CN112471484A - Litsea cubeba powder oil and preparation method thereof - Google Patents
Litsea cubeba powder oil and preparation method thereof Download PDFInfo
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- CN112471484A CN112471484A CN202011365324.7A CN202011365324A CN112471484A CN 112471484 A CN112471484 A CN 112471484A CN 202011365324 A CN202011365324 A CN 202011365324A CN 112471484 A CN112471484 A CN 112471484A
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- litsea cubeba
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- 240000002262 Litsea cubeba Species 0.000 title claims abstract description 30
- 235000012854 Litsea cubeba Nutrition 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000843 powder Substances 0.000 title claims abstract description 18
- 239000003921 oil Substances 0.000 claims abstract description 58
- 238000000034 method Methods 0.000 claims abstract description 37
- 239000000463 material Substances 0.000 claims abstract description 36
- 239000001289 litsea cubeba fruit oil Substances 0.000 claims abstract description 30
- 108010010803 Gelatin Proteins 0.000 claims abstract description 14
- 229920000881 Modified starch Polymers 0.000 claims abstract description 14
- 229920000159 gelatin Polymers 0.000 claims abstract description 14
- 239000008273 gelatin Substances 0.000 claims abstract description 14
- 235000019322 gelatine Nutrition 0.000 claims abstract description 14
- 235000011852 gelatine desserts Nutrition 0.000 claims abstract description 14
- 240000003183 Manihot esculenta Species 0.000 claims abstract description 12
- 235000016735 Manihot esculenta subsp esculenta Nutrition 0.000 claims abstract description 12
- 239000008120 corn starch Substances 0.000 claims abstract description 12
- 235000020357 syrup Nutrition 0.000 claims abstract description 12
- 239000006188 syrup Substances 0.000 claims abstract description 12
- 239000004368 Modified starch Substances 0.000 claims abstract description 11
- 235000019426 modified starch Nutrition 0.000 claims abstract description 11
- 229920002261 Corn starch Polymers 0.000 claims abstract description 9
- 239000004519 grease Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims description 25
- 239000003094 microcapsule Substances 0.000 claims description 21
- 239000011259 mixed solution Substances 0.000 claims description 20
- 239000011550 stock solution Substances 0.000 claims description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 8
- 230000001804 emulsifying effect Effects 0.000 claims description 8
- 238000009777 vacuum freeze-drying Methods 0.000 claims description 8
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims description 5
- 238000004132 cross linking Methods 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 5
- 239000012154 double-distilled water Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 239000002537 cosmetic Substances 0.000 abstract description 5
- 239000003814 drug Substances 0.000 abstract description 5
- 229940079593 drug Drugs 0.000 abstract description 5
- 150000001875 compounds Chemical class 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 230000007547 defect Effects 0.000 abstract 1
- 230000006866 deterioration Effects 0.000 abstract 1
- 235000013305 food Nutrition 0.000 abstract 1
- 239000000047 product Substances 0.000 description 13
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 10
- 239000011162 core material Substances 0.000 description 8
- 239000000341 volatile oil Substances 0.000 description 7
- 241000196324 Embryophyta Species 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 239000003208 petroleum Substances 0.000 description 5
- 238000001694 spray drying Methods 0.000 description 5
- 239000004278 EU approved seasoning Substances 0.000 description 4
- 235000011194 food seasoning agent Nutrition 0.000 description 4
- 239000002304 perfume Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 230000001953 sensory effect Effects 0.000 description 3
- 238000000967 suction filtration Methods 0.000 description 3
- GLZPCOQZEFWAFX-UHFFFAOYSA-N Geraniol Chemical compound CC(C)=CCCC(C)=CCO GLZPCOQZEFWAFX-UHFFFAOYSA-N 0.000 description 2
- 238000012695 Interfacial polymerization Methods 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- CRPUJAZIXJMDBK-UHFFFAOYSA-N camphene Chemical compound C1CC2C(=C)C(C)(C)C1C2 CRPUJAZIXJMDBK-UHFFFAOYSA-N 0.000 description 2
- 238000005189 flocculation Methods 0.000 description 2
- 230000016615 flocculation Effects 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- XMGQYMWWDOXHJM-UHFFFAOYSA-N limonene Chemical compound CC(=C)C1CCC(C)=CC1 XMGQYMWWDOXHJM-UHFFFAOYSA-N 0.000 description 2
