CN104403798B - Preparation method of eucommia ulmoides mixed essential oil - Google Patents
Preparation method of eucommia ulmoides mixed essential oil Download PDFInfo
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- CN104403798B CN104403798B CN201410672273.0A CN201410672273A CN104403798B CN 104403798 B CN104403798 B CN 104403798B CN 201410672273 A CN201410672273 A CN 201410672273A CN 104403798 B CN104403798 B CN 104403798B
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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
- C11B9/027—Recovery of volatiles by distillation or stripping
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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
- C11B9/022—Refining
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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
- C11B9/025—Recovery by solvent extraction
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
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Abstract
The invention discloses a preparation method of eucommia ulmoides mixed essential oil, which belongs to the extraction of plant essential oil in the chemical field. According to the invention, effective components are respectively extracted from green leaves, branches and bark of eucommia ulmoides through different extraction processes, and then the active components are mixed through a special process to finally obtain the eucommia ulmoides essential oil, so that the leaves, branches and bark of eucommia ulmoides are utilized to the maximum extent, the extraction yield of the eucommia ulmoides essential oil is improved, the finally obtained eucommia ulmoides essential oil has the medicinal function and the health care function of the three, the application of the eucommia ulmoides essential oil is greatly enriched, and the economic value of eucommia ulmoides is improved.
Description
Technical Field
The invention relates to the field of extraction of plant essential oil, in particular to a preparation method of eucommia ulmoides mixed essential oil.
Background
Eucommia bark is a rare Chinese medicinal material in China, has a cultivation history of more than two thousand years in China, has high medicinal value, belongs to a rare nourishing medicinal material, and is sweet in taste and warm in nature. Has effects in tonifying liver and kidney, strengthening muscle and bone, regulating Chong and ren meridians, and preventing miscarriage. Can be used for treating lumbago, leg pain, soreness, weakness, and asthenia due to kidney yang deficiency, and symptoms such as hypochondriac instability, and scrotum pruritus due to liver qi deficiency. It is listed as the superior in Shen nong Ben Cao Jing. The eucommia ulmoides leaves are raw materials for preparing the eucommia ulmoides tea, and the eucommia ulmoides tea has high health care value. The modern research on eucommia bark has the effects of clearing away in-vivo garbage, strengthening the metabolism of human cell substances, preventing the aging of musculoskeletal tissues, balancing the blood pressure of a human body, decomposing in-vivo cholesterol, reducing in-vivo fat, restoring the elasticity of blood vessels, inducing diuresis, clearing heat, resisting bacteria in a broad spectrum, exciting central nerves and improving the pharmacological action of white blood cells.
The plant essential oil is volatile aromatic substance extracted from flower, leaf, stem, root or fruit of plant by steam distillation, extrusion, cold soaking or solvent extraction. Essential oils are lipophilic and very soluble in oils and fats, because the molecular chains of essential oils are usually relatively short, which makes them very permeable to the skin and enter the body via the abundant capillaries under the subcutaneous fat. The essential oil is composed of a plurality of very small molecules, and the high volatile substances can be absorbed by nasal mucosa tissues to enter the body, so that messages are directly sent to the brain, and the emotion and the physiological function of the body are regulated through the peripheral system of the brain. Therefore, in aromatherapy, the essential oils can strengthen physiological and psychological functions. Each plant essential oil has a chemical structure to determine its flavor, color, fluidity and its mode of operation with the system, and each plant essential oil has a specific set of functional characteristics.
Disclosure of Invention
The invention aims to provide a method for extracting essential oil from eucommia ulmoides, the extracted essential oil not only has good health care value, but also has certain medicinal value, and the economic value of eucommia ulmoides cultivation is improved.
