CN110540904A - method for extracting wormwood essential oil - Google Patents

method for extracting wormwood essential oil Download PDF

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Publication number
CN110540904A
CN110540904A CN201810526854.1A CN201810526854A CN110540904A CN 110540904 A CN110540904 A CN 110540904A CN 201810526854 A CN201810526854 A CN 201810526854A CN 110540904 A CN110540904 A CN 110540904A
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CN
China
Prior art keywords
folium artemisiae
artemisiae argyi
essential oil
extraction
steps
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
CN201810526854.1A
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Chinese (zh)
Inventor
杨成东
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Jiangsu Able Biotechnology Co Ltd
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Jiangsu Able Biotechnology Co Ltd
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Priority to CN201810526854.1A priority Critical patent/CN110540904A/en
Publication of CN110540904A publication Critical patent/CN110540904A/en
Withdrawn legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/022Refining
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/025Recovery by solvent extraction

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Extraction Or Liquid Replacement (AREA)
  • Fats And Perfumes (AREA)

Abstract

The invention relates to a method for extracting wormwood essential oil, and relates to a method for extracting essential oil from a natural plant, namely folium artemisiae argyi, which comprises the following steps: (1) cleaning fresh folium Artemisiae Argyi stems and leaves, soaking in water, placing into sieve basket, soaking in liquid nitrogen, and repeating for 2-3 times; (2) drying the folium artemisiae argyi in the step (1) at a low temperature, and crushing to obtain folium artemisiae argyi powder; (3) extracting folium Artemisiae Argyi powder by supercritical CO2 extraction method; (4) and (3) allowing CO2 containing the extract to flow out of the extraction kettle, and allowing the extract to enter a separation kettle for reduced pressure separation to obtain folium Artemisiae Argyi essential oil. The extraction method of the folium artemisiae argyi essential oil avoids considering the loss of effective components in the folium artemisiae argyi extraction process, and improves the quality and the yield of the folium artemisiae argyi essential oil.