- CDOSHBSSFJOMGT-UHFFFAOYSA-N linalool Chemical compound CC(C)=CCCC(C)(O)C=C CDOSHBSSFJOMGT-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000001490 (3R)-3,7-dimethylocta-1,6-dien-3-ol Substances 0.000 description 1
- CDOSHBSSFJOMGT-JTQLQIEISA-N (R)-linalool Natural products CC(C)=CCC[C@@](C)(O)C=C CDOSHBSSFJOMGT-JTQLQIEISA-N 0.000 description 1
- WTEVQBCEXWBHNA-UHFFFAOYSA-N Citral Natural products CC(C)=CCCC(C)=CC=O WTEVQBCEXWBHNA-UHFFFAOYSA-N 0.000 description 1
- 235000005979 Citrus limon Nutrition 0.000 description 1
- 244000131522 Citrus pyriformis Species 0.000 description 1
- 241000255925 Diptera Species 0.000 description 1
- 239000001856 Ethyl cellulose Substances 0.000 description 1
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 1
- 239000005792 Geraniol Substances 0.000 description 1
- GLZPCOQZEFWAFX-YFHOEESVSA-N Geraniol Natural products CC(C)=CCC\C(C)=C/CO GLZPCOQZEFWAFX-YFHOEESVSA-N 0.000 description 1
- 229920002153 Hydroxypropyl cellulose Polymers 0.000 description 1
- 239000005913 Maltodextrin Substances 0.000 description 1
- 229920002774 Maltodextrin Polymers 0.000 description 1
- PXRCIOIWVGAZEP-UHFFFAOYSA-N Primaeres Camphenhydrat Natural products C1CC2C(O)(C)C(C)(C)C1C2 PXRCIOIWVGAZEP-UHFFFAOYSA-N 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 235000010489 acacia gum Nutrition 0.000 description 1
- 239000001785 acacia senegal l. willd gum Substances 0.000 description 1
- XCPQUQHBVVXMRQ-UHFFFAOYSA-N alpha-Fenchene Natural products C1CC2C(=C)CC1C2(C)C XCPQUQHBVVXMRQ-UHFFFAOYSA-N 0.000 description 1
- JZQOJFLIJNRDHK-CMDGGOBGSA-N alpha-irone Chemical compound CC1CC=C(C)C(\C=C\C(C)=O)C1(C)C JZQOJFLIJNRDHK-CMDGGOBGSA-N 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 229930006739 camphene Natural products 0.000 description 1
- ZYPYEBYNXWUCEA-UHFFFAOYSA-N camphenilone Natural products C1CC2C(=O)C(C)(C)C1C2 ZYPYEBYNXWUCEA-UHFFFAOYSA-N 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229940043350 citral Drugs 0.000 description 1
- 238000005354 coacervation Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 235000019325 ethyl cellulose Nutrition 0.000 description 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- WTEVQBCEXWBHNA-JXMROGBWSA-N geranial Chemical compound CC(C)=CCC\C(C)=C\C=O WTEVQBCEXWBHNA-JXMROGBWSA-N 0.000 description 1
- 229940113087 geraniol Drugs 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 239000001863 hydroxypropyl cellulose Substances 0.000 description 1
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 229930002839 ionone Natural products 0.000 description 1
- 150000002499 ionone derivatives Chemical class 0.000 description 1
- 230000002147 killing effect Effects 0.000 description 1
- 229940087305 limonene Drugs 0.000 description 1
- 235000001510 limonene Nutrition 0.000 description 1
- 229930007744 linalool Natural products 0.000 description 1
- 229940035034 maltodextrin Drugs 0.000 description 1
- 238000005360 mashing Methods 0.000 description 1
- JPTOCTSNXXKSSN-UHFFFAOYSA-N methylheptenone Chemical compound CCCC=CC(=O)CC JPTOCTSNXXKSSN-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 230000001151 other effect Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001846 repelling effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000013268 sustained release Methods 0.000 description 1
- 239000012730 sustained-release form Substances 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- MWOOGOJBHIARFG-UHFFFAOYSA-N vanillin Chemical compound COC1=CC(C=O)=CC=C1O MWOOGOJBHIARFG-UHFFFAOYSA-N 0.000 description 1
- FGQOOHJZONJGDT-UHFFFAOYSA-N vanillin Natural products COC1=CC(O)=CC(C=O)=C1 FGQOOHJZONJGDT-UHFFFAOYSA-N 0.000 description 1
- 235000012141 vanillin Nutrition 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- 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
- A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
- A23L27/20—Synthetic spices, flavouring agents or condiments
- A23L27/202—Aliphatic compounds
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
- A23D9/007—Other edible oils or fats, e.g. shortenings, cooking oils characterised by ingredients other than fatty acid triglycerides
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
- A23D9/02—Other edible oils or fats, e.g. shortenings, cooking oils characterised by the production or working-up
- A23D9/04—Working-up
-
- 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)
- A61K36/54—Lauraceae (Laurel family), e.g. cinnamon or sassafras
-
- 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
-
- 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
-
- 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
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
- A61K8/732—Starch; Amylose; Amylopectin; Derivatives thereof
