CN108559635B - Extraction process of perilla oil - Google Patents
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- CN108559635B CN108559635B CN201810535059.9A CN201810535059A CN108559635B CN 108559635 B CN108559635 B CN 108559635B CN 201810535059 A CN201810535059 A CN 201810535059A CN 108559635 B CN108559635 B CN 108559635B
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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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Abstract
The invention discloses an extraction process of perilla oil, belonging to the technical field of essential oil extraction and comprising the following steps: (1) pulverizing folium Perillae to obtain Perillae herba powder; (2) putting the perilla powder into an extraction kettle, adding 2-5 times of an extracting agent by weight, and extracting by using subcritical butane to obtain an extract liquid; (3) separating the extractive solution to obtain solvent and mixed oil of Perillae herba, recovering solvent, introducing into solvent tank, collecting mixed oil of Perillae herba, and further processing to obtain Perilla oil. By improving the extraction process, the loss of the perilla essential oil is less, and the extraction rate is high.
Description
Technical Field
The invention relates to the technical field of essential oil extraction, and particularly relates to a perilla herb oil extraction process.
Background
Perilla frutescens, which is pungent and warm in nature and has the aroma of perilla frutescens, is mainly used in the pharmaceutical and food industries. The perilla herb oil also contains rich alpha-linolenic acid, and has obvious health care effect and medical efficacy on human bodies. The extraction process of perilla herb oil in the prior art comprises a low-temperature squeezing process, a supercritical fluid extraction process and the like.
Chinese patent publication No. CN106135466A discloses a high-efficiency extraction process of perilla oil, which comprises the following steps: step 1: collecting fructus Perillae, air drying or oven drying to make water content of the seed less than 8%; selecting raw materials and removing impurities to ensure that the purity of grains reaches more than 99 percent; step 2: carrying out primary squeezing extraction by adopting a double-screw cold squeezer; and step 3: precipitating and finely filtering the crude oil obtained in the step 2 to obtain a primary extracted oil product; and 4, step 4: crushing the cake obtained in the step 2, sieving the crushed cake with a 40-mesh sieve, and performing secondary squeezing extraction in a supercritical extraction system to obtain a secondary extracted oil product; and 5: after two times of extraction, the residual rate of the oil and fat in the obtained cake is lower than 2%. The invention combines the advantages and disadvantages of the cold pressing method and the supercritical extraction method, the extraction rate can reach more than 98%, but the process is complicated and the cost is high.
The response surface optimization and the chemical composition research of the perilla essential oil microwave extraction process disclosed in the university of Jiangjiang river school newspaper of Linmennan et al specifically disclose that the optimal process parameters of the microwave extraction are as follows: cyclohexane is used as an extracting agent, the microwave power is 329W, the microwave time is 80 s, and the material-liquid ratio is 1: and 6, soaking for 56 min, wherein the actual yield is 1.783%, and analyzing by a gas chromatography-mass spectrometer to identify 17 substances in the perilla essential oil, wherein the contents of perillaldehyde and limonene are the highest. The extraction agent adopted by the method is cyclohexane, and partial components with larger polarity cannot be extracted, so that the extraction rate is lower.
Disclosure of Invention
In view of the above, the present invention provides a perilla herb oil extraction process, which is improved to reduce loss of perilla herb essential oil and increase extraction rate.
The technical scheme of the invention is as follows:
a perilla herb oil extraction process comprises the following steps:
(1) pulverizing folium Perillae to obtain Perillae herba powder;
(2) putting the perilla powder into an extraction kettle, adding 2-5 times of an extracting agent by weight, and extracting by using subcritical butane to obtain an extract liquid;
(3) separating the extractive solution to obtain solvent and mixed oil of Perillae herba, recovering solvent, introducing into solvent tank, collecting mixed oil of Perillae herba, and further processing to obtain Perilla oil.
Further, the lixiviant in the step (2) is soybean oil.
Further, in the step (2), the leaching agent is petroleum ether: ethanol: soybean oil according to a weight ratio of 1: 1-3: 9, and mixing.
Further, the extraction temperature in the step (2) is 55-60 ℃, the extraction pressure is 0.9-1.1MPa, and the extraction time is 5-8 h.
