CN113122392A - Compound traditional Chinese medicine herbal essential oil and application thereof - Google Patents
Compound traditional Chinese medicine herbal essential oil and application thereof Download PDFInfo
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- CN113122392A CN113122392A CN202110394210.3A CN202110394210A CN113122392A CN 113122392 A CN113122392 A CN 113122392A CN 202110394210 A CN202110394210 A CN 202110394210A CN 113122392 A CN113122392 A CN 113122392A
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- 239000000341 volatile oil Substances 0.000 title claims abstract description 53
- 239000003814 drug Substances 0.000 title claims abstract description 33
- 150000001875 compounds Chemical class 0.000 title claims abstract description 30
- 239000002994 raw material Substances 0.000 claims abstract description 79
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 67
- 239000012528 membrane Substances 0.000 claims abstract description 61
- 108090000790 Enzymes Proteins 0.000 claims abstract description 26
- 102000004190 Enzymes Human genes 0.000 claims abstract description 26
- 238000000926 separation method Methods 0.000 claims abstract description 25
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 235000006679 Mentha X verticillata Nutrition 0.000 claims abstract description 8
- 235000002899 Mentha suaveolens Nutrition 0.000 claims abstract description 8
- 235000001636 Mentha x rotundifolia Nutrition 0.000 claims abstract description 8
- 241000951473 Schizonepeta Species 0.000 claims abstract description 8
- 239000012530 fluid Substances 0.000 claims abstract description 7
- 239000003921 oil Substances 0.000 claims abstract description 7
- 210000004379 membrane Anatomy 0.000 claims description 53
- 238000004821 distillation Methods 0.000 claims description 44
- 238000002791 soaking Methods 0.000 claims description 44
- 238000002156 mixing Methods 0.000 claims description 32
- 235000019476 oil-water mixture Nutrition 0.000 claims description 28
- 229940088598 enzyme Drugs 0.000 claims description 25
- 239000007788 liquid Substances 0.000 claims description 23
- 239000000203 mixture Substances 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 20
- 238000004140 cleaning Methods 0.000 claims description 19
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 14
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- 238000001914 filtration Methods 0.000 claims description 14
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- JLPULHDHAOZNQI-ZTIMHPMXSA-N 1-hexadecanoyl-2-(9Z,12Z-octadecadienoyl)-sn-glycero-3-phosphocholine Chemical compound 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 7
- 241001116389 Aloe Species 0.000 claims description 7
- 235000011399 aloe vera Nutrition 0.000 claims description 7
- 229940088990 ammonium stearate Drugs 0.000 claims description 7
- JPNZKPRONVOMLL-UHFFFAOYSA-N azane;octadecanoic acid Chemical compound [NH4+].CCCCCCCCCCCCCCCCCC([O-])=O JPNZKPRONVOMLL-UHFFFAOYSA-N 0.000 claims description 7
- 239000011521 glass Substances 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 7
- 229940083466 soybean lecithin Drugs 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 238000003815 supercritical carbon dioxide extraction Methods 0.000 claims description 7
- 239000011787 zinc oxide Substances 0.000 claims description 7
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- 238000005470 impregnation Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 235000019198 oils Nutrition 0.000 claims description 6
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- 102100032487 Beta-mannosidase Human genes 0.000 claims description 5
- 108010059892 Cellulase Proteins 0.000 claims description 5
- 235000013162 Cocos nucifera Nutrition 0.000 claims description 5
- 244000060011 Cocos nucifera Species 0.000 claims description 5
- 108010055059 beta-Mannosidase Proteins 0.000 claims description 5
- 229940106157 cellulase Drugs 0.000 claims description 5
- PSLIMVZEAPALCD-UHFFFAOYSA-N ethanol;ethoxyethane Chemical compound CCO.CCOCC PSLIMVZEAPALCD-UHFFFAOYSA-N 0.000 claims description 5
- 229940059442 hemicellulase Drugs 0.000 claims description 5
- 108010002430 hemicellulase Proteins 0.000 claims description 5
- 229940085127 phytase Drugs 0.000 claims description 5
- 229920001721 polyimide Polymers 0.000 claims description 5
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 5
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 5
- 239000004642 Polyimide Substances 0.000 claims description 4
- 238000007605 air drying Methods 0.000 claims description 4
- 238000000643 oven drying Methods 0.000 claims description 4
- 239000002033 PVDF binder Substances 0.000 claims description 3
- 239000004698 Polyethylene Substances 0.000 claims description 3
- 229920000573 polyethylene Polymers 0.000 claims description 3
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 3
- 239000004695 Polyether sulfone Substances 0.000 claims description 2
- 238000000222 aromatherapy Methods 0.000 claims description 2
- 229940087559 grape seed Drugs 0.000 claims description 2
- 229920000747 poly(lactic acid) Polymers 0.000 claims description 2
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 2
- 229920006393 polyether sulfone Polymers 0.000 claims description 2
- 239000004626 polylactic acid Substances 0.000 claims description 2
- 244000061520 Angelica archangelica Species 0.000 claims 2
- 239000003905 agrochemical Substances 0.000 claims 1
- 230000003796 beauty Effects 0.000 claims 1
- 238000010276 construction Methods 0.000 claims 1
- 239000011148 porous material Substances 0.000 abstract description 2
