CN110591823A - Extraction and separation method of gardenia volatile oil - Google Patents
Extraction and separation method of gardenia volatile oil Download PDFInfo
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- CN110591823A CN110591823A CN201910935246.0A CN201910935246A CN110591823A CN 110591823 A CN110591823 A CN 110591823A CN 201910935246 A CN201910935246 A CN 201910935246A CN 110591823 A CN110591823 A CN 110591823A
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- gardenia
- volatile oil
- extraction
- reduced pressure
- carbon dioxide
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Classifications
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/022—Refining
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
-
- 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
Abstract
The invention relates to the technical field of plant extraction of essential oil, in particular to an extraction and separation method of gardenia volatile oil. According to the invention, the gardenia volatile oil is extracted from the gardenia by means of pretreatment, supercritical extraction, dewaxing and steam reduced pressure distillation, so that the purification efficiency of the gardenia volatile oil is effectively improved, and the high-purity gardenia volatile oil is obtained.
Description
Technical Field
The invention belongs to the technical field of essential oil extraction from plants, and particularly relates to an extraction and separation method of gardenia volatile oil.
Background
Gardenia jasminoides Ellis, a small evergreen shrub, is a plant belonging to the genus Gardenia of the family Rubiaceae. The gardenia is cultivated in the wild, has strong adaptability and is mainly distributed in tropical and subtropical regions. The gardenia is a fragrant flower plant of gardenia of rubiaceae, has strong cultivation adaptability, white flower and strong fragrance, and is one of the eight famous fragrant flowers in China. The gardenia is a rare natural spice, the contained effective component of gardenia volatile oil is used as a high-grade spice to be applied to various products, and the gardenia volatile oil has the effects of clearing heat and purging fire, treating fever, relieving pressure, moisturizing and moistening skin; according to research, the gardenia volatile oil contains linalool, jasmine lactone, farnesene, beta-myrcene, methyl benzoate, ocimene and other main components.
The plant essential oil is extracted from flower, leaf, root, bark, fruit, seed, resin, etc. of herbaceous plant by distillation and squeezing. The essential oil has high volatility and small molecular weight, and can be easily absorbed by human body, quickly permeate into internal organs of human body, and discharge redundant components out of human body, the whole process only needs several minutes, and the fragrance of the plant can directly stimulate the secretion of pituitary gland, the secretion of enzyme and hormone, etc., balance internal functions, and play a role in beautifying and protecting skin.
However, in the prior art, the gardenia plant essential oil extracted from the natural raw material of the gardenia has the defects of less volatile oil amount and low purification yield, thereby causing resource waste and being difficult to meet the market demand.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides an extraction and separation method of gardenia volatile oil, which is characterized in that the gardenia volatile oil is extracted from the gardenia in the modes of fermentation, supercritical extraction, dewaxing and steam reduced pressure distillation, so that the purification efficiency of the gardenia volatile oil is effectively improved, and the high-purity gardenia volatile oil is obtained.
In order to achieve the preset purpose, the invention adopts the technical scheme that:
an extraction and separation method of gardenia volatile oil comprises the following steps:
(1) pretreatment: selecting fresh gardenia, drying at 50-70 ℃ for 2-4h after cleaning, then cutting the gardenia into pieces, completely immersing the cut gardenia in salt water, sealing and fermenting at normal temperature for 4-6 days, and then filtering and washing to obtain a pretreatment raw material;
(2) supercritical extraction: extracting 25-50kg of pretreated raw material with high-pressure supercritical carbon dioxide, and charging gasified CO into the extractor2After extraction, CO is added2Inputting the mixed solution with the gardenia volatile oil into a separator, performing reduced pressure separation to obtain crude gardenia volatile oil, repeating the operation for 3-5 times, and combining the crude gardenia volatile oil obtained each time;
wherein the extraction pressure is 15-25MPa, the extraction temperature is 40-55 ℃, the extraction time is 60-90min, the carbon dioxide flow is 10L/h-15L/h, the pressure of carbon dioxide charging is 4-10MPa, the pressure in the separator is 8MPa-15MPa, and the temperature is 20-45 ℃;
(3) dewaxing: adding the combined gardenia volatile oil crude product obtained in the step (2) into an alcohol solvent, and performing centrifugation, precipitate removal and water washing to obtain dewaxed gardenia volatile oil;
(4) and (3) carrying out reduced pressure distillation on water vapor: and (3) carrying out steam reduced pressure distillation on the dewaxed gardenia volatile oil prepared in the step (3) at the temperature of 50-65 ℃, and taking distillate to obtain the gardenia volatile oil.