Further, the extraction step in the step (2) is as follows: maintaining for 1-3min when the pressure of the extraction kettle is increased to 0.9-1.1MPa, and then releasing the pressure to normal pressure; then continuously increasing the pressure to 0.9-1.1MPa, and extracting for 5-8 h.
Further, the water content of the perilla leaves in the step (1) is 7-9%.
Furthermore, the crushing in the step (1) is carried out at a low temperature of-50 to-90 ℃, and the particle size after crushing is 30-50 meshes.
Further, the crushing in the step (1) is that the temperature is reduced to-50 to-90 ℃, the temperature is uniformly raised to the room temperature at the speed of 2 ℃/min, and then the low-temperature crushing is carried out at the temperature of-50 to-90 ℃, and the particle size after the crushing is 30 to 50 meshes.
Further, the further processing in step (3) comprises adding 0.1-0.2% ODO to the oil to obtain perilla oil
The invention has the beneficial effects that:
1. the invention discloses an extraction process of perilla herb oil, which is optimized through a crushing process and an extraction process, can reduce the loss of essential oil to the maximum extent, and is simple in extraction process, the finally prepared perilla herb oil is a mixture of perilla herb essential oil (perilla herb extract) and soybean oil, is yellow oily matter, and the extraction rate of the perilla herb essential oil is 4.5-5.8%.
2. The perilla leaf crushing process adopts low-temperature crushing, the crushing temperature is-50 to-90 ℃, and the loss of essential oil can be reduced to the maximum extent; on the other hand, the temperature can be reduced to-50 to-90 ℃, because the water content of the purple perilla is 7-9 percent and the water content in the purple perilla tissue is more than that of the surface, the water in the purple perilla tissue is frozen at low temperature to form a large amount of ice grains, so that cells are expanded to damage cell walls; slowly heating to room temperature, wherein the surface temperature of the perilla is higher than that of the interior of the tissue, and pressure difference is formed in the process of melting ice crystals to further cause cell wall damage; and then the mixture is crushed to 30-50 meshes at low temperature, so that the loss of essential oil can be reduced, the wall breaking effect can be achieved, and the subsequent extraction is convenient.
3. When subcritical butane is adopted for extracting the perilla, and soybean oil is not added, the final extract is viscous grease, an extracting agent is added during extraction, wherein the extracting agent contains the soybean oil, on one hand, part of grease components in the perilla can be blended into the soybean oil, so that the extraction rate of fat-soluble components in essential oil is increased, and in the subsequent separation process, the perilla essential oil is dispersed in the soybean oil, and the final product is fluid grease, so that the subsequent treatment is convenient; further, petroleum ether: ethanol: soybean oil according to a weight ratio of 1: 1-3: 9, because the main component in the perilla essential oil of this application is alkene and aldehyde (ketone) alcohol, wherein alkene polarity is bigger, and aldehyde (ketone) alcohol polarity is bigger, and pure solvent extraction all can lead to the loss volume of essential oil bigger, this application adopts petroleum ether: ethanol: the soybean oil mixed solvent can greatly improve the extraction rate of polar components and non-polar components in the extraction process.
4. The extraction kettle is maintained for 1-3min when the pressure of the extraction kettle is increased to 0.9-1.1MPa in the extraction process, then the pressure is released to normal pressure, and in the pressure increasing and pressure releasing process, a solvent can be immersed in perilla tissues to be expanded and dissolved out, so that the tissues are damaged, and the mass transfer dissolution of subsequent essential oil components is improved.
5. In order to improve the stability of the final product, ODO (caprylic capric glyceride) with the mass fraction of 0.1-0.2% is added into the mixed oil of the soybean oil and the perilla extract, so that the product can be prevented from layering and has better stability.
Detailed Description
The invention is further described with reference to specific examples.