- 230000003075 superhydrophobic effect Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 32
- 241000125175 Angelica Species 0.000 description 11
- 238000000605 extraction Methods 0.000 description 9
- 239000011259 mixed solution Substances 0.000 description 9
- 241000219095 Vitis Species 0.000 description 5
- 235000009754 Vitis X bourquina Nutrition 0.000 description 5
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- 235000014787 Vitis vinifera Nutrition 0.000 description 5
- 238000003860 storage Methods 0.000 description 4
- 241000196324 Embryophyta Species 0.000 description 3
- 125000003118 aryl group Chemical group 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
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- 238000007654 immersion Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002560 therapeutic procedure Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
-
- 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)
- A61K36/23—Apiaceae or Umbelliferae (Carrot family), e.g. dill, chervil, coriander or cumin
- A61K36/232—Angelica
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- A—HUMAN NECESSITIES
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- 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
- A61K36/284—Atractylodes
-
- 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
- A61K36/534—Mentha (mint)
-
- 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
- A61K36/538—Schizonepeta
-
- 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)
- A61K36/87—Vitaceae or Ampelidaceae (Vine or Grape family), e.g. wine grapes, muscadine or peppervine
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- 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)
- A61K36/88—Liliopsida (monocotyledons)
- A61K36/886—Aloeaceae (Aloe family), e.g. aloe vera
-
- 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)
- A61K36/88—Liliopsida (monocotyledons)
- A61K36/896—Liliaceae (Lily family), e.g. daylily, plantain lily, Hyacinth or narcissus
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P39/00—General protective or antinoxious agents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
- B01D17/0202—Separation of non-miscible liquids by ab- or adsorption
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/022—Refining
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/027—Recovery of volatiles by distillation or stripping
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- A—HUMAN NECESSITIES
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/19—Preparation or pretreatment of starting material involving fermentation using yeast, bacteria or both; enzymatic treatment
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- A—HUMAN NECESSITIES
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- 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 or 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
- A61K2236/37—Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction
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- Health & Medical Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Veterinary Medicine (AREA)
- Medicinal Chemistry (AREA)
- Public Health (AREA)
- General Health & Medical Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Pharmacology & Pharmacy (AREA)
- Botany (AREA)
- Medical Informatics (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Biotechnology (AREA)
- Epidemiology (AREA)
- Alternative & Traditional Medicine (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Wood Science & Technology (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Toxicology (AREA)
- General Chemical & Material Sciences (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
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- Thermal Sciences (AREA)
- Medicines Containing Plant Substances (AREA)
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Abstract
The invention provides compound traditional Chinese medicine herbal essential oil and application thereof, wherein the raw materials comprise 800 parts of schizonepeta, 750 parts of mint 550-; the mixed enzyme is adopted for treatment in a preparation process, so that the oil yield of the raw material is effectively improved; in addition, the oil-water separation process adopts the base membrane treated by the treatment fluid and the modified solution, a super-hydrophobic oleophilic layer can be formed on the surface and the inner pores of the base membrane, the essential oil can be quickly separated, and the preparation efficiency is high.
Description
Technical Field
The invention belongs to the technical field of essential oil, and particularly relates to compound traditional Chinese medicine herbal essential oil and application thereof.
Background
Essential oil is a volatile substance extracted from aromatic plants, has the characteristics of strong permeability, various biological activities and the like, and is a main raw material for improving various diseases in aromatherapy. Aromatic medicinal plants play an important role in relieving and improving plants.
The traditional Chinese medicine essential oil is prepared by using modern scientific and technological means in limited and precise aspects of planting and collecting raw materials, extracting and refining products and absorbing the essential oil, so that the efficacy of the traditional Chinese medicine essential oil is greatly improved, and the aim of 'pure natural herbal essence' is not violated. The Chinese medicinal essential oil is the combination of Chinese traditional medicine health preservation and western essential oil soul therapy, and plays the most deep role of the essential oil to human body.