Description

method for extracting wormwood essential oil
Technical Field
the invention relates to a method for extracting natural plant essential oil, in particular to a method for extracting folium artemisiae argyi essential oil.
background
folium Artemisiae Argyi, perennial herb or slightly half-shrub, the plant has strong fragrance, and has effects of warming channels, removing dampness, dispelling cold, stopping bleeding, diminishing inflammation, relieving asthma, relieving cough, preventing miscarriage, and resisting allergy. The folium Artemisiae Argyi essential oil is volatile aromatic substance extracted from leaves and stems of folium Artemisiae Argyi, is generally light yellow or yellowish green, has effects of warming channels, dredging collaterals, invigorating qi, promoting blood circulation, dispelling cold, relieving pain, improving local circulation, and enhancing immunity, and is usually applied to acupuncture point or affected part, and repeatedly kneaded to be absorbed. The folium Artemisiae Argyi essential oil contains mainly small molecule volatile terpenoid, and also contains aliphatic compounds and small molecule aromatic compounds.
In the prior art, water distillation, solvent extraction, supercritical fluid extraction, direct steam distillation and microwave-assisted extraction processes are applied to the extraction research of the folium artemisiae argyi essential oil, and the ultrasonic extraction process and the semi-bionic extraction process are less applied to the extraction research of the essential oil of enterprises. The water distillation and solvent extraction methods inevitably cause changes in the components, thereby changing the overall flavor profile, and often lose top note, the product loses freshness, and contamination with solvent residues is difficult to avoid. And supercritical CO2
The CO2 fluid has a special solubility effect on organic matters. The technology has unique advantages for separating macromolecular, heat-sensitive or chemically unstable substances which are difficult to solve by the traditional separation method, so that the technology receives wide attention in the fields of food, spice, medicine, chemical industry and the like.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide an extraction method of folium artemisiae argyi essential oil, which avoids the loss of effective components in the processing of folium artemisiae argyi.
in order to achieve the above object, the present invention is implemented by the following technical solutions: a method for extracting wormwood essential oil comprises the following steps:
(1) cleaning fresh folium Artemisiae Argyi stems and leaves, soaking in water, placing into screen basket, totally immersing in liquid nitrogen for 30-60min, lifting, placing at room temperature for 5-10min, totally immersing screen basket in liquid nitrogen for 30-60min, and repeating for 2-3 times;
(2) Drying the folium artemisiae argyi in the step (1) at a low temperature, crushing, and sieving with a 5-30-mesh sieve to obtain folium artemisiae argyi powder;
(3) Uniformly mixing the wormwood powder and a solvent, placing the mixture into an extraction kettle, introducing supercritical CO2 into the extraction kettle, controlling the temperature of the extraction kettle to be 40-50 ℃ and the extraction pressure to be 30-45 Mpa;
(4) and (3) allowing CO2 containing the extract to flow out of the extraction kettle, and allowing the extract to enter a separation kettle for reduced pressure separation to obtain folium Artemisiae Argyi essential oil.
By immersing the stem leaves of the folium artemisiae argyi rich in water into low-temperature liquid nitrogen, water in cell sap is frozen, the volume is enlarged, cell walls are punctured, effective ingredients in folium artemisiae argyi cells are promoted to be separated out, and then drying is carried out under the low-temperature condition, so that the effective ingredients in the folium artemisiae argyi are prevented from losing. According to the invention, the low-temperature vacuum drying process comprises the following steps: alternately stacking folium Artemisiae Argyi in vacuum drying oven, controlling vacuum degree at 0.009-0.36Mpa, and vacuum drying at 40-52 deg.C.
preferably, the wormwood is dried until the water content is below 5%.
according to the invention, in order to further separate out effective components in the folium artemisiae argyi, the folium artemisiae argyi powder is fully mixed with 0.01-0.08 times of biological enzyme and stands for 30-60min before being implanted into an extraction kettle, the cell wall of the folium artemisiae argyi is decomposed by the biological enzyme, and the biological enzyme is preferably at least one of beta-glucosidase, pectinase and cellulase.
According to the present invention, in order to facilitate the subsequent removal of the solvent, the solvent of the present invention is a low boiling point solvent, and preferably, the solvent is at least one of acetone, ethanol, methanol and dichloromethane.
according to the invention, the pressure of the separation kettle is 7-9Mpa, and the temperature is 25-30 ℃.
compared with the prior art, the extraction method of the folium artemisiae argyi essential oil provided by the invention effectively avoids the loss of effective components in the folium artemisiae argyi extraction process, and improves the quality and yield of the folium artemisiae argyi essential oil.
The specific implementation mode is as follows:
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further clarified by combining the specific embodiments in the next work.
Example 1:
A method for extracting wormwood essential oil comprises the following steps:
(1) cleaning fresh folium Artemisiae Argyi stems and leaves, soaking in water for 25min, placing into screen basket, totally soaking in liquid nitrogen for 50min, lifting, placing at room temperature for 8min, totally soaking screen basket in liquid nitrogen for 50min, and repeating the above steps for 3 times;
(2) Drying the folium artemisiae argyi in the step (1) at a low temperature, crushing, and sieving with a 20-mesh sieve to obtain folium artemisiae argyi powder;
The low-temperature vacuum drying process comprises the following steps: piling folium Artemisiae Argyi in a vacuum drying oven in a staggered manner, controlling the vacuum degree at 0.009Mpa and the vacuum drying temperature at 40 deg.C, and oven drying folium Artemisiae Argyi until the water content is below 5%;
(3) Mixing folium Artemisiae Argyi powder and 0.05 times weight of beta-glucosidase thoroughly, standing for 50min, mixing with acetone, placing into an extraction kettle, introducing supercritical CO2 into the extraction kettle, controlling the temperature of the extraction kettle at 45 deg.C and the extraction pressure at 40 Mpa;
(4) and allowing CO2 containing the extract to flow out of the extraction kettle, and allowing the extract to enter a separation kettle for reduced pressure separation, wherein the pressure of the separation kettle is 8Mpa, and the temperature is 28 deg.C, to obtain folium Artemisiae Argyi essential oil.
example 2:
A method for extracting wormwood essential oil comprises the following steps:
(1) Cleaning fresh folium Artemisiae Argyi stems and leaves, soaking in water for 20min, placing into screen basket, totally soaking in liquid nitrogen for 30min, lifting, placing at room temperature for 5min, totally soaking screen basket in liquid nitrogen for 30min, and repeating for 2 times;
(2) drying the folium artemisiae argyi in the step (1) at a low temperature, crushing, and sieving with a 5-mesh sieve to obtain folium artemisiae argyi powder;
The low-temperature vacuum drying process comprises the following steps: piling folium Artemisiae Argyi in a vacuum drying oven in a staggered manner, controlling the vacuum degree at 0.009Mpa and the vacuum drying temperature at 40 deg.C, and oven drying folium Artemisiae Argyi until the water content is below 5%;
(3) Mixing folium Artemisiae Argyi powder with 0.01 times weight of pectase, standing for 30min, mixing with ethanol, placing into an extraction kettle, introducing supercritical CO2 into the extraction kettle, controlling the temperature of the extraction kettle at 40 deg.C and the extraction pressure at 30 Mpa;
(4) And allowing CO2 containing the extract to flow out of the extraction kettle, and separating under reduced pressure in a separation kettle at 20 deg.C under 5Mpa to obtain folium Artemisiae Argyi essential oil.
Example 3:
a method for extracting wormwood essential oil comprises the following steps:
(1) cleaning fresh folium Artemisiae Argyi stems and leaves, soaking in water for 30min, placing into screen basket, totally soaking in liquid nitrogen for 60min, lifting, placing at room temperature for 10min, totally soaking screen basket in liquid nitrogen for 60min, and repeating the above steps for 3 times;
(2) Drying the folium artemisiae argyi in the step (1) at a low temperature, crushing, and sieving with a 30-mesh sieve to obtain folium artemisiae argyi powder;
The low-temperature vacuum drying process comprises the following steps: piling folium Artemisiae Argyi in a vacuum drying oven in a staggered manner, controlling the vacuum degree at 0.009Mpa and the vacuum drying temperature at 40 deg.C, and oven drying folium Artemisiae Argyi until the water content is below 5%;
(3) uniformly mixing folium Artemisiae Argyi powder with 0.08 times weight of cellulase, standing for 60min, mixing with acetone, placing into an extraction kettle, introducing supercritical CO2 into the extraction kettle, controlling the temperature of the extraction kettle at 50 deg.C and the extraction pressure at 45 Mpa;
(4) And (3) allowing CO2 containing the extract to flow out of the extraction kettle, and allowing the extract to enter a separation kettle for reduced pressure separation, wherein the pressure of the separation kettle is 10Mpa, and the temperature is 30 ℃, so as to obtain the folium artemisiae argyi essential oil.
the foregoing shows and describes the general principles, essential features, and inventive features of this invention. The present invention is not limited to the above-described embodiments, and the above-described embodiments and the description are only for illustrating the principle of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the present invention, and these changes and modifications are all within the scope of the present invention.