In order to achieve the purpose, the technical scheme provided by the invention is as follows: a preparation method of eucommia ulmoides mixed essential oil comprises the following steps:
1) selecting fresh green leaves of eucommia ulmoides, cleaning the leaves with clear water, then placing the leaves above a sieve plate of a distillation kettle, adding a proper amount of water at the bottom of the distillation kettle, isolating the leaves from the eucommia ulmoides, and then distilling to obtain distillate generated by distillation for later use;
during distillation, the distillation speed is controlled to be 4-5% of the volume of the steamer, and simultaneously the flow rate of cooling water is controlled, so that the temperature of condensate discharged in the first half hour of the distillate is 20-25 ℃, the temperature of condensate discharged in the half hour is 50-55 ℃, and finally the weight of the distillate discharged is controlled to be 3 times of that of the eucommia leaves;
2) selecting branches of eucommia ulmoides, drying, crushing to obtain particles with the particle size not more than 50 meshes, soaking in alcohol with the volume concentration of 40-50% for 3-5h according to the weight ratio of 1:5, and then applying ultrasonic waves to the branches, wherein the application mode of the ultrasonic waves is as follows: firstly, applying ultrasonic wave with the frequency of 350-370KHz for 1min and stopping for 0.5min, then applying ultrasonic wave with the frequency of 100-120KHz and stopping for 0.5min, circulating the application process of the ultrasonic wave for 4-6 times, and filtering to obtain powder and filtrate for later use;
3) selecting bark of eucommia ulmoides, drying, crushing to obtain particles with the particle size not more than 50 meshes, soaking the bark of eucommia ulmoides in sesame oil with the temperature of 70-80 ℃ for 2-3 hours according to the weight ratio of 1:4, filtering to obtain eucommia ulmoides powder, mixing the eucommia ulmoides powder and the powder obtained in the step 2) according to the weight ratio of 1:2, putting the mixture into an extraction reaction kettle, extracting by using ethanol, and collecting an extract for later use;
4) uniformly mixing the extract obtained in the step 3), the filtrate obtained in the step 2) and the distillate obtained in the step 1) according to the weight ratio of 1:2:1, adding carbon powder accounting for 5% of the total weight of the extract, applying microwave to the mixture to enable the temperature of the mixed solution to reach 90-95 ℃, keeping the state for 0.5-1h, naturally cooling, and filtering the carbon powder to obtain a filtrate for later use;
5) and (3) carrying out oil-water separation on the filtrate obtained in the step 4) by adopting a distillation method to obtain an oil phase, namely the product.
The bark of eucommia bark is perennial bark or trunk bark with more than six years, and the branch of eucommia bark is annual twig.
Has the advantages that: according to the invention, effective components are respectively extracted from green leaves, branches and bark of eucommia ulmoides through different extraction processes, and then the active components are mixed through a special process to finally obtain the eucommia ulmoides essential oil, so that the leaves, branches and bark of eucommia ulmoides are utilized to the maximum extent, the extraction yield of the eucommia ulmoides essential oil is improved, the finally obtained eucommia ulmoides essential oil has the medicinal function and the health care function of the three, the application of the eucommia ulmoides essential oil is greatly enriched, and the economic value of eucommia ulmoides is improved.
Detailed Description
The invention is further illustrated with reference to specific examples. The bark used in the following examples is selected from perennial bark (such as perennial branch bark) or trunk bark of more than six years, and the branch of eucommia bark is selected from annual twig.
Example 1
A preparation method of eucommia ulmoides mixed essential oil comprises the following steps:
1) selecting fresh green leaves of eucommia ulmoides, cleaning the leaves with clear water, then placing the leaves above a sieve plate of a distillation kettle, adding a proper amount of water at the bottom of the distillation kettle, isolating the leaves from the eucommia ulmoides, and then distilling to obtain distillate generated by distillation for later use;
during distillation, the distillation speed is controlled to be 4% of the volume of the steamer, and simultaneously the cooling water flow is controlled, so that the temperature of condensate discharged in the first half hour of the distillate is 20-25 ℃, the temperature of the condensate discharged in the second half hour is 50-55 ℃, and finally the weight of the distillate discharged is controlled to be 3 times of that of the eucommia leaves;
2) selecting branches of eucommia ulmoides, drying, crushing to obtain particles with the particle size not more than 50 meshes, soaking in 40% alcohol by weight for 5 hours, and applying ultrasonic waves to the branches, wherein the application mode of the ultrasonic waves is as follows: firstly, applying ultrasonic wave with the frequency of 350KHz for 1min and stopping for 0.5min, then applying ultrasonic wave with the frequency of 100KHz and stopping for 0.5min, circulating the application process of the ultrasonic wave for 6 times, and filtering to obtain powder and filtrate for later use;
3) selecting bark of eucommia ulmoides, drying, crushing to obtain particles with the particle size not more than 50 meshes, soaking the bark of eucommia ulmoides in sesame oil with the temperature of 70 ℃ for 3 hours according to the weight ratio of 1:4, filtering to obtain eucommia ulmoides powder, mixing the eucommia ulmoides powder and the powder obtained in the step 2) according to the weight ratio of 1:2, putting the mixture into an extraction reaction kettle, extracting with ethanol, and collecting an extract for later use;
4) uniformly mixing the extract obtained in the step 3), the filtrate obtained in the step 2) and the distillate obtained in the step 1) according to the weight ratio of 1:2:1, adding carbon powder accounting for 5% of the total weight of the extract, applying microwaves to the mixture to enable the temperature of the mixed solution to reach 90 ℃, keeping the mixed solution for 1 hour, naturally cooling the mixed solution, and filtering the carbon powder to obtain a filtrate for later use;
5) and (3) carrying out oil-water separation on the filtrate obtained in the step 4) by adopting a distillation method to obtain an oil phase, namely the product.