Example 1
A perilla herb oil extraction process comprises the following steps:
(1) pulverizing folium Perillae at-50 deg.C to obtain powder with particle size of 30 mesh, wherein the water content of folium Perillae is 7%;
(2) putting perilla powder into an extraction kettle, adding 2 times of soybean oil as an extractant by weight, soaking for 30min, starting a vacuum pump, injecting a solvent butane in a solvent tank into the extraction kettle through the pressure difference between the extraction kettle and the solvent tank when the pressure in the extraction kettle reaches-0.1 MPa, extracting for 8h under the conditions that the extraction temperature is 55 ℃ and the extraction pressure is 0.9MPa, and then feeding an extract into a separation tank;
(3) desolventizing the extractive solution in a separating tank at 55 deg.C and-0.1 MPa for 5min, separating butane, returning to the solvent tank, and collecting mixed perilla oil (mixture of perilla essential oil and soybean oil) from outlet valve of the separating tank.
In the extraction process of the step (2), the ratio of perilla powder to butane liquid is 1 Kg: 5L.
The extraction rate of perilla essential oil was (perilla oil-soybean oil)/perilla leaf 100%, and the extraction rate in this example was 4.5%.
Example 2
A perilla herb oil extraction process comprises the following steps:
(1) pulverizing folium Perillae at-70 deg.C to obtain powder with particle size of 40 mesh, wherein the water content of folium Perillae is 9%;
(2) putting perilla powder into an extraction kettle, adding 3 times of soybean oil as an extractant by weight, soaking for 30min, starting a vacuum pump, injecting a solvent butane in a solvent tank into the extraction kettle through the pressure difference between the extraction kettle and the solvent tank when the pressure in the extraction kettle reaches-0.1 MPa, extracting for 7h under the conditions that the extraction temperature is 60 ℃ and the extraction pressure is 1.0MPa, and then feeding an extract into a separation tank;
(3) desolventizing the extractive solution in a separating tank at 55 deg.C and-0.1 MPa for 5min, separating butane, returning to the solvent tank, and collecting mixed perilla oil (mixture of perilla essential oil and soybean oil) from outlet valve of the separating tank.
In the extraction process of the step (2), the ratio of perilla powder to butane liquid is 1 Kg: 5L.
The extraction rate of perilla essential oil in this example was 4.7%.
Example 3
A perilla herb oil extraction process comprises the following steps:
(1) pulverizing folium Perillae at-90 deg.C to obtain powder with particle size of 50 mesh, wherein the water content of folium Perillae is 8%;
(2) putting the perilla powder into an extraction kettle, and adding 3 times of an extracting agent by weight, wherein the extracting agent is petroleum ether: ethanol: soybean oil according to a weight ratio of 1: 1: 9, soaking for 30min, starting a vacuum pump, injecting a solvent butane in a solvent tank into an extraction kettle through the pressure difference between the extraction kettle and the solvent tank when the pressure in the extraction kettle reaches-0.1 MPa, extracting for 5h under the conditions that the extraction temperature is 65 ℃ and the extraction pressure is 1.1MPa, and then feeding an extract into a separation tank;
(3) desolventizing the extractive solution in a separating tank at 55 deg.C and-0.1 MPa for 5min, separating butane, returning to the solvent tank, and collecting mixed perilla oil (mixture of perilla essential oil and soybean oil) from outlet valve of the separating tank.
In the extraction process of the step (2), the ratio of perilla powder to butane liquid is 1 Kg: 5L.
The extraction rate of perilla essential oil in this example was 5.3%.
Example 4
A perilla herb oil extraction process comprises the following steps:
(1) cooling to-60 deg.C before pulverizing folium Perillae, uniformly heating to room temperature at 2 deg.C/min, and pulverizing at-60 deg.C to obtain powder with particle size of 40 mesh, wherein the water content of folium Perillae is 8%;
(2) putting the perilla powder into an extraction kettle, and adding an extracting agent with the weight 4 times that of the perilla powder, wherein the extracting agent is petroleum ether: ethanol: soybean oil according to a weight ratio of 1: 2: 9, soaking for 30min, maintaining for 3min when the pressure of the extraction kettle is increased to 1.0MPa, then relieving the pressure to normal pressure, performing subcritical butane extraction for 7h at the temperature of 60 ℃ and the extraction pressure of 1.0MPa, and feeding the extract into a separation tank;
(3) desolventizing and separating the extractive solution in a separating tank at 55 deg.C and-0.1 MPa for 5min, separating butane, returning to the solvent tank, and collecting mixed perilla oil from outlet valve of the separating tank;
(4) distilling under reduced pressure to separate ethanol and petroleum ether, and adding 0.1% ODO to obtain Perilla oil.
