CN113046170B - Preparation method and application of avocado oil rich in furan lipid unsaponifiable matter - Google Patents
Preparation method and application of avocado oil rich in furan lipid unsaponifiable matter Download PDFInfo
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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
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/025—Pretreatment by enzymes or microorganisms, living or dead
-
- 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)
- A61K36/48—Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
-
- 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
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P1/00—Drugs for disorders of the alimentary tract or the digestive system
- A61P1/02—Stomatological preparations, e.g. drugs for caries, aphtae, periodontitis
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P19/00—Drugs for skeletal disorders
- A61P19/02—Drugs for skeletal disorders for joint disorders, e.g. arthritis, arthrosis
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P29/00—Non-central analgesic, antipyretic or antiinflammatory agents, e.g. antirheumatic agents; Non-steroidal antiinflammatory drugs [NSAID]
-
- 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
- C11B3/00—Refining fats or fatty oils
- C11B3/10—Refining fats or fatty oils by 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
- C11B3/00—Refining fats or fatty oils
- C11B3/12—Refining fats or fatty oils by distillation
-
- 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
- C11B3/00—Refining fats or fatty oils
- C11B3/16—Refining fats or fatty oils by mechanical means
-
- 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
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/19—Preparation or pretreatment of starting material involving fermentation using yeast, bacteria or both; enzymatic treatment
-
- 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
- A61K2236/31—Extraction of the material involving untreated material, e.g. fruit juice or sap obtained from fresh plants
-
- 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
Abstract
The invention belongs to the technical field of active ingredient extraction, and particularly relates to a preparation method and application of avocado oil rich in furan lipid unsaponifiable matters. Comprises the steps of distillation, cyclization, saponification, extraction, washing, concentration and the like, and the process can effectively extract unsaponifiable matters. The process method is simple and suitable for industrial popularization and application. The prepared unsaponifiable matter can be used for preparing medicaments for treating arthritis, rheumatoid arthritis and periodontitis and has better effect.
Description
Technical Field
The invention belongs to the technical field of active ingredient extraction, and particularly relates to a preparation method and application of avocado oil rich in furan lipid unsaponifiable matters.
Background
The unsaponifiable matter is a matter which does not react with alkali when the oil and fat are saponified, and is insoluble in water but soluble in ether. The unsaponifiable matter comprises sterol, high molecular fatty alcohol, saturated or unsaturated hydrocarbon, wax, pigment, vitamins, etc., wherein the most important components are squalene, tocopherol, and sterol. Most vegetable oils contain about 1% unsaponifiables.
The content of unsaponifiable matters in the vegetable oil is one of indexes for identifying the quality of the oil. When the vegetable oil is mixed with mineral oil and paraffin, the unsaponifiable matter value of the vegetable oil is increased, so that the purity and the mixing condition of the oil can be identified by measuring the unsaponifiable matters in the oil. In addition, in the soap-making industry, the unsaponifiable value of fats and oils is also often measured to determine whether the fats and oils are suitable for soap-making, and fats and oils having an unsaponifiable content exceeding 2% to 3% are not suitable for soap-making.
The unsaponifiable matter also has quite strong biological activity, and the unsaponifiable matter in the prepared oil or the refined oil can be used for developing foods, health-care foods, medicines and the like. When extracting oil from plant raw materials and preparing unsaponifiable matters in the oil by a traditional method, the oil is usually extracted from the raw materials firstly, an extraction solution is removed, potassium hydroxide and ethanol solution are added into the oil for heating and saponification, after saponification is finished, petroleum ether, diethyl ether and other solutions are used for extraction to obtain extracts of petroleum ether and diethyl ether layers, then the extracts are respectively washed by alkali-containing ethanol and ethanol, and the petroleum ether and the diethyl ether are volatilized to obtain the unsaponifiable matters in the oil.
In addition, there are many other extraction methods in the prior art, for example, chinese patent application CN 103445996 a discloses a method for extracting unsaponifiable matter from shea butter, which comprises the steps of ester exchange, molecular distillation, crystallization, etc., so as to obtain a high-purity unsaponifiable matter composition, wherein the content of unsaponifiable matter in the composition can reach 60%, 70% or even higher, the composition contains high content of triterpene alcohols and sterols, can exist in solid form, and can prolong shelf life, thus being applicable to various uses.
