstract description 30
- 230000003078 antioxidant effect Effects 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 16
- 241001529742 Rosmarinus Species 0.000 title claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000605 extraction Methods 0.000 claims abstract description 9
- 239000000341 volatile oil Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 239000000284 extract Substances 0.000 claims description 9
- 238000005516 engineering process Methods 0.000 claims description 7
- 239000003921 oil Substances 0.000 claims description 5
- 238000004061 bleaching Methods 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 4
- 230000001476 alcoholic effect Effects 0.000 claims description 3
- 239000007854 depigmenting agent Substances 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 3
- 238000012423 maintenance Methods 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims 2
- 239000002244 precipitate Substances 0.000 abstract description 5
- 239000004927 clay Substances 0.000 abstract description 4
- 239000007788 liquid Substances 0.000 abstract 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract 2
- 238000001035 drying Methods 0.000 abstract 2
- 238000000926 separation method Methods 0.000 abstract 1
- 235000006708 antioxidants Nutrition 0.000 description 22
- 239000000047 product Substances 0.000 description 10
- 230000000694 effects Effects 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- QRYRORQUOLYVBU-VBKZILBWSA-N Carnosic acid Natural products CC([C@@H]1CC2)(C)CCC[C@]1(C(O)=O)C1=C2C=C(C(C)C)C(O)=C1O QRYRORQUOLYVBU-VBKZILBWSA-N 0.000 description 5
- 244000178231 Rosmarinus officinalis Species 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000003463 adsorbent Substances 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 239000000049 pigment Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000000194 supercritical-fluid extraction Methods 0.000 description 3
- DOUMFZQKYFQNTF-WUTVXBCWSA-N (R)-rosmarinic acid Chemical compound C([C@H](C(=O)O)OC(=O)\C=C\C=1C=C(O)C(O)=CC=1)C1=CC=C(O)C(O)=C1 DOUMFZQKYFQNTF-WUTVXBCWSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- BGNXCDMCOKJUMV-UHFFFAOYSA-N Tert-Butylhydroquinone Chemical compound CC(C)(C)C1=CC(O)=CC=C1O BGNXCDMCOKJUMV-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- -1 diterpene phenolic acids Chemical class 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000008030 elimination Effects 0.000 description 2
- 238000003379 elimination reaction Methods 0.000 description 2
- 239000003925 fat Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- WCGUUGGRBIKTOS-GPOJBZKASA-N (3beta)-3-hydroxyurs-12-en-28-oic acid Chemical compound C1C[C@H](O)C(C)(C)[C@@H]2CC[C@@]3(C)[C@]4(C)CC[C@@]5(C(O)=O)CC[C@@H](C)[C@H](C)[C@H]5C4=CC[C@@H]3[C@]21C WCGUUGGRBIKTOS-GPOJBZKASA-N 0.000 description 1
- 241000722824 Ardisia crenata Species 0.000 description 1
- XUSYGBPHQBWGAD-PJSUUKDQSA-N Carnosol Chemical compound CC([C@@H]1C2)(C)CCC[C@@]11C(=O)O[C@@H]2C2=C1C(O)=C(O)C(C(C)C)=C2 XUSYGBPHQBWGAD-PJSUUKDQSA-N 0.000 description 1
- MMFRMKXYTWBMOM-UHFFFAOYSA-N Carnosol Natural products CCc1cc2C3CC4C(C)(C)CCCC4(C(=O)O3)c2c(O)c1O MMFRMKXYTWBMOM-UHFFFAOYSA-N 0.000 description 1
- 235000008495 Chrysanthemum leucanthemum Nutrition 0.000 description 1
- 241000207923 Lamiaceae Species 0.000 description 1
- CEEMRWKKNNEQDT-UHFFFAOYSA-N Rosmanol Natural products CC(C)c1cc2C(OC(=O)C)C3OC(=O)C4(CCCC(C)(C)C34)c2c(OC(=O)C)c1OC(=O)C CEEMRWKKNNEQDT-UHFFFAOYSA-N 0.000 description 1
- ZZAFFYPNLYCDEP-HNNXBMFYSA-N Rosmarinsaeure Natural products OC(=O)[C@H](Cc1cccc(O)c1O)OC(=O)C=Cc2ccc(O)c(O)c2 ZZAFFYPNLYCDEP-HNNXBMFYSA-N 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 241000404542 Tanacetum Species 0.000 description 1