-
- 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
- A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
- A61K8/922—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
-
- 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
- A61K9/5036—Polysaccharides, e.g. gums, alginate; Cyclodextrin
-
- 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
Abstract
The invention discloses litsea cubeba powdered oil and a preparation method thereof, the method creatively selects cassava modified starch, corn starch syrup and gelatin as a compound wall material through experimental comparison, and the compound wall material has good film forming property, high biological safety, relatively low cost and great industrial value. The process makes up the defects of unstable, volatile, easy oxidation and deterioration of the litsea cubeba oil, prolongs the shelf life to 3 years and widens the application field of the litsea cubeba oil. Meanwhile, the process is simple to operate and high in embedding rate, and the microencapsulated litsea cubeba oil powder grease prepared by the process has the embedding rate as high as 92% and the oil content as high as 50%. The obtained powdered oil has good fluidity and solubility and excellent slow release effect, and the effective slow release time of the powdered oil in the air can reach 2-3 months. No harmful substance is added in the preparation process, and the produced litsea cubeba powdered oil can be directly applied to the fields of cosmetics, medicines, foods and the like.
Description
Technical Field
The invention relates to litsea cubeba powdered oil and a preparation method thereof, belonging to the technical field of plant essential oil slow release.
Background
The Litsea cubeba oil is natural essential oil extracted from fresh Litsea cubeba fruit, has strong lemon fragrance, is yellowish, and contains main chemical components such as citral, limonene, methylheptenone, linalool, geraniol, vanillin, camphene, etc. The natural perfume belongs to one of natural perfumes, is also a main source of synthetic perfumes such as ionone, irone and the like, has excellent mosquito repelling and killing, anti-oxidation, bacteriostasis and other effects, and can be directly applied to various fields such as cosmetics, medicines, synthetic perfumes, seasonings and the like.
However, most of plant essential oils including the litsea cubeba oil have instability, the natural litsea cubeba oil is easily influenced by external conditions and is sensitive to heat and light, the natural litsea cubeba oil is difficult to store due to strong volatility, fast release, easy oxidation and the like, and the direct addition and use of the natural litsea cubeba oil cannot meet the requirements of people, so that the application range of the natural litsea cubeba oil in partial fields is limited, and the application of terminal products of the natural litsea cubeba oil is restricted. At present, the plant essential oil slow release technology becomes a main international approach for solving the problem, and microencapsulation of the plant essential oil into solid powdered oil is one of the main methods for slow release of the plant essential oil. The preparation method of the microcapsule mainly comprises a complex coacervation method, a spray drying method, a single flocculation method, an in-situ polymerization method, an interfacial polymerization method and the like. Different methods, selection of different wall materials and determination of reaction conditions in the preparation process of the essential oil microcapsule directly influence the embedding rate and the sustained-release effect of the product. For example, when the microcapsule is prepared by a spray drying method, the core material is in high-temperature airflow, some active substances are easy to inactivate, the application range of the microcapsule is limited, the solvent of the microcapsule prepared by the method is quick to evaporate, the capsule wall of the microcapsule is easy to crack, and the compactness needs to be improved; the microcapsule prepared by the single flocculation method has larger grain diameter and narrower application range; when the microcapsule is prepared by the interfacial polymerization method, the performance of the microcapsule in a dispersion state is greatly influenced, and factors such as stirring speed, solution viscosity, the types and the amounts of the emulsifier and the stabilizer can greatly influence the properties of the microcapsule and are difficult to control. Therefore, the preparation method of the litsea cubeba powder oil with high benefit and high quality is to be researched and found by people.