Chinese patent application CN 111012810A is a preparation method of unsaponifiable matter in ginseng seed oil, belonging to the field of preparation methods of ginseng extracts. Processing dry ginseng seeds into powder, adding petroleum ether, extracting by a reflux method, and pouring out a petroleum ether solution after extraction is finished; adding sodium hydroxide and ethanol solution into petroleum ether solution, stirring and heating; standing after heating, and washing a petroleum ether layer with sodium hydroxide and ethanol solution; washing the petroleum ether layer with ethanol solution; concentrating petroleum ether layer under reduced pressure or normal pressure to obtain unsaponifiable matter of ginseng seed oil. The preparation efficiency of unsaponifiable matters in the grease is improved by 20-50%, and the consumption of petroleum ether is reduced by about 50%. The unsaponifiable matter mainly contains squalene, beta-sitosterol and beta-resinol which are detected by gas chromatography and mass spectrometry, and the three substances account for more than 60 percent of the total unsaponifiable matter by a normalization method.
Avocado oil has higher nutritive value, but distillate in the avocado oil refining process is often treated as waste and is not reasonably utilized, so that the avocado resource waste is caused, and economic and environmental burdens are caused by treatment of a large amount of waste. Therefore, in order to more effectively utilize the byproducts in the avocado oil refining process, the invention provides a process for preparing unsaponifiable matters by utilizing the byproducts.
Disclosure of Invention
In order to overcome the technical problems, the invention provides a preparation method and application of avocado oil rich in furan lipid unsaponifiable matters. The process can effectively extract unsaponifiable matter. The prepared unsaponifiable matter can be used for preparing the medicine for treating arthritis and periodontitis and has better effect.
In order to achieve the above purpose, the technical scheme provided by the invention is as follows:
a method for preparing unsaponifiable matter comprises the following steps:
(1) distilling avocado oil under vacuum, cyclizing distillate, and concentrating to obtain avocado oil concentrated solution;
(2) treating avocado oil concentrated solution with active carbon, diluting with ethanol, adding potassium hydroxide, and saponifying to obtain saponified product;
(3) diluting the saponified product with purified water, adding 1, 2-dichloroethane for extraction, centrifuging, and removing the supernatant; adding purified water for washing;
(4) drying under reduced pressure to remove 1, 2-dichloroethane, and purging with steam and nitrogen to obtain avocado oil unsaponifiable matter.
Preferably, the preparation method of the avocado oil comprises the following steps:
removing skin and core of avocado and avocado, pulping, adjusting pH value, performing enzymolysis, adding demulsifier, adding in water bath under shaking, centrifuging, layering, and extracting upper oil; making avocado oil.
Preferably, the enzyme for enzymolysis is xylanase and alkaline protease, wherein the mass ratio of the xylanase to the alkaline protease is 1-5: 1; preferably 3: 1.
Preferably, the xylanase is used in an amount of 0.5-2% of the pulp mass of avocado.
Preferably, the enzyme activity of the xylanase is 5000-40000U/g; the enzyme activity of the alkaline protease is 300000-600000U/g;
preferably, the demulsifier is a mixture of phospholipase and ethanol, and is used in an amount of 0.5-1.5% of the pulp mass of avocado;
the mass ratio of the phospholipase to the ethanol is 1: 3-5.
Preferably, the preparation method of the avocado oil comprises the following steps:
removing skin and core of avocado and avocado, pulping, adjusting pH to 3-4, adjusting temperature to 40-50 deg.C, adding xylanase, and performing enzymolysis for 30-60 min; adjusting pH to 7-8, adding alkaline protease, performing enzymolysis for 40-60min, adding demulsifier, adding in water bath under shaking, centrifuging, and extracting upper oil; making avocado oil.
Preferably, the pH at which the xylitol enzyme is enzymatically hydrolyzed is 3.5.
Preferably, the pH at the time of alkaline protease hydrolysis is 7.4.
Preferably, in step (1), the distillation is carried out at a pressure of from 0.1 to 0.15mbar and a temperature of from 150 ℃ to 180 ℃.
Preferably, the cyclization is performed on specific fatty acid in avocado oil, and the fatty acid capable of forming five-membered cyclic lactone is formed, and preferably, the cyclization product is furan lipid.
Preferably, the cyclization is carried out under the action of a catalyst.
Preferably, the catalyst used in the avocado oil cyclization process is any one of acidic alumina, hydrochloric acid, sulfuric acid or acetic acid.