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000003026 anti-oxygenic effect Effects 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 235000004654 carnosol Nutrition 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229930004069 diterpene Natural products 0.000 description 1
- 239000008157 edible vegetable oil Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229930003944 flavone Natural products 0.000 description 1
- 235000011949 flavones Nutrition 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 229930182470 glycoside Natural products 0.000 description 1
- 150000002338 glycosides Chemical class 0.000 description 1
- 150000008282 halocarbons Chemical class 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 235000014593 oils and fats Nutrition 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 239000002304 perfume Substances 0.000 description 1
- 235000009048 phenolic acids Nutrition 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- DOUMFZQKYFQNTF-MRXNPFEDSA-N rosemarinic acid Natural products C([C@H](C(=O)O)OC(=O)C=CC=1C=C(O)C(O)=CC=1)C1=CC=C(O)C(O)=C1 DOUMFZQKYFQNTF-MRXNPFEDSA-N 0.000 description 1
- LCAZOMIGFDQMNC-FORWCCJISA-N rosmanol Chemical compound C1CCC(C)(C)[C@@H]2[C@H]3[C@@H](O)C(C=C(C(=C4O)O)C(C)C)=C4[C@]21C(=O)O3 LCAZOMIGFDQMNC-FORWCCJISA-N 0.000 description 1
- TVHVQJFBWRLYOD-UHFFFAOYSA-N rosmarinic acid Natural products OC(=O)C(Cc1ccc(O)c(O)c1)OC(=Cc2ccc(O)c(O)c2)C=O TVHVQJFBWRLYOD-UHFFFAOYSA-N 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000001256 steam distillation Methods 0.000 description 1
- 239000004250 tert-Butylhydroquinone Substances 0.000 description 1
- 235000019281 tert-butylhydroquinone Nutrition 0.000 description 1
- PLSAJKYPRJGMHO-UHFFFAOYSA-N ursolic acid Natural products CC1CCC2(CCC3(C)C(C=CC4C5(C)CCC(O)C(C)(C)C5CCC34C)C2C1C)C(=O)O PLSAJKYPRJGMHO-UHFFFAOYSA-N 0.000 description 1
- 229940096998 ursolic acid Drugs 0.000 description 1
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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)
- A61K36/53—Lamiaceae or Labiatae (Mint family), e.g. thyme, rosemary or lavender
-
- 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
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/10—General cosmetic use
Abstract
The invention provides a method for extracting lipid-soluble and water-soluble antioxidants from rosemary. The method comprises the following steps: (1) naturally drying in harvested tender stems and leaves of rosemary in shadow places; (2) distilling the naturally dried rosemary by using steam, thereby obtaining rosemary essential oil and residues; (3) crushing the residues obtained after the essential oil is extracted, adding an ethanol solution with certain concentration, performing ultrasonic auxiliary extraction for multiple times, andperforming centrifugal separation after extraction, thereby obtaining leach liquids, and combining the leach liquids; (4) decoloring the leach liquids, adding a certain amount of activated clay into the leach liquids, stirring and maintaining for a certain time at a certain temperature, and removing the activated clay, thereby obtaining a decolored leach liquid; (5) performing vacuum concentration on the decolored leach liquid till a certain volume is achieved, and separating out the precipitate; (6) centrifuging the concentrated solution to obtain precipitate and water phase; and (7) respectively drying the precipitate and the water phase in vacuum, thereby obtaining a lipid-soluble antioxidant and a water-soluble antioxidant.
Description
Technical field
The present invention relates to Herba Rosmarini Officinalis the combined extraction method of various active composition, from Herba Rosmarini Officinalis raw material, especially extract fat-soluble and method that is water soluble antioxidant.