Preferably, the mass fraction of the saline solution in the step (1) is 10% -15%, and the volume ratio of the mass of the gardenia to the saline solution is 1 g: 4-6 mL.
Preferably, the alcohol solvent in the step (3) is absolute methanol, ethanol or edible n-butanol, and the volume ratio of the gardenia volatile oil crude product to the alcohol solvent is 1: 2-3.
Preferably, the centrifugation process of step (3) is: centrifuging at 10000rpm/min of 5000-.
Preferably, the pressure of the steam reduced pressure distillation in the step (4) is 0.03MPa-0.05MPa, and the time of the reduced pressure distillation is 3h-5 h.
Compared with the prior art, the invention has the beneficial effects that:
1. the method comprises the steps of drying the gardenia in a pretreatment stage until the water in the gardenia is reserved to 30-40%, expanding the cell holes on the surface of the leaves while finishing the water, facilitating the diffusion of volatile oil, enabling the oil yield to be 10-15% higher than that of fresh branches and branches, fermenting in salt water, further aging the cells on the surface of the leaves in the fermentation process, facilitating the precipitation of the essential oil, testing to prove that the oil yield after fermentation is 5-8% higher than that of the directly extracted gardenia without fermentation, after fermentation, carrying out high-pressure supercritical carbon dioxide extraction on the gardenia pretreatment raw material, fully contacting the supercritical carbon dioxide with the gardenia volatile oil under a supercritical state, and enabling the carbon dioxide to selectively extract the gardenia volatile oil components with different polarities, boiling points and molecular weights in sequence, and the pressure reduction separation is carried out in the separator, so that the carbon dioxide and the obtained gardenia volatile oil crude product are also separated, and an organic solvent is not required to be added in the high-pressure supercritical carbon dioxide extraction process, so that the waste of part of gardenia volatile oil in the purification process is avoided, and the high-pressure supercritical carbon dioxide extraction method realizes two technologies of extraction and separation without the separation step, so that 64-75% of gardenia volatile oil crude product is obtained in the high-pressure supercritical carbon dioxide extraction, and the crude extract with high purification yield is obtained by the pretreatment and supercritical extraction modes.
2. The method realizes the purification of the gardenia volatile oil through dewaxing and steam reduced pressure distillation, removes non-volatile essential oil, ester compounds and wax in the gardenia volatile oil crude product in the dewaxing process, removes part of alcohol solvent in the centrifugation process, and removes the alcohol solvent through multiple times of water washing.
Detailed Description
In order to make the technical solutions of the present invention better understood and enable those skilled in the art to practice the present invention, the following embodiments are further described, but the present invention is not limited to the following embodiments.
Example 1
An extraction and separation method of gardenia volatile oil comprises the following steps:
(1) pretreatment: selecting 26.5kg of fresh gardenia, drying at 50 ℃ for 4h after cleaning, then cutting the gardenia into pieces, adding the cut gardenia into 80L of salt solution with the mass fraction of 10%, sealing and fermenting for 6 days at normal temperature, and then removing the salt solution after filtering and deionized water washing to obtain a pretreatment raw material;
(2) supercritical extraction: extracting 25kg of pretreated raw material with high pressure supercritical carbon dioxide at 15MPa and 55 deg.C for 90min, and introducing gasified CO into the extractor2The flow rate of carbon dioxide is 10L/h, the pressure of carbon dioxide is 4Mpa, and CO is added after extraction2Inputting the mixed solution with the gardenia volatile oil into a separator for decompression separation, wherein the pressure in the separator is 8MPa, the temperature is 45 ℃, performing the operation for 5 times, and mixing the extraction liquid obtained after each extraction to obtain a gardenia volatile oil crude product;
(3) dewaxing: adding the gardenia volatile oil crude product obtained in the step (2) into an alcohol solvent, centrifuging for 20min at 12000, removing precipitates, and washing with deionized water for 8 times to obtain dewaxed gardenia volatile oil;
(4) and (3) carrying out reduced pressure distillation on water vapor: and (3) carrying out steam reduced pressure distillation on the dewaxed gardenia volatile oil prepared in the step (3) for 5 hours at the temperature of 50 ℃ and the pressure of 0.05Mpa, and taking distillate to obtain the gardenia volatile oil with the yield of 53%.