Preferably, in step (1), the cyclization is carried out under the protection of nitrogen.
Preferably, in step (1), the temperature of the cyclization is 70-85 ℃.
Preferably, in the step (2), the mass of the potassium hydroxide is 40-50% of the mass of the avocado oil.
Preferably, in the step (2), the volume of the ethanol is 2-3 times of that of the avocado oil concentrated solution.
Preferably, in the step (2), the time of the activated carbon treatment is 30-60 min. Preferably, in the step (3), the amount of the purified water added upon dilution is 2 to 3 times the mass of the saponified product.
Preferably, in the step (3), the 1, 2-dichloroethane is used in an amount of 5 to 6 times by mass based on the saponified product.
Preferably, in the step (3), the rotation speed of the centrifugation is 1500-.
Preferably, in the step (4), the reduced pressure drying condition is a pressure of 100-500 pa; the temperature is 30-40 ℃.
Preferably, in the step (4), the ventilation rate of the water vapor purging is 20-50L/min;
preferably, in the step (4), the aeration rate of the nitrogen purge is 20-50L/min.
Preferably, in the step (4), the number of times of the water vapor and nitrogen purges is 3 to 5.
Another object of the present invention is to provide an unsaponifiable matter obtained by the unsaponifiable production method.
The invention also aims to provide the application of the unsaponifiable matter in preparing a medicament for treating arthritis or/and periodontitis.
The invention also aims to provide a medicament for treating arthritis or/and periodontitis, which contains the unsaponifiable matter.
Preferably, the raw materials for preparing the unsaponifiable matters in the medicine comprise avocado oil and soybean oil.
Preferably, the mass ratio of the avocado oil unsaponifiable matter to the soybean oil unsaponifiable matter in the medicine is 1: 3-2: 3.
preferably, the preparation method of the soybean oil unsaponifiable matter comprises the following steps:
(1) distilling soybean oil under vacuum, collecting distillate, and concentrating to obtain soybean oil concentrate;
(2) treating the soybean oil concentrated solution with active carbon, diluting with ethanol, adding potassium hydroxide, and saponifying to obtain saponified product;
(3) diluting the saponified product with purified water, adding 1, 2-dichloroethane for extraction, centrifuging, and removing the supernatant; adding purified water for washing;
(4) drying under reduced pressure to remove 1, 2-dichloroethane, and purging with steam and nitrogen to obtain soybean oil unsaponifiable matter.
Compared with the prior art, the invention has the technical advantages that:
(1) the active carbon is added in the invention to remove impurities, such as aromatic impurities like benzopyrene and pesticides.
(2) The distillate (by-product) obtained by refining and deodorizing avocado oil (i.e. distilling) is subjected to cyclization and then saponification. The method utilizes byproducts produced in the avocado oil refining process, most of unsaponifiable matter components wanted by the product are enriched in the byproducts, and then cyclization is carried out to generate more furan compounds, and then saponification reaction is carried out to further realize the effect of enriching and purifying the unsaponifiable matters, so that the unsaponifiable matters rich in furan lipids, sterols and other components are finally obtained.
The distillation plays a role in enrichment, the utilization of byproducts is more economical and environment-friendly than the direct saponification of avocado oil, and the yield of unsaponifiable matters is improved. The distilled and refined vegetable oil can remove special odor and retain the original economic benefit and value of the oil and fat for utilization.
(3) Avocado contains derivatives of persin, which are extracted from avocado and undergo chemical transformation by dehydration and intramolecular cyclization to produce beneficial substances. Polar compounds in the unsaponifiable matter, such as aliphatic polyacetyls of aliphatic polyhydroxy alcohols or persins, are precursors of aliphatic furans, which can form, by chemical conversion, beneficial substances such as furanic lipids.
(4) The preparation method of the unsaponifiable matter provided by the invention uses avocado oil as a raw material, and the prepared unsaponifiable matter can be used for preparing a medicine for treating arthritis or/and periodontitis, and the medicine can reduce damage of connective tissues and be used for treating or relieving inflammation related to damage of the connective tissues, such as arthritis, rheumatoid arthritis, periodontitis and the like.