Technical background
Herba Rosmarini Officinalis, another name tansy, belong to Labiatae undershrub or perennial herb spice berry, originate in Mediterranean Region, China successfully introduced a fine variety in late 1970s, promoted throughout the country subsequently.Be mainly used in extracting quintessence oil and antioxidant except can be used as Herba Rosmarini Officinalis.Rosemary ethereal oil is traditional natural perfume material, also have certain natural anticorrosion effect and clinical efficacy simultaneously, the function of its composition in medicines and health protection, as antiinflammatory, antitumor, the very big concern that anticancer, Cardiovarscular, the liver protecting and ALT lowering etc. aspect also receives domestic and international numerous scholars and researcher.Rosemary antioxidant product category is many, and comprise carnosol, rosmanol, rosmarinic acid, carnosic acid, ursolic acid etc., wherein diterpene phenolic acids is oxidation-resistant active ingredient main in Herba Rosmarini Officinalis.Rosemary antioxidant is because of the antioxygenic property of its uniqueness---safe, efficient, heat-resisting, wide spectrum, and replace artificial antioxidant BHA, BHT, TBHQ etc. to become one of emphasis of food, daily-use chemical industry, the research and development of medicines and health protection aspect in recent years.
Current rosemary ethereal oil mainly uses traditional extraction by steam distillation, also has use CO in the recent period
2the report of supercritical extraction.Rosemary antioxidant then mainly takes edible oil and fat, organic solvent, supercritical CO
2supercritical extraction, aqueous alkali and superheated water etc. extract, and also can comprehensively use several extracting method.Mainly there is following deficiency in the production technology extracting antioxidant in Herba Rosmarini Officinalis: needs to carry out supercritical extraction, freeze and separate or lyophilization (1) some technical process existing, and its equipment investment is large, causes production cost high; (2) most of production technology generally only obtains mixing antioxidant, is not separated it further again, causes product single, and can not water-soluble or liposoluble complete, limit the range of application of this antioxidant, resource added value is low; (3) decolorizing effect is not good, cause product colour Wei ?yellow; (4) the existing irrationality of technique in production application: is that in process, some uses the organic solvent extraction antioxidants such as halogenated hydrocarbons, acetone or methanol, these solvents are harmful to operator's health, and in product, the dissolvent residual of trace is harmful; Two is use acid or alkali liquor in some technology, and soda acid can cause the destruction of part effective ingredient in Herba Rosmarini Officinalis, and as glycoside material facile hydrolysis under acid or alkali condition, flavone compound is easily degraded in the basic conditions and loses antioxidant activity.
Decolouring is divided into adsorption bleaching and chemical decolorization, and oils and fats pretreatment generally adopts adsorption bleaching.The quality of decolorizing effect directly has influence on product quality and cost, therefore selects the adsorbent that is suitable for of crucial importance.Conventional adsorbent has active carbon and hargil.Active carbon can optionally adsorpting pigment and stink substance as adsorbent, but expensive, the oily rate of acticarbon is high.Hargil is also known as bleaching clay, and after acidification, its surface area increases greatly, and absorption property improves greatly, and this hargil is called active hargil (or claiming Emathlite).Depigmenting agent conventional when hargil is oil and fat refining.Active hargil is large compared with the k value of natural clay, therefore this experiment adopts active hargil as depigmenting agent.
Summary of the invention
The object of the invention is to the shortcoming overcoming existing technique, there is provided a kind of in Herba Rosmarini Officinalis, extract fat-soluble and method that is water soluble antioxidant, there is the advantages such as yield is high, raw material utilizes fully, production cost is low, greatly improve the application performance of rosemary antioxidant product simultaneously, improve Herba Rosmarini Officinalis added value.