Example 2
A preparation method of eucommia ulmoides mixed essential oil comprises the following steps:
1) selecting fresh green leaves of eucommia ulmoides, cleaning the leaves with clear water, then placing the leaves above a sieve plate of a distillation kettle, adding a proper amount of water at the bottom of the distillation kettle, isolating the leaves from the eucommia ulmoides, and then distilling to obtain distillate generated by distillation for later use;
during distillation, the distillation speed is controlled to be 5% of the volume of the steamer, and simultaneously the cooling water flow is controlled, so that the temperature of condensate discharged in the first half hour of the distillate is 20-25 ℃, the temperature of the condensate discharged in the second half hour is 50-55 ℃, and finally the weight of the distillate discharged is controlled to be 3 times of that of the eucommia leaves;
2) selecting branches of eucommia ulmoides, drying, crushing to obtain particles with the particle size not more than 50 meshes, soaking in 50% alcohol according to the weight ratio of 1:5 for 3 hours, and then applying ultrasonic waves to the branches, wherein the application mode of the ultrasonic waves is as follows: firstly, applying ultrasonic wave with the frequency of 370KHz for 1min and stopping for 0.5min, then applying ultrasonic wave with the frequency of 120KHz and stopping for 0.5min, circulating the application process of the ultrasonic wave for 4 times, and filtering to obtain powder and filtrate for later use;
3) selecting bark of eucommia ulmoides, drying, crushing to obtain particles with the particle size not more than 50 meshes, soaking the bark of eucommia ulmoides in sesame oil with the temperature of 80 ℃ for 2 hours according to the weight ratio of 1:4, filtering to obtain eucommia ulmoides powder, mixing the eucommia ulmoides powder and the powder obtained in the step 2) according to the weight ratio of 1:2, putting the mixture into an extraction reaction kettle, extracting with ethanol, and collecting an extract for later use;
4) uniformly mixing the extract obtained in the step 3), the filtrate obtained in the step 2) and the distillate obtained in the step 1) according to the weight ratio of 1:2:1, adding carbon powder accounting for 5% of the total weight of the extract, applying microwaves to the mixture to enable the temperature of the mixed solution to reach 95 ℃, keeping the state for 0.5h, naturally cooling the mixed solution, and filtering the carbon powder to obtain a filtrate for later use;
5) and (3) carrying out oil-water separation on the filtrate obtained in the step 4) by adopting a distillation method to obtain an oil phase, namely the product.
Example 3
A preparation method of eucommia ulmoides mixed essential oil comprises the following steps:
1) selecting fresh green leaves of eucommia ulmoides, cleaning the leaves with clear water, then placing the leaves above a sieve plate of a distillation kettle, adding a proper amount of water at the bottom of the distillation kettle, isolating the leaves from the eucommia ulmoides, and then distilling to obtain distillate generated by distillation for later use;
during distillation, the distillation speed is controlled to be 4.5% of the volume of the steamer, and simultaneously the flow rate of cooling water is controlled, so that the temperature of condensate discharged in the first half hour of the distillate is 20-25 ℃, the temperature of condensate discharged in the half hour is 50-55 ℃, and finally the weight of the distillate discharged is controlled to be 3 times of that of the eucommia leaves;
2) selecting branches of eucommia ulmoides, drying, crushing to obtain particles with the particle size not more than 50 meshes, soaking in 45% alcohol by weight ratio of 1:5 for 4 hours, and applying ultrasonic waves to the branches, wherein the application mode of the ultrasonic waves is as follows: firstly, applying ultrasonic wave with the frequency of 360KHz for 1min and stopping for 0.5min, then applying ultrasonic wave with the frequency of 110KHz and stopping for 0.5min, circulating the application process of the ultrasonic wave for 5 times, and filtering to obtain powder and filtrate for later use;
3) selecting bark of eucommia ulmoides, drying, crushing to obtain particles with the particle size not more than 50 meshes, soaking the bark of eucommia ulmoides in sesame oil with the temperature of 75 ℃ for 2.5 hours according to the weight ratio of 1:4, filtering to obtain eucommia ulmoides powder, mixing the eucommia ulmoides powder and the powder obtained in the step 2) according to the weight ratio of 1:2, putting the mixture into an extraction reaction kettle, extracting by using ethanol, and collecting an extract for later use;
4) uniformly mixing the extract obtained in the step 3), the filtrate obtained in the step 2) and the distillate obtained in the step 1) according to the weight ratio of 1:2:1, adding carbon powder accounting for 5% of the total weight of the extract, applying microwaves to the mixture to enable the temperature of the mixed solution to reach 93 ℃, keeping the state for 0.8h, naturally cooling, and filtering the carbon powder to obtain a filtrate for later use;
5) and (3) carrying out oil-water separation on the filtrate obtained in the step 4) by adopting a distillation method to obtain an oil phase, namely the product.