Detailed Description
The present invention will be described below with reference to specific examples to make the technical aspects of the present invention easier to understand and grasp, but the present invention is not limited thereto. The experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
Example 1
A method for preparing unsaponifiable matter comprises the following steps:
(1) preparing avocado oil: removing skin and core of avocado and avocado, pulping, adjusting pH to 3.5, adjusting temperature to 45 deg.C, adding 1.2% xylanase, and performing enzymolysis for 40 min; adjusting the pH value to 7.4, adding alkaline protease (the mass ratio of xylanase to alkaline protease is 3:1), performing enzymolysis for 50min, adding a mixture of 1.0% of phospholipase and ethanol (the mass ratio of phospholipase to ethanol is 1:4) according to the mass of avocado pulp, performing emulsion breaking, adding in water bath by oscillation, performing centrifugal layering, and extracting upper oil; preparing avocado oil; wherein the enzyme activity of the xylanase is 10000U/g; the enzyme activity of the alkaline protease is 500000U/g;
(2) distilling avocado oil at 0.12mbar and 160 deg.C, collecting distillate, adding acidic alumina, cyclizing at 80 deg.C under nitrogen protection, and concentrating to obtain avocado oil concentrated solution;
(3) treating the avocado oil concentrated solution with active carbon for 40min, diluting with 3 times volume of ethanol, adding potassium hydroxide 45% of avocado oil by mass, and saponifying to obtain saponified product;
(4) adding purified water with the mass of 2 times of that of the saponified product to dilute the saponified product, adding 1, 2-dichloroethane with the mass of 5 times of that of the saponified product to extract the saponified product, performing centrifugal separation at 2000rpm, and removing supernatant; adding purified water for washing;
(5) at a pressure of 100 pa; drying under reduced pressure at 30 deg.C to remove 1, 2-dichloroethane, simultaneously purging with steam and nitrogen for 3 times, wherein the ventilation rate of steam purging is 30L/min and the ventilation rate of nitrogen purging is 20L/min during each purging to obtain avocado oil unsaponifiable matter.
Example 2
A method for preparing unsaponifiable matter comprises the following steps:
(1) preparing avocado oil: removing skin and core of avocado and avocado, pulping, adjusting pH to 3, adjusting temperature to 40 deg.C, adding 0.5% xylanase, and performing enzymolysis for 60 min; adjusting the pH value to 7, adding alkaline protease (the mass ratio of xylanase to alkaline protease is 1:1), performing enzymolysis for 40min, adding 0.5% of a mixture of phospholipase and ethanol (the mass ratio of phospholipase to ethanol is 1:5) according to the mass of avocado pulp, performing emulsion breaking, adding in water bath by shaking, centrifuging and layering, and extracting upper oil; preparing avocado oil; wherein the enzyme activity of the xylanase is 5000U/g; the enzyme activity of the alkaline protease is 600000U/g;
(2) distilling avocado oil at 0.1mbar and 180 deg.C, collecting distillate, adding acidic alumina, cyclizing at 70 deg.C under nitrogen protection, and concentrating to obtain avocado oil concentrated solution;
(3) treating the avocado oil concentrated solution with active carbon for 60min, diluting with 2 times volume of ethanol, adding potassium hydroxide 40% of avocado oil by mass, and saponifying to obtain saponified product;
(4) adding purified water with the mass of 3 times into the saponified product for dilution, then adding 1, 2-dichloroethane with the mass of 6 times into the saponified product for extraction, performing centrifugal separation at 3000rpm, and removing supernatant; adding purified water for washing;
(5) at a pressure of 500 pa; drying under reduced pressure at 40 deg.C to remove 1, 2-dichloroethane, simultaneously purging with steam and nitrogen for 4 times, wherein the ventilation rate of steam purging is 50L/min and the ventilation rate of nitrogen purging is 20L/min during each purging to obtain avocado oil unsaponifiable matter.