Chinese patent application 201210140302.X discloses a litsea cubeba oil mildew-proof and moth-proof slow-release microcapsule and a preparation method thereof, wherein ethyl cellulose, high-substituted hydroxypropyl cellulose, Arabic gum and maltodextrin are used as wall materials, and the preparation method mainly comprises the steps of emulsification, homogenization, drying and the like. Although the preparation method is simple, the spray drying method is adopted to dry the homogenized litsea cubeba oil emulsion, and the product is in high-temperature airflow in the process, so that partial active substances in litsea cubeba oil are inactivated and a few wall materials are cracked, and the quality of the product is influenced. And the cost of the selected wall material is relatively high. .
Disclosure of Invention
In order to solve the problems, the invention aims to provide litsea cubeba powdered oil and a preparation method thereof. The method selects cassava modified starch, corn starch syrup and gelatin as compound wall materials, is green and healthy, has low cost and can be industrially produced; meanwhile, vacuum freezing is adopted, so that the damage of high-temperature airflow in spray drying to product components is avoided. The yield of the obtained litsea cubeba powdered oil is as high as 92 percent, the product quality meets the national standard, the storage period is longer, the slow release effect is stable, and the litsea cubeba powdered oil can be directly applied to the fields of cosmetics, medicines, seasonings and the like.
The technical scheme of the invention is as follows:
the invention discloses a preparation method of litsea cubeba powdered oil, which comprises the following steps:
(1) mixing the cassava modified starch and the corn starch syrup, adding 7-10 times of double distilled water into the mixture, and stirring and dissolving at 65-75 ℃ to obtain a wall material stock solution A;
(2) adding gelatin into water for soaking, heating to dissolve the gelatin to obtain wall material stock solution B with the mass fraction of 1-3%, and standing for 3-4 h for later use;
(3) cooling to reduce the temperature of the wall material stock solution A prepared in the step (1) to about 25 ℃, and adding core litsea cubeba oil to prepare a mixed solution C;
(4) stirring the mixed solution C prepared in the step (3), controlling the stirring temperature, stirring, emulsifying and dispersing for 10min, adding the wall material stock solution B prepared in the step (2) into the dispersion liquid in the stirrer, keeping the temperature unchanged, and continuing homogenizing and emulsifying for 15 min;
(5) adding the emulsified mixed solution obtained in the step (4) into a high-pressure homogenizer, and homogenizing for 2-3 times under 30-35 MPa;
(6) placing the homogenized mixed solution obtained in the step (5) in an ice bath, rapidly cooling to below 10 ℃, adding 25% glutaraldehyde, dropwise adding 10% NaOH solution to adjust the pH of the system to 9-10, adding a stirrer, controlling the rotation speed of the stirrer to be 300r/min, performing crosslinking and curing for 60min, and standing for 10-12 h to completely settle the microcapsules;
(7) and (4) carrying out vacuum freeze drying on the product obtained in the step (6) to obtain the litsea cubeba powdered oil.
Further, the mass ratio of the cassava modified starch to the corn starch syrup in the step (1) is 0.7: 1.
Further, the mass ratio of the core litsea cubeba oil to the wall material prepared in the step (1) is 1: 1-6.
Further, the solute mass of the wall material raw liquid B prepared in the step (2) and the wall material raw liquid A prepared in the step (1) is 2: 1.
Further, in the process of the step (7), the drying method is vacuum freeze drying.
Further, the stirring speed in the step (4) is 1200-1600 r/min.