For achieving the above object, the invention provides a kind of fat-soluble and method that is water soluble antioxidant extracted in Herba Rosmarini Officinalis, comprising the steps:
(1) the rosemary plant tender stem of gathering and leaf natural shade are done;
(2) vapor distillation is carried out 1 ~ 3 hour to naturally shady dry Herba Rosmarini Officinalis, obtain rosemary ethereal oil and residue;
(3) pulverize residue after extraction quintessence oil, add 50% alcoholic solution of 8 ~ 12 times (relatively dry Herba Rosmarini Officinaliss), then ultrasonic assistant extracts 1 ~ 3 time, carries out centrifugalize, obtain lixiviating solution after extraction, merges lixiviating solution;
(4) desolventing technology is carried out to lixiviating solution, in lixiviating solution, add 1 ~ 10% active hargil, under 50 ~ 100 DEG C of conditions, stir maintenance 20 ~ 50 min, remove active hargil and obtain the lixiviating solution that decolours;
(5) decolouring lixiviating solution is carried out vacuum concentration, volume concentration to 10 ~ 20%, separate out and precipitate in a large number;
(6) concentrated solution centrifugal 10 ~ 20 min under 4000 r/min conditions are precipitated and aqueous portion;
(7) respectively precipitation and aqueous portion are carried out vacuum drying, obtain fat-soluble antioxidant and water soluble antioxidant.
This process equipment is simple, small investment, and decolorizing effect is remarkable, is applicable to suitability for industrialized production.Products obtained therefrom cost is low, and yield is high, fat-soluble and good water solubility, of many uses.
Detailed description of the invention
Be specifically described the present invention below by embodiment, following examples, only for the present invention is further described, can not be interpreted as limiting the scope of the present invention.
Embodiment 1: a kind ofly extract fat-soluble and method that is water soluble antioxidant in Herba Rosmarini Officinalis, comprises the following steps:
(1) raw material is the Herba Rosmarini Officinalis that Minquan County, Henan Province produces, and the rosemary plant tender stem of gathering and leaf natural shade is done, then gets 100 g vapor distillation 3 hours, obtain rosemary ethereal oil and residue; Pulverize residue after extraction quintessence oil, add 50% alcoholic solution of 10 times (relatively dry Herba Rosmarini Officinaliss), then ultrasonic assistant extracts 2 times, merges the lixiviating solution that two times centrifugal obtains; In lixiviating solution, add 4% active hargil, under 55 DEG C of conditions, stir maintenance 30 min, remove active hargil and obtain the lixiviating solution that decolours; Decolouring lixiviating solution is carried out vacuum concentration, volume concentration to 10%, separate out and precipitate in a large number; Concentrated solution centrifugal 15 min under 4000 r/min conditions are precipitated and aqueous portion; Respectively precipitation and aqueous portion are carried out vacuum drying, obtain fat-soluble antioxidant carnosic acid 5.64 g and water soluble antioxidant 9.78 g, yield is respectively 5.64% and 9.78%, and total antioxidation agent yield is 15.42%.
Embodiment 2 ~ 5:
The extracting method of the present embodiment is substantially the same manner as Example 1, and difference is: active soil addition being changed by 4% is 2%(example 2), 6%(example 3), 8%(example 4) and, 10%(example 5).Example 1 ~ 5 is the impact of the active hargil of different proportion on the elimination of pigment and finished product yield is described.In calculated example 2 ~ 5 antioxidant yield and compare with example 1, result is as table 1.
The elimination of table 1 different activities hargil addition on pigment, the impact of product interest rate
| Active hargil addition (%) | Water soluble antioxidant yield (%) | Fat-soluble antioxidant interest rate (%) | Decolorizing effect and product colour | Total antioxidation yield (%) |
| 2% | 10.02 | 6.17 | Difference, light green/yellow green | 16.19 |
| 6% | 9.34 | 5.69 | Generally, light green/faint yellow | 15.03 |
| 8% | 8.86 | 5.36 | Good, light green/yellow | 14.22 |
| 10% | 8.37 | 4.81 | Good, light green/dark yellow | 13.18 |
| 4% | 9.78 | 5.94 | Generally, light green/yellow green | 15.72 |
Claims (3)
1. in Herba Rosmarini Officinalis, extract a fat-soluble and method that is water soluble antioxidant, it is characterized in that comprising the following steps: the rosemary plant tender stem of gathering and leaf natural shade are done by (1); (2) vapor distillation is carried out 1 ~ 3 hour to naturally shady dry Herba Rosmarini Officinalis, obtain rosemary ethereal oil and residue; (3) pulverize residue after extraction quintessence oil, add 50% alcoholic solution of 8 ~ 12 times (relatively dry Herba Rosmarini Officinaliss), then ultrasonic assistant extracts 1 ~ 3 time, carries out centrifugalize, obtain lixiviating solution after extraction, merges lixiviating solution; (4) desolventing technology is carried out to lixiviating solution, in lixiviating solution, add 1 ~ 10% active hargil, under 50 ~ 100 DEG C of conditions, stir maintenance 20 ~ 50 min, remove active hargil and obtain the lixiviating solution that decolours; (5) decolouring lixiviating solution is carried out vacuum concentration, volume concentration to 10 ~ 20%, separate out precipitation; (6) concentrated solution centrifugal 10 ~ 20 min under 4000 r/min conditions are precipitated and aqueous portion; (7) respectively precipitation and aqueous portion are carried out vacuum drying, obtain fat-soluble antioxidant and water soluble antioxidant.