Example 3
A method for preparing unsaponifiable matter comprises the following steps:
(1) preparing avocado oil: removing skin and core of avocado and avocado, pulping, adjusting pH to 4, adjusting temperature to 50 deg.C, adding 2% xylanase, and performing enzymolysis for 30 min; adjusting the pH value to 8, adding alkaline protease (the mass ratio of xylanase to alkaline protease is 5:1), performing enzymolysis for 60min, adding a mixture of 1.5% phospholipase and ethanol (the mass ratio of phospholipase to ethanol is 1:3) according to the mass of avocado pulp, performing emulsion breaking, adding in water bath by shaking, centrifuging and layering, and extracting upper oil; preparing avocado oil; wherein the enzyme activity of the xylanase is 40000U/g; the enzyme activity of the alkaline protease is 300000U/g;
(2) distilling avocado oil at 0.15mbar and 150 deg.C, collecting distillate, adding hydrochloric acid, cyclizing at 85 deg.C under nitrogen protection, and concentrating to obtain avocado oil concentrate;
(3) treating the avocado oil concentrated solution with active carbon for 30min, diluting with 3 times volume of ethanol, adding potassium hydroxide 50% of avocado oil, and saponifying to obtain saponified product;
(4) adding purified water with the mass of 2 times of that of the saponified product to dilute the saponified product, adding 1, 2-dichloroethane with the mass of 5 times of that of the saponified product to extract the saponified product, performing centrifugal separation at 1500rpm, and removing supernatant; adding purified water for washing;
(5) at a pressure of 100 pa; drying under reduced pressure at 30 deg.C to remove 1, 2-dichloroethane, simultaneously purging with steam and nitrogen for 5 times, wherein the ventilation rate of steam purging is 20L/min and the ventilation rate of nitrogen purging is 50L/min during each purging to obtain avocado oil unsaponifiable matter.
Comparative example 1
The difference compared to example 1 is only the enzyme in the preparation of avocado oil.
A method for preparing unsaponifiable matter comprises the following steps:
(1) preparing avocado oil: removing skin and core of avocado and avocado, pulping, adjusting pH to 3.5, adjusting temperature to 45 deg.C, adding 1.2% xylanase, and performing enzymolysis for 40 min; adding a mixture of 1.0% of phospholipase and ethanol (the mass ratio of the phospholipase to the ethanol is 1:4) according to the mass of avocado pulp to demulsify, adding in water bath by shaking, centrifuging and layering to extract upper oil; preparing avocado oil; wherein the enzyme activity of the xylanase is 10000U/g;
(2) - (5) same as in example 1.
Comparative example 2
The difference compared to example 1 is only the enzyme in the preparation of avocado oil.
A method for preparing unsaponifiable matter comprises the following steps:
(1) preparing avocado oil: pulping avocado flesh, removing skin and core, adjusting temperature to 45 deg.C, adjusting pH to 7.4, adding 1.2% alkaline protease, performing enzymolysis for 50min, adding 1.0% phospholipase-ethanol mixture (phospholipase-ethanol mass ratio of 1:4) to demulsify, adding in water bath under shaking, centrifuging, and layering to obtain upper oil; preparing avocado oil; wherein the enzyme activity of the alkaline protease is 500000U/g;
(2) - (5) same as in example 1.
Comparative example 3
Compared with example 1, the difference is only the enzymolysis condition in the preparation of avocado oil.
A method for preparing unsaponifiable matter comprises the following steps:
(1) preparing avocado oil: removing skin and core of avocado and avocado, pulping, adjusting pH to 3.5, adjusting temperature to 45 deg.C, adding 1.2% xylanase, and performing enzymolysis for 40 min; adjusting the pH value to 7.4, adding alkaline protease (the mass ratio of xylanase to alkaline protease is 1:5), performing enzymolysis for 50min, adding a mixture of 1.0% of phospholipase and ethanol (the mass ratio of phospholipase to ethanol is 1:4) according to the mass of avocado pulp, performing emulsion breaking, adding in water bath by oscillation, performing centrifugal layering, and extracting upper oil; preparing avocado oil; wherein the enzyme activity of the xylanase is 10000U/g; the enzyme activity of the alkaline protease is 500000U/g;
(2) - (5) same as in example 1.
Comparative example 4
The difference compared to example 1 is only in the demulsifier at the time of avocado oil preparation.
A method for preparing unsaponifiable matter comprises the following steps:
(1) preparing avocado oil: removing skin and core of avocado and avocado, pulping, adjusting pH to 3.5, adjusting temperature to 45 deg.C, adding 1.2% xylanase, and performing enzymolysis for 40 min; adjusting the pH value to 7.4, adding alkaline protease (the mass ratio of xylanase to alkaline protease is 3:1), performing enzymolysis for 50min, adding 1.0% ethanol based on the avocado pulp mass, performing emulsion breaking, adding in water bath shaking, centrifuging, layering, and extracting upper oil; preparing avocado oil; wherein the enzyme activity of the xylanase is 10000U/g; the enzyme activity of the alkaline protease is 500000U/g;
(2) - (5) same as in example 1.