Further, the stirring temperature in the step (4) is 30 ℃.
Further, the concentration of the gelatin solution in the step (2) is 2%.
The invention also comprises the litsea cubeba powder grease prepared by the method.
The invention has the following beneficial effects:
the litsea cubeba powder oil wall material prepared by the process technology is green and healthy and has lower cost, and the competitiveness of industrial products is improved. The microcapsule embedding rate can reach 92%, the oil content can reach 50%, and the yield is higher than that of most existing processes. The natural slow release time of the obtained litsea cubeba oil powder grease can reach 2-3 months, the quality guarantee period can reach 3 years, and the litsea cubeba oil powder grease has a good application prospect in the fields of cosmetics, medicines, seasonings and the like. Meanwhile, the method abandons a common spray drying method in the drying process and selects vacuum freeze drying, thereby avoiding the damage of high-temperature airflow to product components in the drying process and ensuring that each active component in the litsea cubeba oil is protected to the maximum extent.
Detailed Description
In order to better understand the present invention, the following examples are further provided for illustration, which are only used for explaining the present invention and do not limit the present invention in any way.
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art, and the raw materials used are commercially available products.
1. Modified cassava starch: influence of corn starch syrup quality ratio on preparation of powdered oil
Examples 1 to 6
1) Mixing cassava modified starch and corn starch syrup according to the ratio of 0.7:1, adding 7 times of double distilled water into the mixture, and stirring and dissolving at 70 ℃ to obtain a wall material raw solution A; 2) adding gelatin into water, soaking, heating to dissolve the gelatin to obtain wall material stock solution B with mass fraction of 2%, and standing for 4 h; 3) cooling to reduce the temperature of the wall material stock solution A to about 25 ℃, and respectively adding core litsea cubeba oil according to the proportion shown in the following table to prepare a mixed solution C; 4) adding the mixed solution C prepared in the step (3) into a stirrer, controlling the temperature to be 30 ℃, controlling the stirring speed of the stirrer to be 1400r/min, stirring, emulsifying and dispersing for 10min, adding the wall material stock solution B prepared in the step (2) into the dispersion liquid in the stirrer, keeping the temperature unchanged, and continuing homogenizing and emulsifying for 15 min; 5) adding the emulsified mixed solution obtained in the step (4) into a high-pressure homogenizer, and homogenizing for 3 times under 35 MPa; 6) and (3) placing the homogenized mixed solution obtained in the step (5) in an ice bath, rapidly cooling to below 10 ℃, adding 25% glutaraldehyde, dropwise adding 10% NaOH solution to adjust the pH of the system to 9-10, adding a stirrer, controlling the rotation speed of the stirrer to be 300r/min, performing crosslinking and curing for 60min, and standing for 10h to completely settle the microcapsules. 7) And (4) carrying out vacuum freeze drying on the product obtained in the step (6) to obtain the litsea cubeba powdered oil.
The test results are shown in the table below, when the mass ratio of the core litsea cubeba oil to the wall material prepared from the cassava modified starch and the corn starch syrup in the step 1) is 1:1-1:6, stable litsea cubeba oil powder grease can be obtained. Meanwhile, under the condition of comprehensively considering the embedding rate and the oil content, the optimal preparation condition is that the mass ratio of the core litsea cubeba oil to the wall material prepared from the cassava modified starch and the corn starch syrup in the step 1) is 1: 3.