2. according to the preparation method described in claim 1, it is characterized in that, in described step (4), carry out desolventing technology to lixiviating solution, depigmenting agent used is active hargil.
3. according to the preparation method described in claim 1, it is characterized in that, in described step (4), to lixiviating solution desolventing technology condition be: active hargil amount is 1 ~ 10%, bleaching temperature is 30 ~ 100 DEG C, and the time is 20 ~ 50 min.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410786659.4A CN104490994A (en) | 2014-12-18 | 2014-12-18 | Method for extracting lipid-soluble and water-soluble antioxidant from rosemary |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410786659.4A CN104490994A (en) | 2014-12-18 | 2014-12-18 | Method for extracting lipid-soluble and water-soluble antioxidant from rosemary |
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| CN104490994A true CN104490994A (en) | 2015-04-08 |
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| CN201410786659.4A Pending CN104490994A (en) | 2014-12-18 | 2014-12-18 | Method for extracting lipid-soluble and water-soluble antioxidant from rosemary |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106831403A (en) * | 2017-01-18 | 2017-06-13 | 河南佳尚农业科技发展有限公司 | It is a kind of that fat-soluble and water soluble antioxidant method is extracted from rosemary |
| WO2017148180A1 (en) * | 2016-03-02 | 2017-09-08 | 禹州市天源生物科技有限公司 | Rosemary moisturizing solution and manufacturing method therefor |
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| WO2017148180A1 (en) * | 2016-03-02 | 2017-09-08 | 禹州市天源生物科技有限公司 | Rosemary moisturizing solution and manufacturing method therefor |
| CN106831403A (en) * | 2017-01-18 | 2017-06-13 | 河南佳尚农业科技发展有限公司 | It is a kind of that fat-soluble and water soluble antioxidant method is extracted from rosemary |
| CN109161443A (en) * | 2017-11-13 | 2019-01-08 | 湖南诺泽生物科技有限公司 | A kind of fresh rosemary processing method |
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| CN111727032B (en) * | 2018-02-15 | 2023-09-01 | 罗伯特公司 | Method for obtaining rosmarinic acid-enriched extract from fresh plant material |
| CN108783159A (en) * | 2018-06-29 | 2018-11-13 | 贵州省现代农业发展研究所 | A kind of Pitaya Flower Healthy Drink and preparation method thereof |
| CN108783157A (en) * | 2018-06-29 | 2018-11-13 | 贵州省现代农业发展研究所 | A kind of dragon fruit rose flower beverage and preparation method thereof |
| CN109536171A (en) * | 2019-01-04 | 2019-03-29 | 湖北瑞晟生物有限责任公司 | A kind of extraction process of water solubility rosemary antioxidant |
| CN110664635A (en) * | 2019-11-05 | 2020-01-10 | 湖北创界生物科技有限公司 | Moisturizing and hydrating mask composition, mask and preparation method of mask |
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| CN111869810A (en) * | 2020-07-23 | 2020-11-03 | 贵州省蚕业研究所(贵州省辣椒研究所) | Natural antioxidant and preparation method thereof |
| CN114315566A (en) * | 2021-12-13 | 2022-04-12 | 绿谷植源(清远)生物科技有限公司 | Method for simultaneously preparing rosemary oil soluble and fat soluble antioxidant |
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