CN111196950A - Method for extracting citronella essential oil - Google Patents

Method for extracting citronella essential oil Download PDF

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Publication number
CN111196950A
CN111196950A CN201811371169.2A CN201811371169A CN111196950A CN 111196950 A CN111196950 A CN 111196950A CN 201811371169 A CN201811371169 A CN 201811371169A CN 111196950 A CN111196950 A CN 111196950A
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China
Prior art keywords
citronella
essential oil
extraction
extracting
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.)
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Application number
CN201811371169.2A
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Chinese (zh)
Inventor
叶桂银
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Nanjing Emont Biotechnology Co Ltd
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Nanjing Emont Biotechnology Co Ltd
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Priority to CN201811371169.2A priority Critical patent/CN111196950A/en
Publication of CN111196950A publication Critical patent/CN111196950A/en
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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
    • C11B9/025Recovery by solvent extraction
    • 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

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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)
  • Fats And Perfumes (AREA)
  • Extraction Or Liquid Replacement (AREA)

Abstract

The invention relates to a method for extracting essential oil from a natural plant citronella, which comprises the following steps: (1) cleaning fresh citronella, soaking in water, placing into a screen basket, and soaking in liquid nitrogen for 2-3 times; (2) drying the citronella in the step (1) at a low temperature, and crushing to obtain citronella powder; (3) extracting citronella powder by a supercritical CO2 extraction method; (4) and (4) 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 the citronella essential oil. The extraction method of the citronella essential oil provided by the invention avoids considering the loss of effective components in the citronella extraction process, and improves the quality and yield of the citronella essential oil.