Comparative example 5
The difference compared to example 1 is only in the demulsifier at the time of avocado oil preparation.
A method for preparing unsaponifiable matter comprises the following steps:
(1) preparing avocado oil: removing skin and core of avocado and avocado, pulping, adjusting pH to 3.5, adjusting temperature to 45 deg.C, adding 1.2% xylanase, and performing enzymolysis for 40 min; adjusting the pH value to 7.4, adding alkaline protease (the mass ratio of xylanase to alkaline protease is 3:1), performing enzymolysis for 50min, adding a mixture of 1.0% of phospholipase and ethanol (the mass ratio of phospholipase to ethanol is 4:1) according to the mass of avocado pulp, performing emulsion breaking, adding in water bath by oscillation, performing centrifugal layering, and extracting upper oil; preparing avocado oil; wherein the enzyme activity of the xylanase is 10000U/g; the enzyme activity of the alkaline protease is 500000U/g;
(2) - (5) same as in example 1.
Comparative example 6
The only difference compared to example 1 is the distillation conditions.
A method for preparing unsaponifiable matter comprises the following steps:
(1) the same as example 1;
(2) distilling avocado oil at 0.12mbar and 120 deg.C, collecting distillate, adding acidic alumina, cyclizing at 80 deg.C under nitrogen protection, and concentrating to obtain avocado oil concentrated solution;
(3) - (5) same as in example 1.
Comparative example 7
The only difference compared to example 1 is the ring closure temperature.
A method for preparing unsaponifiable matter comprises the following steps:
(1) the same as example 1;
(2) distilling avocado oil at 0.12mbar and 160 deg.C, collecting distillate, adding acidic alumina, cyclizing at 50 deg.C under nitrogen protection, and concentrating to obtain avocado oil concentrated solution;
(3) - (5) same as in example 1.
Comparative example 8
The difference compared to example 1 is only the method of preparation of the avocado oil.
A method for preparing unsaponifiable matter comprises the following steps:
(1) peeling and removing core of avocado and avocado, and drying the pulp at 85 deg.C for 48 hr to obtain dried pulp; squeezing the dried pulp, and filtering to obtain avocado oil.
(2) - (5) same as in example 1.
Examples of effects
1. Separating avocado oil unsaponifiable matter by thin layer chromatography
(1) Thin plate for chromatography
Silica gel plate: for separation of unsaponifiable matter, about 20mg of mixed sample can be separated from each plate, 20G of silica gel G is mixed with 56ml of distilled water, and then coated on a glass plate of 20cm × 25cm, dried at room temperature, and activated in an oven at 110 ℃ for 90 min.
(2) Developing agent
Developing agent I: petroleum ether: ether 7:3 (V/V); developing agent II: dichloromethane: petroleum ether is 7:3 (V/V).
(3) Color development method
After the thin layer is developed, after the developing agent is completely volatilized, 0.02 percent rhodamine 6G ethanol solution is sprayed, the color bands are immediately observed under an ultraviolet lamp, and boundaries among the bands are respectively marked by pins.
(4) Collecting and eluting
The bands were collected separately, eluted thoroughly with ether, concentrated to near dryness and the solvent was drained off under reduced pressure.
2. Detection and analysis of unsaponifiable matter by gas chromatography
(1) Chromatographic conditions are as follows:
a chromatographic column: DB5(30m x 0.32mm, 0.25 um).
Temperature of the column: after maintaining the temperature at 60 ℃ for 1 minute, the temperature is raised to 180 ℃ at 30 ℃/min, maintained at 180 ℃ for 5 minutes, and raised to 285 ℃ at 3 ℃/min.
Sample injection temperature: after a duration of 0.1 minute at 40 ℃ the temperature was increased by 100 ℃ per minute until 260 ℃.
A detector: FID. Temperature of the probe: 290 deg.c.
Carrier gas: helium gas.
Outflow pressure: 0.5 bar.
(2) And (4) performing qualitative determination by using the relative retention time of each chromatographic peak, and calculating the relative content of each component by using a peak area normalization method.
The results are shown in Table 1.
TABLE 1 composition and amount of avocado oil unsaponifiables
Therefore, the preparation method of the avocado oil unsaponifiable matter provided by the invention has better extraction efficiency, and the use of raw materials in the process and the process have important influence on the extraction effect of the unsaponifiable matter and the effective components thereof.