However, the price of the traditional Chinese medicine herbal essential oil is always high due to the factors of low raw material cost, low extraction rate, low purity and the like, so that aiming at the problems, the invention provides the compound traditional Chinese medicine herbal essential oil which is prepared by compound extraction of a plurality of traditional Chinese medicine herbal raw materials, has the advantages of simple preparation process, high extraction rate and high purity, and provides a new technical direction for the development of the field of the traditional Chinese medicine herbal essential oil.
Disclosure of Invention
The first object of the present invention is to: providing a compound traditional Chinese medicine herbal essential oil;
the second object of the present invention is to: providing a mixed enzyme for extracting the essential oil of the compound traditional Chinese medicine;
the third object of the present invention is to: provides the application field of the compound traditional Chinese medicine herbal essential oil.
The invention is realized by the following technical scheme: the compound traditional Chinese medicine herbal essential oil comprises 800 parts by weight of schizonepeta herb, 750 parts by weight of mint, 700 parts by weight of angelica, 500 parts by weight of rhizoma atractylodis, 600 parts by weight of aloe, 400 parts by weight of grape seed and 20-40 parts by weight of mixed enzyme, and the specific process comprises the following steps:
(1) respectively cleaning the raw materials with clean water, and mixing herba schizonepetae, angelica and rhizoma atractylodis to obtain a component A of the raw material; mixing the rest materials to obtain a raw material component B; the raw material A, B is mixed with water with the temperature of 40-60 ℃ according to the mass ratio of 1: 5-10, respectively adding 30% of mixed enzyme by weight, respectively soaking for 12-18h, heating to 85-100 ℃, and continuing to soak for 24-48 h; respectively filtering, mixing the soaking solutions to obtain a mixed soaking solution, and mixing the filter residues to obtain a mixed raw material;
(2) transferring the mixed raw materials into a distillation retort, flatly paving the mixed raw materials on a middle sieve plate, placing the mixed impregnation liquid at the bottom of the distillation retort, heating the bottom of the distillation retort, and adopting a steam distillation mode, wherein the flow rate of steam is 15-25 m/s; collecting vapor liquid from the upper end of the distillation retort through a condenser, wherein the obtained vapor liquid is an oil-water mixture 1, and the mixed raw material of the distillation retort is reserved for later use;
(3) mixing the distilled mixed raw materials with water of 45-55 ℃ according to the proportion of 1: 1, placing the mixture in a closed glass tank, adding the rest of mixed enzyme, slowly stirring at the rotation speed of 300r/min for 1-2h, standing for 6-12h, transferring the mixture to a distillation tank, distilling the mixture in a water distillation mode, and collecting distillate to obtain an oil-water mixture 2;
(4) the oil-water mixture 1 and the oil-water mixture 2 are mixed and then are separated by an oil-water separation membrane to obtain mixed crude oil and water; extracting the mixed crude oil by a supercritical carbon dioxide extraction device, and then decoloring, filtering and removing impurities to obtain the essential oil.
The mixed enzyme is prepared from the following components in a mass ratio of 1: 1: 3: 2, phytase, cellulase, hemicellulase, mannanase.
The preparation method of the oil-water separation membrane comprises the following steps:
(1) cleaning a base film: placing the basement membrane in a cleaning agent, ultrasonically cleaning for 30-60min, and drying at 30-50 ℃ to constant weight;
(2) and base film pretreatment: soaking the base membrane in 40-60 deg.C treatment solution by soaking for 5-9h, taking out, naturally drying to no drop, soaking with pure water for 3 times, 3-5min each time, taking out, naturally drying to obtain pretreated base membrane;
(3) and preparing an oil-water separation membrane: intermittently soaking the pretreated base membrane in 35-45 deg.C modified solution for 30min, taking out, air drying for 10min, circulating for 5 times, and oven drying at 50-65 deg.C.
The base membrane is one of a polyethylene membrane, a polyvinylidene fluoride membrane, a polyimide membrane, a polyether sulfone membrane, a polyacrylonitrile membrane and a polylactic acid membrane;
the cleaning agent is prepared from the following raw materials in a mass ratio of 1: 1: 8, mixed solution of fatty alcohol-polyoxyethylene ether, cocoanut diethanol amine and ethanol;
the treating fluid is prepared from the following components in percentage by mass: 1: 3-7: 5-8: 40-50 of mixed solution of soybean lecithin, diethanolamine, ammonium stearate, nano zinc oxide and acetone;
the modified solution is a polyoxypropylene glycerol ether-ethanol solution with the molar volume of 0.05-0.2 mol/L.