Example 2
(1) Pretreatment: selecting 42kg of fresh gardenia, drying the gardenia at 60 ℃ for 3h after cleaning, then shearing the gardenia into pieces, adding the cut gardenia into 126L of saline solution with the mass fraction of 12%, sealing and fermenting for 5 days at normal temperature, and then removing the saline solution after filtering and deionized water washing to obtain a pretreatment raw material;
(2) supercritical extraction: extracting 40kg of pretreated raw material with high pressure supercritical carbon dioxide at 20MPa and 50 deg.C for 75min, charging gasified CO into the extractor2The flow rate of carbon dioxide is 13L/h, the pressure of carbon dioxide is 8Mpa, and CO is added after extraction is finished2Inputting the mixed solution with the gardenia volatile oil into a separator for decompression separation, wherein the pressure in the separator is 12MPa, the temperature is 40 ℃, performing the operation for 4 times, and mixing the extraction liquid obtained after each extraction to obtain a gardenia volatile oil crude product;
(3) dewaxing: adding the gardenia volatile oil crude product obtained in the step (2) into an alcohol solvent, centrifuging for 15min at 15000rpm/min, removing precipitates, and washing with deionized water for 7 times to obtain dewaxed gardenia volatile oil;
(4) and (3) carrying out reduced pressure distillation on water vapor: and (3) carrying out steam reduced pressure distillation on the dewaxed gardenia volatile oil prepared in the step (3) at the temperature of 55 ℃ and the pressure of 0.04Mpa for 4 hours, and taking distillate to obtain the gardenia volatile oil with the yield of 58%.
Example 3
(1) Pretreatment: selecting 53kg of fresh gardenia, drying at 70 ℃ for 2h after cleaning, then shearing the gardenia into pieces, adding the pieces into 318L of salt water with the mass fraction of 15%, sealing and fermenting for 4 days at normal temperature, and then filtering and washing to obtain a pretreatment raw material;
(2) supercritical extraction: extracting 50kg of pretreated raw material with high pressure supercritical carbon dioxide at 25MPa and 40 deg.C for 60min, and introducing gasified CO into the extractor2The flow rate of carbon dioxide is 15L/h, the pressure of carbon dioxide is 10Mpa, and CO is added after extraction is finished2Separating the mixed solution with Gardenia volatile oil under reduced pressure in a separator at pressure of 15MPa and temperature of 20 deg.C for 3 times, and mixing the extractive solutionsMixing to obtain crude product of volatile oil of Gardenia;
(3) dewaxing: adding the gardenia volatile oil crude product obtained in the step (2) into an alcohol solvent, centrifuging at 20000rpm/min for 10min, removing precipitates, and washing with deionized water for 6 times to obtain dewaxed gardenia volatile oil;
(4) and (3) carrying out reduced pressure distillation on water vapor: and (3) carrying out steam reduced pressure distillation on the dewaxed gardenia volatile oil prepared in the step (3) for 3 hours at the temperature of 65 ℃ and the pressure of 0.03Mpa, and taking distillate to obtain the gardenia volatile oil with the yield of 63%.
The gardenia volatile oil prepared by the preparation method of the example 1-the example 3 is colorless and transparent, has rich fragrance, and has the same fragrance as that of a standard product, and since the gardenia volatile oil of the example 1-the example 3 has the same color and fragrance as those of a standard product, the gardenia volatile oil of the example 2 is taken as an example, and the yield, color and fragrance of the invention are compared and explained with those of the gardenia volatile oil samples obtained in the comparison 1-the comparison 4.
Comparative example 1
The same procedure as in example 2 was followed, except that the pretreatment process of step (1) was carried out as follows: selecting fresh gardenia, cleaning, and directly fermenting in salt water without drying.
Comparative example 2
The same procedure as in example 2 was followed, except that the pretreatment process of step (1) was carried out as follows: selecting fresh gardenia, cleaning, drying at 60 ℃ for 3h, and not fermenting.
Comparative example 3
The same procedure as in example 2 was conducted except that the steam distillation under reduced pressure step of step (4) was not conducted.
Comparative example 4
Extracting fresh gardenia at normal temperature by using petroleum ether, filtering, concentrating under reduced pressure to obtain an extract, and dewaxing the obtained extract by using absolute ethyl alcohol at the low temperature of between 15 ℃ below zero and 20 ℃ below zero to obtain gardenia volatile oil (the gardenia volatile oil extraction method in the prior art).