2. Influence of stirring temperature on preparation of powdered oil
Examples 7 to 11
1) Mixing cassava modified starch and corn starch syrup according to a ratio of 0.7:1, adding 7 times of double distilled water into the mixture, and stirring and dissolving at 70 ℃ to obtain a wall material stock solution A; 2) adding gelatin into water, soaking, heating to dissolve the gelatin to obtain wall material stock solution B with mass fraction of 2%, and standing for 4 h; 3) cooling to reduce the temperature of the wall material stock solution A to about 25 ℃, and adding the core litsea cubeba oil according to the optimal proportion obtained in the above cases to prepare a mixed solution C; 4) adding the mixed solution C prepared in the step (3) into a stirrer, controlling the temperature to be respectively shown in the following table, controlling the stirring speed of the stirrer to be 1400r/min, stirring, emulsifying and dispersing for 10min, adding the wall material stock solution B prepared in the step (2) into the dispersion liquid in the stirrer, keeping the temperature unchanged, and continuing homogenizing and emulsifying for 15 min; 5) adding the emulsified mixed solution obtained in the step (4) into a high-pressure homogenizer, and homogenizing for 3 times under 35 MPa; 6) placing the homogenized mixed solution obtained in the step (5) in an ice bath, rapidly cooling to below 10 ℃, adding 25% glutaraldehyde, dropwise adding 10% NaOH solution to adjust the pH of the system to 9-10, adding a stirrer, controlling the rotation speed of the stirrer to be 300r/min, performing crosslinking and curing for 60min, and standing for 10h to completely settle the microcapsules; 7) and (4) carrying out vacuum freeze drying on the product obtained in the step (6) to obtain the litsea cubeba powdered oil.
The test results are shown in the following table, which shows that the optimum production conditions are obtained when the stirring temperature in step 4) is 30 ℃ in consideration of the embedding rate and the oil content.
3. Influence of stirring speed on preparation of powdered oil
Examples 12 to 15
1) Mixing cassava modified starch and corn starch syrup according to a ratio of 0.7:1, adding 7 times of double distilled water into the mixture, and stirring and dissolving at 70 ℃ to obtain a wall material stock solution A; 2) adding gelatin into water, soaking, heating to dissolve the gelatin to obtain wall material stock solution B with mass fraction of 2%, and standing for 4 h; 3) when the temperature is reduced to reduce the temperature of the wall material stock solution A to about 25 ℃, adding the core litsea cubeba oil according to the optimal proportion obtained in the cases 1 to 6 to prepare a mixed solution C; 4) adding the mixed solution C prepared in the step (3) into a stirrer, controlling the temperature to be the optimal temperature of 30 ℃ obtained in the case 7-11, respectively controlling the stirring speed of the stirrer to be 800-; 5) adding the emulsified mixed solution obtained in the step (4) into a high-pressure homogenizer, and homogenizing for 3 times under 35 MPa; 6) placing the homogenized mixed solution obtained in the step (5) in an ice bath, rapidly cooling to below 10 ℃, adding 25% glutaraldehyde, dropwise adding 10% NaOH solution to adjust the pH of the system to 9-10, adding a stirrer, controlling the rotation speed of the stirrer to be 300r/min, performing crosslinking and curing for 60min, and standing for 10h to completely settle the microcapsules; 7) and (4) carrying out vacuum freeze drying on the product obtained in the step (6) to obtain the litsea cubeba powdered oil.
The test results are shown in the following table, which shows that the optimum production conditions are achieved when the stirring rate in step 4) is around 1400r/min, taking into account the embedding rate and the oil content.
The method for measuring the embedding rate and the oil content of the powdered oil in the experimental result is as follows:
1. determination of oil embedding rate of litsea cubeba oil powder
The embedding rate of the powdered oil is the proportion of the oil embedded by the wall material to the total oil, and is an important index for evaluating the microencapsulation efficiency, and the calculation formula is as follows:
embedding rate 1- (surface oil content/total oil content) x 100% ═ 1-surface oil content (r)
The method for measuring the oil content of the surface comprises the following steps: the surface oil content is determined by petroleum ether extraction method, weighing 2G (m) litsea cubeba oil powder oil microcapsule, placing in a wide-mouth bottle, adding 40mL petroleum ether, leaching under gentle shaking and stirring for 2min, then immediately leaching with G3 sand core, performing suction filtration with a bucket, washing the filter residue with 25mL petroleum ether for 1min, immediately performing suction filtration, finally transferring the filtrate to a cone bottle (m1) with constant weight, evaporating to dryness by a rotary evaporator and recovering petroleum ether, and drying the cone bottle with constant weight (m2) in a vacuum drying oven at 65 ℃.
Surface oil content [ (m2-m1)/m ] x 100%
m represents the weight (g) of the weighed powdered oil.
m 1-constant weight of conical bottle (g)
m2- -oil and Erlenmeyer flask quality (g) after drying to constant weight
Substituting the formula II into the formula I to obtain the surface oil content.