Claims (3)
1. The preparation method of the eucommia ulmoides mixed essential oil is characterized by comprising the following steps of:
1) selecting fresh green leaves of eucommia ulmoides, cleaning the leaves with clear water, then placing the leaves above a sieve plate of a distillation kettle, adding a proper amount of water at the bottom of the distillation kettle, isolating the leaves from the eucommia ulmoides, and then distilling to obtain distillate generated by distillation for later use;
during distillation, the distillation speed is controlled to be 4-5% of the volume of the steamer, and simultaneously the flow rate of cooling water is controlled, so that the temperature of condensate discharged in the first half hour of the distillate is 20-25 ℃, the temperature of condensate discharged in the half hour is 50-55 ℃, and finally the weight of the distillate discharged is controlled to be 3 times of that of the eucommia leaves;
2) selecting branches of eucommia ulmoides, drying, crushing to obtain particles with the particle size not more than 50 meshes, soaking in alcohol with the volume concentration of 40-50% for 3-5h according to the weight ratio of 1:5, and then applying ultrasonic waves to the branches, wherein the application mode of the ultrasonic waves is as follows: firstly, applying ultrasonic wave with the frequency of 350-370KHz for 1min and stopping for 0.5min, then applying ultrasonic wave with the frequency of 100-120KHz and stopping for 0.5min, circulating the application process of the ultrasonic wave for 4-6 times, and filtering to obtain powder and filtrate for later use;
3) selecting bark of eucommia ulmoides, drying, crushing to obtain particles with the particle size not more than 50 meshes, soaking the bark of eucommia ulmoides in sesame oil with the temperature of 70-80 ℃ for 2-3 hours according to the weight ratio of 1:4, filtering to obtain eucommia ulmoides powder, mixing the eucommia ulmoides powder and the powder obtained in the step 2) according to the weight ratio of 1:2, putting the mixture into an extraction reaction kettle, extracting by using ethanol, and collecting an extract for later use;
4) uniformly mixing the extract obtained in the step 3), the filtrate obtained in the step 2) and the distillate obtained in the step 1) according to the weight ratio of 1:2:1, adding carbon powder accounting for 5% of the total weight of the extract, applying microwave to the mixture to enable the temperature of the mixed solution to reach 90-95 ℃, keeping the state for 0.5-1h, naturally cooling, and filtering the carbon powder to obtain a filtrate for later use;
5) and (3) carrying out oil-water separation on the filtrate obtained in the step 4) by adopting a distillation method to obtain an oil phase, namely the product.
2. The method for preparing eucommia ulmoides essential oil mixture according to claim 1, which is characterized in that: the bark of the eucommia bark is perennial bark, and the branch of the eucommia bark is annual twig.
3. The preparation method of eucommia ulmoides mixed essential oil according to claim 2, which is characterized by comprising the following steps: the bark of eucommia bark is selected from trunk bark which grows for more than six years.
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| CN115725368A (en) * | 2021-08-27 | 2023-03-03 | 杨美琳 | Preparation method of folium cortex eucommiae essential oil, folium cortex eucommiae essential oil and application |
| CN115721683A (en) * | 2021-08-27 | 2023-03-03 | 杨美琳 | Electronic atomized liquid and preparation and use methods thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1400299A (en) * | 2001-08-06 | 2003-03-05 | 张康健 | Method for continuously extracting eucommia oil and aucuboside from eucommia seed |
| JP2008031230A (en) * | 2006-07-27 | 2008-02-14 | Soda Aromatic Co Ltd | Agent for suppressing degradation smell of citral |
| CN102796610A (en) * | 2012-08-18 | 2012-11-28 | 湘西老爹生物有限公司 | Production technology for extracting eucommia oil and eucommia protein from eucommia kernels |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020178605A1 (en) * | 2001-05-21 | 2002-12-05 | Henry Aoki | Method of reduction of aroma extract and resulting extract |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1400299A (en) * | 2001-08-06 | 2003-03-05 | 张康健 | Method for continuously extracting eucommia oil and aucuboside from eucommia seed |
| JP2008031230A (en) * | 2006-07-27 | 2008-02-14 | Soda Aromatic Co Ltd | Agent for suppressing degradation smell of citral |
| CN102796610A (en) * | 2012-08-18 | 2012-11-28 | 湘西老爹生物有限公司 | Production technology for extracting eucommia oil and eucommia protein from eucommia kernels |
Non-Patent Citations (1)
| Title |
|---|
| 云南楚雄杜仲叶挥发油的化学成分分析;黄相中等;《云南民族大学学报(自然科学版)》;20110910;第20卷(第05期);356-360 * |
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