The above detailed description is specific to one possible embodiment of the present invention, and the embodiment is not intended to limit the scope of the present invention, and all equivalent implementations or modifications without departing from the scope of the present invention should be included in the technical scope of the present invention.
Claims (7)
1. A method for preparing unsaponifiable matter comprises the following steps:
(1) distilling avocado oil under 0.1-0.15mbar and 150-180 deg.C vacuum, cyclizing distillate, and concentrating to obtain avocado oil concentrated solution; the cyclization is carried out under the action of a catalyst, and the temperature of the cyclization is 70-85 ℃; the catalyst is acidic alumina or hydrochloric acid;
(2) treating avocado oil concentrated solution with active carbon, diluting with ethanol, adding potassium hydroxide, and saponifying to obtain saponified product;
(3) diluting the saponified product with purified water, adding 1, 2-dichloroethane for extraction, centrifuging, and removing the supernatant; adding purified water for washing;
(4) drying under reduced pressure to remove 1, 2-dichloroethane, and simultaneously purging with steam and nitrogen to obtain avocado oil unsaponifiable matter; the aeration rate of the nitrogen purging is 20-50L/min;
the preparation method of the avocado oil comprises the following steps:
removing skin and core of avocado, pulping pulp, adjusting pH value, performing enzymolysis, adding demulsifier, adding in water bath under shaking, centrifuging, and layering to obtain upper oil; preparing avocado oil;
wherein the enzyme for enzymolysis is xylanase and alkaline protease, and the mass ratio of the xylanase to the alkaline protease is 1-5: 1; the enzymolysis is to adjust the pH value to 3-4, add xylanase and carry out enzymolysis for 30-60 min; adjusting pH to 7-8, adding alkaline protease, and performing enzymolysis for 40-60 min; the demulsifier is a mixture of phospholipase and ethanol, and the mass ratio of the phospholipase to the ethanol is 1: 3-5;
the use amount of the xylanase is 0.5-2% of the pulp mass of the avocado; the using amount of the demulsifier is 0.5-1.5% of the pulp quality of the avocado.
2. The method for producing an unsaponifiable matter according to claim 1 wherein the mass ratio of xylanase to alkaline protease is 3: 1.
3. The method for producing an unsaponifiable matter of claim 1 wherein in step (2), the activated carbon treatment is carried out for 30 to 60 minutes; the mass of the potassium hydroxide is 40-50% of the mass of the avocado oil; in the step (3), the adding amount of the purified water is 2-3 times of the mass of the saponified product when the purified water is diluted; in the step (3), the dosage of the 1, 2-dichloroethane is 5-6 times of the mass of the saponified product; in the step (3), the rotation speed of the centrifugation is 1500-3000 rpm; in the step (4), the reduced pressure drying condition is a pressure of 100-; the temperature is 30-40 ℃; in the step (4), the ventilation rate of the water vapor purging is 20-50L/min; in the step (4), the frequency of the steam and nitrogen purging is 3-5 times.
4. An unsaponifiable matter obtainable by a process for the preparation of an unsaponifiable matter according to any one of claims 1-3.
5. Use of an unsaponifiable matter according to claim 4 in the manufacture of a medicament for the treatment of arthritis and/or periodontitis.
6. A medicament for the treatment of arthritis or/and periodontitis comprising the unsaponifiable matter of claim 4.
7. The medicament for treating arthritis or/and periodontitis according to claim 6, wherein the unsaponifiable matter of the medicament further comprises unsaponifiables of soybean oil; the mass ratio of the avocado oil unsaponifiable matter to the soybean oil unsaponifiable matter in the medicine is 1: 3-2: 3;
the preparation method of the soybean oil unsaponifiable matter comprises the following steps:
(1) distilling soybean oil under vacuum, collecting distillate, and concentrating to obtain soybean oil concentrate;
(2) treating the soybean oil concentrated solution with active carbon, diluting with ethanol, adding potassium hydroxide, and saponifying to obtain saponified product;
(3) diluting the saponified product with purified water, adding 1, 2-dichloroethane for extraction, centrifuging, and removing the supernatant; adding purified water for washing;
(4) drying under reduced pressure to remove 1, 2-dichloroethane, and purging with steam and nitrogen to obtain soybean oil unsaponifiable matter.
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