Claims (6)

1. the extraction method of the folium artemisiae argyi essential oil is characterized by comprising the following steps:
(1) cleaning fresh folium Artemisiae Argyi stems and leaves, soaking in water, placing into screen basket, totally immersing in liquid nitrogen for 30-60min, lifting, placing at room temperature for 5-10min, totally immersing screen basket in liquid nitrogen for 30-60min, and repeating for 2-3 times;
(2) Drying the folium artemisiae argyi in the step (1) at a low temperature, crushing, and sieving with a 5-30-mesh sieve to obtain folium artemisiae argyi powder;
(3) uniformly mixing the wormwood powder and a solvent, placing the mixture into an extraction kettle, introducing supercritical CO2 into the extraction kettle, controlling the temperature of the extraction kettle to be 40-50 ℃ and the extraction pressure to be 30-45 Mpa;
(4) and (3) allowing CO2 containing the extract to flow out of the extraction kettle, and allowing the extract to enter a separation kettle for reduced pressure separation to obtain folium Artemisiae Argyi essential oil.
2. The method for extracting essential oil of artemisia argyi as claimed in claim 1, which comprises the following steps: in the step (3), the folium artemisiae argyi powder is fully and uniformly mixed with 0.01-0.08 times of biological enzyme before being placed in an extraction kettle, and is kept stand for 30-60min, wherein the biological enzyme is one of beta-glucosidase, pectinase and cellulase.
3. the method for extracting essential oil of artemisia argyi as claimed in claim 1, which comprises the following steps: in the step (2), the folium artemisiae argyi is dried in vacuum at low temperature, and the process comprises the following steps: alternately stacking folium Artemisiae Argyi in vacuum drying oven, controlling vacuum degree at 0.009-0.36Mpa, and vacuum drying at 40-52 deg.C.
4. The method for extracting essential oil of artemisia argyi as claimed in claim 1, which comprises the following steps: in the step (2), the wormwood is dried until the water content is below 5%.
5. the method for extracting essential oil of artemisia argyi as claimed in claim 1, which comprises the following steps: the solvent is a low-boiling point solvent, and preferably, the solvent is at least one of acetone, ethanol, diethyl ether, methanol and dichloromethane.
6. The method for extracting essential oil of artemisia argyi as claimed in claim 1, which comprises the following steps: in the step (4), the pressure of the separation kettle is 7-9Mpa, and the temperature is 25-30 ℃.
CN201810526854.1A 2018-05-29 2018-05-29 method for extracting wormwood essential oil Withdrawn CN110540904A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111019763A (en) * 2019-12-27 2020-04-17 南洋金鳄(成都)生物工程有限公司 Artemisia argyi extraction method without toxic and side effects

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111019763A (en) * 2019-12-27 2020-04-17 南洋金鳄(成都)生物工程有限公司 Artemisia argyi extraction method without toxic and side effects

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Application publication date: 20191206