The invention has the advantages that:
(1) the compound traditional Chinese medicine herbal essential oil prepared by the technical method has high extraction purity and high extraction rate, adopts steam distillation extraction, and has simple and reliable process;
(2) the mixed enzyme is adopted for treatment in a preparation process, so that the oil yield of the raw material is effectively improved;
(3) the oil-water separation process adopts the base membrane treated by the treatment fluid and the modified solution, a layer of super-hydrophobic oleophilic layer can be formed on the surface and the inner pores of the base membrane, the essential oil can be quickly separated, and the preparation efficiency is high.
In order to make the compound traditional Chinese medicine herbal essential oil and the application thereof more clear and clear, the invention is further described with reference to the specific embodiments.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Example 1
The compound traditional Chinese medicine herbal essential oil comprises 650 parts of schizonepeta, 650 parts of mint, 550 parts of angelica, 600 parts of rhizoma atractylodis, 500 parts of aloe, 300 parts of grape seeds and 20-40 parts of mixed enzyme by weight, and the specific process comprises the following steps:
(1) respectively cleaning the raw materials with clean water, and mixing herba schizonepetae, angelica and rhizoma atractylodis to obtain a component A of the raw material; mixing the rest materials to obtain a raw material component B; the raw material A, B is mixed with water at 50 ℃ according to the mass ratio of 1: 8, respectively adding 30 weight percent of mixed enzyme, respectively soaking for 15 hours, heating to 90 ℃, and continuing to soak for 36 hours; respectively filtering, mixing the soaking solutions to obtain a mixed soaking solution, and mixing the filter residues to obtain a mixed raw material;
(2) transferring the mixed raw materials into a distillation retort, flatly paving the mixed raw materials on a middle sieve plate, placing the mixed impregnation liquid at the bottom of the distillation retort, heating the bottom of the distillation retort, and adopting a steam distillation mode, wherein the flow rate of steam is 20 m/s; collecting vapor liquid from the upper end of the distillation retort through a condenser, wherein the obtained vapor liquid is an oil-water mixture 1, and the mixed raw material of the distillation retort is reserved for later use;
(3) mixing the distilled mixed raw materials with 50 ℃ water according to the proportion of 1: 1, placing the mixture in a closed glass tank, adding the rest mixed enzyme, slowly stirring at a rotating speed of 250r/min for 1.5h, standing for 9h, transferring the mixture to a distillation tank, distilling the mixture in water, and collecting distillate to obtain an oil-water mixture 2;
(4) the oil-water mixture 1 and the oil-water mixture 2 are mixed and then are separated by an oil-water separation membrane to obtain mixed crude oil and water; extracting the mixed crude oil by a supercritical carbon dioxide extraction device, and then decoloring, filtering and removing impurities to obtain the essential oil.
The mixed enzyme is prepared from the following components in a mass ratio of 1: 1: 3: 2, phytase, cellulase, hemicellulase, mannanase.
The preparation method of the oil-water separation membrane comprises the following steps:
(1) cleaning a base film: placing the basement membrane in a cleaning agent, ultrasonically cleaning for 45min, and drying at 40 ℃ to constant weight;
(2) and base film pretreatment: soaking the base membrane in 50 deg.C treatment solution by soaking for 5-9h, taking out, naturally drying to no drop, soaking with pure water for 3 times, each time for 4min, taking out, and naturally drying to obtain pretreated base membrane;
(3) and preparing an oil-water separation membrane: intermittently soaking the pretreated base membrane in the modified solution at 40 ℃ for 30min, taking out and airing for 10min, circulating for 5 times, and drying at 60 ℃.
The base film is a polyethylene film;
the cleaning agent is prepared from the following raw materials in a mass ratio of 1: 1: 8, mixed solution of fatty alcohol-polyoxyethylene ether, cocoanut diethanol amine and ethanol;
the treating fluid is prepared from the following components in percentage by mass: 1: 5: 7: 45 of mixed solution of soybean lecithin, diethanol amine, ammonium stearate, nano zinc oxide and acetone;
the modified solution is a polyoxypropylene glycerol ether-ethanol solution with the molar volume of 0.15 mol/L.