Description

Method for extracting citronella essential oil
Technical Field
The invention relates to a method for extracting natural plant essential oil, in particular to a method for extracting citronella essential oil.
Background
Citronella is a perennial herb of the citronella, is native to south India and Sri Lanka, and common varieties are Cistus citrina in West India and Cistus citrina in east India. The citronella essential oil extracted from citronella can be used for preparing industrial daily chemicals such as mosquito repellents, high-grade perfumes, shampoos, cosmetics and the like, besides, the citronella essential oil is used for treating fever, anxiety and the like caused by cold in some countries and regions, and the citronella essential oil is developed and utilized as a health-care tea for clearing heat and removing toxicity in countries such as Brazil and the like.
The citronella essential oil also has great benefits for refreshing the brain, purifying the room and softening the skin; it can also be used for cleaning oily skin and sweaty feet. Essential oils are very volatile and evaporate quickly upon contact with air, and for this reason they must be stored in sealable bottles and capped quickly once the bottle is opened for use. A few drops of citronella essential oil are dripped into hot water for soaking feet, so that the purpose of activating blood and channels and collaterals can be achieved, and the effect of removing beriberi and foot odor can also be achieved.
In the prior art, water distillation, solvent extraction, supercritical fluid extraction, direct steam distillation and microwave-assisted extraction processes are applied to extraction research of citronella essential oil, while ultrasonic extraction and semi-bionic extraction techniques are less applied to extraction research of essential oil in 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 for citronella essential oil, which avoids the loss of effective components in citronella treatment.
In order to achieve the above object, the present invention is implemented by the following technical solutions: a method for extracting citronella essential oil comprises the following steps:
(1) cleaning and soaking fresh citronella stems and leaves in water, then putting the stems and leaves into a screen basket, totally immersing the stems and leaves in liquid nitrogen for 30-60min, then lifting the screen basket, placing the screen basket at room temperature for 5-10min, totally immersing the screen basket in the liquid nitrogen for 30-60min, and repeating the steps for 2-3 times;
(2) drying the citronella in the step (1) at a low temperature, crushing, and sieving with a 5-30-mesh sieve to obtain citronella powder;
(3) mixing citronella powder and solvent uniformly, placing into an extraction kettle, introducing supercritical CO2 into the extraction kettle, controlling the temperature of the extraction kettle at 40-50 ℃ and the extraction pressure at 30-45 Mpa;
(4) and (4) 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 the citronella essential oil.
By immersing the stems and leaves of the citronella which are rich in water into the low-temperature liquid nitrogen, the water in the cell sap is frozen, the volume is enlarged, the cell wall is punctured, the effective components in the citronella cells are promoted to be separated out, and then the stems and leaves are dried under the low-temperature condition, so that the effective components in the citronella are ensured not to be lost. According to the invention, the low-temperature vacuum drying process comprises the following steps: the citronella is alternately stacked in a vacuum drying box, the vacuum degree is controlled to be 0.009-0.36Mpa, and the temperature of vacuum drying is 40-52 ℃.
Preferably, the citronella is dried until the water content is below 5%.
According to the present invention, in order to further precipitate the effective components in the citronella, the citronella powder is fully mixed with 0.01-0.08 times of weight of biological enzyme before being implanted into the extraction kettle, and is left for 30-60min, the cell wall of the citronella is decomposed by the biological enzyme, preferably, the biological enzyme is at least one of β -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 citronella essential oil provided by the invention effectively avoids the loss of effective components in the citronella extraction process, and improves the quality and yield of the citronella 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 citronella essential oil comprises the following steps:
(1) cleaning fresh citronella, soaking in water for 25min, placing into a screen basket, totally immersing in liquid nitrogen for 50min, lifting, placing at room temperature for 8min, totally immersing the screen basket in liquid nitrogen for 50min, and repeating the steps for 3 times;
(2) drying the citronella in the step (1) at a low temperature, crushing, and sieving with a 20-mesh sieve to obtain citronella powder;
the low-temperature vacuum drying process comprises the following steps: alternately stacking the citronella in a vacuum drying box, controlling the vacuum degree to be 0.009Mpa, the vacuum drying temperature to be 40 ℃, and drying the citronella until the water content is below 5%;
(3) mixing citronella powder with β -glucosidase 0.05 times the weight of citronella powder, 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 (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 8Mpa, and the temperature is 28 ℃, so as to obtain the citronella essential oil.
Example 2:
a method for extracting citronella essential oil comprises the following steps:
(1) cleaning fresh citronella, soaking in water for 20min, placing into a screen basket, totally immersing in liquid nitrogen for 30min, lifting, placing at room temperature for 5min, totally immersing the screen basket in liquid nitrogen for 30min, and repeating the steps for 2 times;
(2) drying the citronella in the step (1) at a low temperature, crushing, and sieving with a 5-mesh sieve to obtain citronella powder;
the low-temperature vacuum drying process comprises the following steps: alternately stacking the citronella in a vacuum drying box, controlling the vacuum degree to be 0.009Mpa, the vacuum drying temperature to be 40 ℃, and drying the citronella until the water content is below 5%;
(3) mixing herba Cymbopogonis Citrari powder with 0.01 times weight of pectase, stirring, 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 (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 5Mpa, and the temperature is 20 ℃, so as to obtain the citronella essential oil.
Example 3:
a method for extracting citronella essential oil comprises the following steps:
(1) cleaning fresh citronella, soaking in water for 30min, placing into a screen basket, totally immersing in liquid nitrogen for 60min, lifting, placing at room temperature for 10min, totally immersing the screen basket in liquid nitrogen for 60min, and repeating the steps for 3 times;
(2) drying the citronella in the step (1) at a low temperature, crushing, and sieving with a 30-mesh sieve to obtain citronella powder;
the low-temperature vacuum drying process comprises the following steps: alternately stacking the citronella in a vacuum drying box, controlling the vacuum degree to be 0.009Mpa, the vacuum drying temperature to be 40 ℃, and drying the citronella until the water content is below 5%;
(3) fully and uniformly stirring citronella powder and 0.08 times of cellulase, standing for 60min, uniformly mixing the citronella powder and acetone, putting the mixture into an extraction kettle, introducing supercritical CO2 into the extraction kettle, and controlling the temperature and the extraction pressure of the extraction kettle to be 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 citronella 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 citronella essential oil is characterized by comprising the following steps:
(1) cleaning fresh citronella, soaking in water, placing into a screen basket, totally immersing in liquid nitrogen for 30-60min, lifting, placing at room temperature for 5-10min, totally immersing the screen basket in liquid nitrogen for 30-60min, and repeating the steps for 2-3 times;
(2) drying the citronella in the step (1) at a low temperature, crushing, and sieving with a 5-30-mesh sieve to obtain citronella powder;
(3) mixing citronella powder and solvent uniformly, placing into an extraction kettle, introducing supercritical CO2 into the extraction kettle, controlling the temperature of the extraction kettle at 40-50 ℃ and the extraction pressure at 30-45 Mpa;
(4) and (4) 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 the citronella essential oil.
2. The method for extracting citronella essential oil according to claim 1, wherein in step (3), citronella powder is fully and uniformly mixed with 0.01-0.08 times of weight of biological enzyme before being placed in an extraction kettle, and is kept still for 30-60min, wherein the biological enzyme is one of β -glucosidase, pectinase and cellulase.
3. The method for extracting citronella essential oil according to claim 1, wherein the method comprises the following steps: in the step (2), the citronella is dried in vacuum at low temperature, and the process comprises the following steps: alternately stacking the citronella in a vacuum drying oven, controlling the vacuum degree to be 0.009-0.36Mpa, and the vacuum drying temperature to be 40-52 ℃.
4. The method for extracting citronella essential oil according to claim 1, wherein the method comprises the following steps: in the step (2), the citronella is dried until the water content is below 5%.
5. The method for extracting citronella essential oil according to claim 1, wherein the method 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 citronella essential oil according to claim 1, wherein the method comprises the following steps: in the step (4), the pressure of the separation kettle is 7-9Mpa, and the temperature is 25-30 ℃.
CN201811371169.2A 2018-11-18 2018-11-18 Method for extracting citronella essential oil Withdrawn CN111196950A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811371169.2A CN111196950A (en) 2018-11-18 2018-11-18 Method for extracting citronella essential oil

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811371169.2A CN111196950A (en) 2018-11-18 2018-11-18 Method for extracting citronella essential oil

Publications (1)

Publication Number Publication Date
CN111196950A true CN111196950A (en) 2020-05-26

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CN201811371169.2A Withdrawn CN111196950A (en) 2018-11-18 2018-11-18 Method for extracting citronella essential oil

Country Status (1)

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CN (1) CN111196950A (en)

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Application publication date: 20200526

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