2. Determination of oil content of litsea cubeba oil powder oil
And (3) putting 20g of the powdered oil prepared in the embodiment into a yarn bag, putting the yarn bag into the same space, taking out 1g of microcapsule sample after one week, mashing the microcapsule sample by using a mortar, extracting litsea cubeba oil in the microcapsule by using petroleum ether for multiple times, carrying out suction filtration, drying filter residue for 2 hours at 50 ℃, cooling the filter residue to room temperature, measuring the weight of the filter residue, and dividing the weight by 1g of the sample to obtain the oil content of the powdered oil.
Sensory test of oil and fat was conducted on the litsea cubeba powder obtained under the optimum preparation conditions (example 15)
The test results are as follows
Table 1 shows sensory test of the obtained Litsea cubeba powder oil
The litsea cubeba powder oil prepared by the process technology meets the national sensory index, physicochemical index and sanitary index of the powder oil, and can be directly applied to the fields of cosmetics, medicines, seasonings and the like.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (9)
1. A preparation method of litsea cubeba powder grease is characterized by comprising the following steps: the method comprises the following steps:
(1) mixing the cassava modified starch and the corn starch syrup, adding 7-10 times of double distilled water into the mixture, and stirring and dissolving at 65-75 ℃ to obtain a wall material stock solution A;
(2) adding gelatin into water for soaking, heating to dissolve the gelatin to obtain wall material stock solution B with the mass fraction of 1-3%, and standing for 3-4 h for later use;
(3) cooling to reduce the temperature of the wall material stock solution A prepared in the step (1) to about 25 ℃, and adding core litsea cubeba oil to prepare a mixed solution C;
(4) stirring the mixed solution C prepared in the step (3) at a certain temperature, stirring, emulsifying and dispersing for 10min, adding the wall material stock solution B prepared in the step (2) into the dispersion solution in the stirrer, keeping the temperature unchanged, and continuing homogenizing and emulsifying for 15 min;
(5) adding the emulsified mixed solution obtained in the step (4) into a high-pressure homogenizer, and homogenizing for 2-3 times under 30-35 MPa;
(6) placing the homogenized mixed solution obtained in the step (5) in an ice bath, rapidly cooling to below 10 ℃, adding 25% glutaraldehyde, dropwise adding 10% NaOH solution to adjust the pH of the system to 9-10, adding a stirrer, controlling the rotation speed of the stirrer to be 300r/min, performing crosslinking and curing for 60min, and standing for 10-12 h to completely settle the microcapsules;
(7) and (4) carrying out vacuum freeze drying on the product obtained in the step (6) to obtain the litsea cubeba powdered oil.
2. The method for preparing the litsea cubeba powdered oil according to claim 1, wherein the mass ratio of the cassava modified starch to the corn starch syrup in the step (1) is 0.7: 1.
3. The method for preparing the litsea cubeba powdered oil according to claim 2, which is characterized by comprising the following steps: the mass ratio of the core litsea cubeba oil to the wall material prepared in the step (1) is 1: 1-6.
4. The method for preparing the litsea cubeba powdered oil according to claim 3, which is characterized by comprising the following steps: the solute mass of the wall material stock solution B prepared in the step (2) and the wall material stock solution A prepared in the step (1) is 2: 1.
5. The method for preparing the litsea cubeba powdered oil according to claim 1, which is characterized by comprising the following steps: in the step (7), the drying method is vacuum freeze drying.
6. The method for preparing the litsea cubeba powdered oil according to claim 5, which is characterized by comprising the following steps: the stirring speed in the step (4) is 1200-1600 r/min.
7. The method for preparing the litsea cubeba powdered oil according to claim 5, which is characterized by comprising the following steps: the stirring temperature in the step (4) is 20-40 ℃.
8. The method for preparing the litsea cubeba powdered oil according to claim 6, which is characterized by comprising the following steps: the concentration of the gelatin solution in the step (2) is 2%.
9. The litsea cubeba powder grease is characterized in that: prepared by the process of claims 1-7.
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