Example 2
The compound traditional Chinese medicine herbal essential oil comprises the following raw materials, by weight, 500 parts of schizonepeta, 550 parts of mint, 400 parts of angelica, 700 parts of rhizoma atractylodis, 600 parts of aloe, 400 parts of grape seeds and 40 parts of mixed enzyme, and the specific process comprises the following steps:
(1) respectively cleaning the raw materials with clean water, and mixing herba schizonepetae, angelica and rhizoma atractylodis to obtain a component A of the raw material; mixing the rest materials to obtain a raw material component B; the raw material A, B is mixed with water at 40 ℃ according to the mass ratio of 1: 5, respectively adding 30 percent of mixed enzyme by weight, respectively soaking for 12 hours, heating to 100 ℃, and continuing to soak for 48 hours; respectively filtering, mixing the soaking solutions to obtain a mixed soaking solution, and mixing the filter residues to obtain a mixed raw material;
(2) transferring the mixed raw materials into a distillation retort, flatly paving the mixed raw materials on a middle sieve plate, placing the mixed impregnation liquid at the bottom of the distillation retort, heating the bottom of the distillation retort, and adopting a steam distillation mode, wherein the flow rate of steam is 25 m/s; collecting vapor liquid from the upper end of the distillation retort through a condenser, wherein the obtained vapor liquid is an oil-water mixture 1, and the mixed raw material of the distillation retort is reserved for later use;
(3) mixing the distilled mixed raw materials with 45 ℃ water according to the proportion of 1: 1, placing the mixture in a closed glass tank, adding the rest mixed enzyme, slowly stirring at a speed of 200r/min for 1h, standing for 12h, transferring the mixture to a distillation tank, distilling the mixture in water, and collecting distillate to obtain an oil-water mixture 2;
(4) the oil-water mixture 1 and the oil-water mixture 2 are mixed and then are separated by an oil-water separation membrane to obtain mixed crude oil and water; extracting the mixed crude oil by a supercritical carbon dioxide extraction device, and then decoloring, filtering and removing impurities to obtain the essential oil.
The mixed enzyme is prepared from the following components in a mass ratio of 1: 1: 3: 2, phytase, cellulase, hemicellulase, mannanase.
The preparation method of the oil-water separation membrane comprises the following steps:
(1) cleaning a base film: placing the basement membrane in a cleaning agent, ultrasonically cleaning for 60min, and drying at 50 ℃ to constant weight;
(2) and base film pretreatment: soaking the base membrane in 40 deg.C treatment solution by soaking for 5 hr, taking out, naturally drying to no drop, soaking with pure water for 3 times, 3min each time, taking out, and naturally drying to obtain pretreated base membrane;
(3) and preparing an oil-water separation membrane: intermittently soaking the pretreated base membrane in a 45 ℃ modified solution for 30min, taking out and airing for 10min, circulating for 5 times, and drying at 65 ℃.
The base film is a polyvinylidene fluoride film;
the cleaning agent is prepared from the following raw materials in a mass ratio of 1: 1: 8, mixed solution of fatty alcohol-polyoxyethylene ether, cocoanut diethanol amine and ethanol;
the treating fluid is prepared from the following components in percentage by mass: 1: 3: 5: 50 of mixed solution of soybean lecithin, diethanol amine, ammonium stearate, nano zinc oxide and acetone;
the modified solution is a polyoxypropylene glycerol ether-ethanol solution with the molar volume of 0.05 mol/L.
Example 3
The compound traditional Chinese medicine herbal essential oil comprises 800 parts of schizonepeta, 750 parts of mint, 700 parts of angelica, 500 parts of rhizoma atractylodis, 400 parts of aloe, 200 parts of grape seeds and 20 parts of mixed enzyme by weight of raw materials, and the specific process comprises the following steps:
(1) respectively cleaning the raw materials with clean water, and mixing herba schizonepetae, angelica and rhizoma atractylodis to obtain a component A of the raw material; mixing the rest materials to obtain a raw material component B; the raw material A, B is mixed with water at 60 ℃ according to the mass ratio of 1: 10, respectively adding 30 percent of mixed enzyme by weight, respectively soaking for 18 hours, heating to 85 ℃, and continuing to soak for 24 hours; respectively filtering, mixing the soaking solutions to obtain a mixed soaking solution, and mixing the filter residues to obtain a mixed raw material;
(2) transferring the mixed raw materials into a distillation retort, flatly paving the mixed raw materials on a middle sieve plate, placing the mixed impregnation liquid at the bottom of the distillation retort, heating the bottom of the distillation retort, and adopting a steam distillation mode, wherein the flow rate of steam is 15 m/s; collecting vapor liquid from the upper end of the distillation retort through a condenser, wherein the obtained vapor liquid is an oil-water mixture 1, and the mixed raw material of the distillation retort is reserved for later use;
(3) mixing the distilled mixed raw materials with water at the temperature of 55 ℃ according to the proportion of 1: 1, placing the mixture in a closed glass tank, adding the rest mixed enzyme, slowly stirring at a rotating speed of 300r/min for 2 hours, standing for 6 hours, transferring the mixture to a distillation tank, distilling the mixture in water, and collecting distillate to obtain an oil-water mixture 2;
(4) the oil-water mixture 1 and the oil-water mixture 2 are mixed and then are separated by an oil-water separation membrane to obtain mixed crude oil and water; extracting the mixed crude oil by a supercritical carbon dioxide extraction device, and then decoloring, filtering and removing impurities to obtain the essential oil.