The following comparisons of the yields, colors and fragrances were made for the samples of example 2 and comparative examples 1-3, and the results are shown in Table 1:
compared with the comparative examples 1 and 2, the example 2 has similar color and fragrance as the example 2, but the yield of the gardenia volatile oil is obviously lower than that of the sample in the example 2, which shows that the drying and fermentation processes in the pretreatment process have great influence on the yield of the gardenia volatile oil; however, the gardenia volatile oil obtained in example 2, comparative example 1 and comparative example 2 has a high content, so that there is no obvious difference in color and fragrance.
Example 2 compared with comparative example 3, the yield is higher than that of example 2 because comparative example 3 does not carry out the steam reduced pressure distillation step, but impurities still remain in the gardenia volatile oil after dewaxing, so the steam reduced pressure distillation step of the last step effectively purifies the gardenia volatile oil to obtain the high-purity gardenia volatile oil; example 4 is the gardenia volatile oil extraction method in the prior art, and compared with comparative example 4, example 2 has a yield, a fragrance and a color which are obviously superior to those of comparative example 4, which shows that the extraction and separation method of gardenia volatile oil of the present invention is superior to the prior art.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (5)
1. An extraction and separation method of gardenia volatile oil is characterized by comprising the following steps:
(1) pretreatment: selecting fresh gardenia, drying at 50-70 ℃ for 2-4h after cleaning, then cutting the gardenia into pieces, completely immersing the cut gardenia in salt water, sealing and fermenting at normal temperature for 4-6 days, and then filtering and washing to obtain a pretreatment raw material;
(2) supercritical extraction: extracting 25-50kg of pretreated raw material with high-pressure supercritical carbon dioxide, and charging gasified CO into the extractor2After extraction, CO is added2Separating under reduced pressure with the mixture of volatile oil to obtain crude volatile oil, repeating the above steps for 3-5 times, and mixing the crude volatile oil obtained each time;
wherein the extraction pressure is 15-25MPa, the extraction temperature is 40-55 ℃, the extraction time is 60-90min, the carbon dioxide flow is 10-15L/h, the carbon dioxide charging pressure is 4-10MPa, the pressure in the separator is 8MPa-15MPa, and the temperature is 20-45 ℃;
(3) dewaxing: adding the combined gardenia volatile oil crude product obtained in the step (2) into an alcohol solvent, and performing centrifugation, precipitate removal and water washing to obtain dewaxed gardenia volatile oil;
(4) and (3) carrying out reduced pressure distillation on water vapor: and (3) carrying out steam reduced pressure distillation on the dewaxed gardenia volatile oil prepared in the step (3) at the temperature of 50-65 ℃, and taking distillate to obtain the gardenia volatile oil.
2. The extraction and separation method of gardenia volatile oil according to claim 1, wherein the mass fraction of the saline solution in the step (1) is 10% -15%, and the volume ratio of the mass of gardenia to the saline solution is 1 g: 3-4 mL.
3. The extraction and separation method of gardenia volatile oil according to claim 1, characterized in that the alcohol solvent in step (3) is absolute methanol, ethanol or edible n-butanol, and the volume ratio of the gardenia volatile oil crude product to the alcohol solvent is 1: 2-3.
4. The method for extracting and separating gardenia volatile oil according to claim 1, wherein the centrifugation process in the step (3) is as follows: centrifuging at 12000-20000rpm/min for 10-20 min.
5. The method for extracting and separating gardenia volatile oil according to claim 1, wherein the pressure of the steam reduced pressure distillation in the step (4) is 0.03Mpa to 0.05Mpa, and the time of the reduced pressure distillation is 3h to 5 h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113230158A (en) * | 2021-05-26 | 2021-08-10 | 南京中医药大学 | Gardenia composite extract capable of improving antioxidant activity and application thereof |
| CN114891563A (en) * | 2021-01-29 | 2022-08-12 | 香奈儿美容香水公司 | Gardenia oil extract and cosmetic composition containing the same |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114891563A (en) * | 2021-01-29 | 2022-08-12 | 香奈儿美容香水公司 | Gardenia oil extract and cosmetic composition containing the same |
| CN113230158A (en) * | 2021-05-26 | 2021-08-10 | 南京中医药大学 | Gardenia composite extract capable of improving antioxidant activity and application thereof |
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Application publication date: 20191220 |