The mixed enzyme is prepared from the following components in a mass ratio of 1: 1: 3: 2, phytase, cellulase, hemicellulase, mannanase.
The preparation method of the oil-water separation membrane comprises the following steps:
(1) cleaning a base film: placing the basement membrane in a cleaning agent, ultrasonically cleaning for 30min, and drying at 30 ℃ to constant weight;
(2) and base film pretreatment: soaking the base membrane in 60 deg.C treatment solution by soaking for 9 hr, taking out, naturally drying to no drop, soaking and washing with pure water for 3 times, 5min each time, taking out, and naturally drying to obtain pretreated base membrane;
(3) and preparing an oil-water separation membrane: intermittently soaking the pretreated base membrane in 35 deg.C modified solution for 30min, taking out, air drying for 10min, circulating for 5 times, and oven drying at 50 deg.C.
The base film is a polyimide film;
the cleaning agent is prepared from the following raw materials in a mass ratio of 1: 1: 8, mixed solution of fatty alcohol-polyoxyethylene ether, cocoanut diethanol amine and ethanol;
the treating fluid is prepared from the following components in percentage by mass: 1: 7: 8: 40 of soybean lecithin, diethanol amine, ammonium stearate, nano zinc oxide and acetone;
the modified solution is a polyoxypropylene glycerol ether-ethanol solution with the molar volume of 0.2 mol/L.
Example 4
The compound traditional Chinese medicine herbal essential oil comprises 650 parts of schizonepeta, 650 parts of mint, 550 parts of angelica, 600 parts of rhizoma atractylodis, 500 parts of aloe and 300 parts of grape seeds by weight, and the specific process comprises the following steps:
(1) respectively cleaning the raw materials with clean water, and mixing herba schizonepetae, angelica and rhizoma atractylodis to obtain a component A of the raw material; mixing the rest materials to obtain a raw material component B; the raw material A, B is mixed with water at 50 ℃ according to the mass ratio of 1: 8, soaking for 15 hours, heating to 90 ℃, and continuing to soak for 36 hours; respectively filtering, mixing the soaking solutions to obtain a mixed soaking solution, and mixing the filter residues to obtain a mixed raw material;
(2) transferring the mixed raw materials into a distillation retort, flatly paving the mixed raw materials on a middle sieve plate, placing the mixed impregnation liquid at the bottom of the distillation retort, heating the bottom of the distillation retort, and adopting a steam distillation mode, wherein the flow rate of steam is 20 m/s; collecting vapor liquid from the upper end of the distillation retort through a condenser, wherein the obtained vapor liquid is an oil-water mixture 1, and the mixed raw material of the distillation retort is reserved for later use;
(3) mixing the distilled mixed raw materials with 50 ℃ water according to the proportion of 1: 1, placing the mixture in a closed glass tank, slowly stirring at the rotating speed of 250r/min for 1.5h, standing for 9h, transferring the mixture to a distillation tank, distilling the mixture in water, and collecting distillate to obtain an oil-water mixture 2;
(4) the oil-water mixture 1 and the oil-water mixture 2 are mixed and then are separated by an oil-water separation membrane to obtain mixed crude oil and water; extracting the mixed crude oil by a supercritical carbon dioxide extraction device, and then decoloring, filtering and removing impurities to obtain the essential oil.
The rest is the same as example 1.
Example 5
The compound traditional Chinese medicine herbal essential oil comprises 650 parts of schizonepeta, 650 parts of mint, 550 parts of angelica, 600 parts of rhizoma atractylodis, 500 parts of aloe, 300 parts of grape seeds and 30 parts of mixed enzyme by weight of raw materials, and the specific process comprises the following steps:
(1) respectively cleaning the raw materials with clean water, and mixing the clean water with water at 50 ℃ according to a mass ratio of 1: 8, respectively adding the mixed enzyme in parts by weight, soaking for 15 hours, heating to 95 ℃, and continuing to soak for 36 hours; filtering to obtain a soaking solution and a mixed raw material;
(2) transferring the mixed raw materials into a distillation retort, flatly paving the mixed raw materials on a middle sieve plate, placing the immersion liquid at the bottom of the distillation retort, heating the bottom of the distillation retort, and adopting a steam distillation mode, wherein the flow rate of steam is 20 m/s; collecting vapor liquid from the upper end of the distillation retort through a condenser, wherein the obtained vapor liquid is an oil-water mixture 1, and the mixed raw material of the distillation retort is reserved for later use;
(3) mixing the distilled mixed raw materials with 50 ℃ water according to the proportion of 1: 1, placing the mixture in a closed glass tank, slowly stirring at the rotating speed of 250r/min for 1.5h, standing for 9h, transferring the mixture to a distillation tank, distilling the mixture in water, and collecting distillate to obtain an oil-water mixture 2;
(4) the oil-water mixture 1 and the oil-water mixture 2 are mixed and then are separated by an oil-water separation membrane to obtain mixed crude oil and water; extracting the mixed crude oil by a supercritical carbon dioxide extraction device, and then decoloring, filtering and removing impurities to obtain essential oil;
the rest is the same as example 1.
Example 6
A method for preparing oil-water separation membrane from Chinese medicinal essential oil comprises:
(1) cleaning a base film: placing the basement membrane in a cleaning agent, ultrasonically cleaning for 45min, and drying at 40 ℃ to constant weight;
(2) and base film pretreatment: soaking the base membrane in 50 deg.C treatment solution by soaking for 7 hr, taking out, naturally drying to no drop, soaking and washing with pure water for 3 times, 4min each time, taking out, and naturally drying to obtain pretreated base membrane;
(3) and preparing an oil-water separation membrane: intermittently soaking the pretreated base membrane in 40 deg.C ethanol solution for 30min, taking out, air drying for 10min, circulating for 5 times, and oven drying at 60 deg.C;
the rest is the same as example 1.
Example 7
A compound traditional Chinese medicine herbal essential oil, wherein the treatment liquid used in the preparation of an oil-water separation membrane is prepared from the following raw materials in a mass ratio of 1: 1: 2: 4: 45 of mixed solution of soybean lecithin, diethanol amine, ammonium stearate, nano zinc oxide and acetone;
the rest is the same as example 1.
Example 8
A compound traditional Chinese medicine herbal essential oil, wherein the treatment liquid used in the preparation of an oil-water separation membrane is prepared from the following raw materials in a mass ratio of 1: 1: 8: 9: 45 of mixed solution of soybean lecithin, diethanol amine, ammonium stearate, nano zinc oxide and acetone;
the rest is the same as example 1.
Example 9
A compound Chinese medicinal essential oil is prepared by separating oil from water with common polyimide membrane, and treating with untreated solution and modified solution;
the rest is the same as example 1.
Test of
Test 1
To better illustrate the differences of the essential oil extraction methods of the above embodiments, the raw material oil yield, the essential oil purity and the storage stability of the compound traditional Chinese medicine herbs are analyzed and compared through experimental data, and the optimal scheme is preferably summarized in the following table 1:
TABLE 1 Compound Chinese medicinal herb essential oil preparation and storage condition table
From the data in the table above, it can be derived:
1. the compound traditional Chinese medicine herbal essential oil of each embodiment is better in embodiments 1, 2 and 3, and particularly best in embodiment 1;
2. comparative example 1, example 4 was conducted without using mixed enzyme treatment for essential oil extraction, and example 5 was conducted by a simple process without subjecting the raw materials to separate treatment, resulting in inferior oil yield and purity compared to the former;
3. in comparative example 1, examples 6, 7 and 8, when the oil-water separation membrane is prepared, the technical scheme does not meet the requirements of the invention, and example 9 adopts a common polyimide membrane separation membrane, so that the purity and the oil yield of essential oil extraction are general, the storage stability is poorer, and suspended matters are generated after storage experiments and are accompanied with turbidity.
Claims (8)
1. The compound traditional Chinese medicine herbal essential oil is characterized in that: the raw materials comprise 800 parts of 500-800 parts of schizonepeta, 750 parts of 550-750 parts of mint, 700 parts of 400-700 parts of angelica, 700 parts of 500-700 parts of rhizoma atractylodis, 600 parts of 400-600 parts of aloe, 400 parts of 200-400 parts of grape seed and 20-40 parts of mixed enzyme by weight, and the specific process comprises the following steps:
(1) respectively cleaning the raw materials with clean water, and mixing herba schizonepetae, angelica and rhizoma atractylodis to obtain a component A of the raw material; mixing the rest materials to obtain a raw material component B; the raw material A, B is mixed with water with the temperature of 40-60 ℃ according to the mass ratio of 1: 5-10, respectively adding 30% of mixed enzyme by weight, respectively soaking for 12-18h, heating to 85-100 ℃, and continuing to soak for 24-48 h; respectively filtering, mixing the soaking solutions to obtain a mixed soaking solution, and mixing the filter residues to obtain a mixed raw material;
(2) transferring the mixed raw materials into a distillation retort, flatly paving the mixed raw materials on a middle sieve plate, placing the mixed impregnation liquid at the bottom of the distillation retort, heating the bottom of the distillation retort, and adopting a steam distillation mode, wherein the flow rate of steam is 15-25 m/s; collecting vapor liquid from the upper end of the distillation retort through a condenser, wherein the obtained vapor liquid is an oil-water mixture 1, and the mixed raw material of the distillation retort is reserved for later use;
(3) mixing the distilled mixed raw materials with water of 45-55 ℃ according to the proportion of 1: 1, placing the mixture in a closed glass tank, adding the rest of mixed enzyme, slowly stirring at the rotation speed of 300r/min for 1-2h, standing for 6-12h, transferring the mixture to a distillation tank, distilling the mixture in a water distillation mode, and collecting distillate to obtain an oil-water mixture 2;
(4) the oil-water mixture 1 and the oil-water mixture 2 are mixed and then are separated by an oil-water separation membrane to obtain mixed crude oil and water; extracting the mixed crude oil by a supercritical carbon dioxide extraction device, and then decoloring, filtering and removing impurities to obtain the essential oil.
2. The compound traditional Chinese medicine herbal essential oil as claimed in claim 1, which is characterized in that: the mixed enzyme is prepared from the following components in a mass ratio of 1: 1: 3: 2, phytase, cellulase, hemicellulase, mannanase.
3. The compound traditional Chinese medicine herbal essential oil as claimed in claim 1, which is characterized in that: the preparation method of the oil-water separation membrane comprises the following steps:
(1) cleaning a base film: placing the basement membrane in a cleaning agent, ultrasonically cleaning for 30-60min, and drying at 30-50 ℃ to constant weight;
(2) and base film pretreatment: soaking the base membrane in 40-60 deg.C treatment solution by soaking for 5-9h, taking out, naturally drying to no drop, soaking with pure water for 3 times, 3-5min each time, taking out, naturally drying to obtain pretreated base membrane;
(3) and preparing an oil-water separation membrane: intermittently soaking the pretreated base membrane in 35-45 deg.C modified solution for 30min, taking out, air drying for 10min, circulating for 5 times, and oven drying at 50-65 deg.C.
4. The compound traditional Chinese medicine herbal essential oil as claimed in claim 3, which is characterized in that: the base membrane is one of a polyethylene membrane, a polyvinylidene fluoride membrane, a polyimide membrane, a polyether sulfone membrane, a polyacrylonitrile membrane and a polylactic acid membrane.
5. The compound traditional Chinese medicine herbal essential oil as claimed in claim 3, which is characterized in that: the cleaning agent is prepared from the following raw materials in a mass ratio of 1: 1: 8, fatty alcohol-polyoxyethylene ether, cocoanut oil diethanol amine and ethanol.
6. The compound traditional Chinese medicine herbal essential oil as claimed in claim 3, which is characterized in that: the treating fluid is prepared from the following components in percentage by mass: 1: 3-7: 5-8: 40-50 of soybean lecithin, diethanol amine, ammonium stearate, nano zinc oxide and acetone.
7. The compound traditional Chinese medicine herbal essential oil as claimed in claim 3, which is characterized in that: the modified solution is a polyoxypropylene glycerol ether-ethanol solution with the molar volume of 0.05-0.2 mol/L.
8. The use of the essential oil of a Chinese medicinal herb as claimed in any of claims 1 to 7 in the fields of medical treatment, agricultural chemicals, beauty, construction, daily use, clothing, and aromatherapy.
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