In the extraction process of the step (2), the ratio of perilla powder to butane liquid is 1 Kg: 5L.
The extraction rate of perilla essential oil in this example was 5.8%.
Example 5
A perilla herb oil extraction process comprises the following steps:
(1) cooling to-70 deg.C before pulverizing folium Perillae, uniformly heating to room temperature at 2 deg.C/min, and pulverizing at-70 deg.C to obtain folium Perillae powder with particle size of 50 mesh and water content of folium Perillae of 9%;
(2) putting the perilla powder into an extraction kettle, and adding 5 times of an extracting agent by weight, wherein the extracting agent is petroleum ether: ethanol: soybean oil according to a weight ratio of 1: 3: 9, soaking for 30min, maintaining for 3min when the pressure of the extraction kettle is increased to 1.1MPa, then relieving the pressure to normal pressure, performing subcritical butane extraction for 7h at the temperature of 65 ℃ and the extraction pressure of 1.1MPa, and feeding the extract into a separation tank;
(3) desolventizing and separating the extractive solution in a separating tank at 55 deg.C and-0.1 MPa for 5min, separating butane, returning to the solvent tank, and collecting mixed perilla oil from outlet valve of the separating tank;
(4) distilling under reduced pressure to separate ethanol and petroleum ether, and adding 0.1% ODO to obtain Perilla oil.
In the extraction process of the step (2), the ratio of perilla powder to butane liquid is 1 Kg: 5L.
The extraction rate of perilla essential oil in this example was 5.7%.
Example 6
A perilla herb oil extraction process comprises the following steps:
(1) cooling to-90 deg.C before pulverizing folium Perillae, uniformly heating to room temperature at 2 deg.C/min, and pulverizing at-90 deg.C to obtain powder with particle size of 40 mesh, wherein the water content of folium Perillae is 9%;
(2) putting the perilla powder into an extraction kettle, and adding 5 times of an extracting agent by weight, wherein the extracting agent is petroleum ether: ethanol: soybean oil according to a weight ratio of 1: 1: 9, soaking for 30min, maintaining for 3min when the pressure of the extraction kettle is increased to 1.0MPa, then relieving the pressure to normal pressure, performing subcritical butane extraction for 6h at the temperature of 60 ℃ and the extraction pressure of 1.0MPa, and feeding the extract into a separation tank;
(3) desolventizing and separating the extractive solution in a separating tank at 55 deg.C and-0.1 MPa for 5min, separating butane, returning to the solvent tank, and collecting mixed perilla oil from outlet valve of the separating tank;
(4) distilling under reduced pressure to separate ethanol and petroleum ether, and adding 0.2% ODO to obtain Perilla oil.
In the extraction process of the step (2), the ratio of perilla powder to butane liquid is 1 Kg: 5L.
The extraction rate of perilla essential oil in this example was 5.6%.
Finally, the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting, and other modifications or equivalent substitutions made by the technical solutions of the present invention by those of ordinary skill in the art should be covered within the scope of the claims of the present invention as long as they do not depart from the spirit and scope of the technical solutions of the present invention.
Claims (4)
1. A process for extracting perilla herb oil is characterized by comprising the following steps: the method comprises the following steps:
(1) pulverizing folium Perillae to obtain Perillae herba powder;
(2) putting the perilla powder into an extraction kettle, adding 2-5 times of an extracting agent by weight, and extracting by using subcritical butane to obtain an extract liquid;
(3) desolventizing and separating the extractive solution in a separating tank at 55 deg.C and-0.1 MPa for 5min, separating butane, returning to the solvent tank, collecting mixed oil of Perillae herba from outlet valve of the separating tank, distilling under reduced pressure to separate ethanol and petroleum ether, and further processing to obtain Perilla oil;
in the step (2), the leaching agent is petroleum ether: ethanol: soybean oil according to a weight ratio of 1: 1-3: 9 mixing the components; the further treatment in the step (3) comprises adding 0.1-0.2% of caprylic/capric glyceride into the oil to obtain perilla oil;
the extraction temperature in the step (2) is 55-60 ℃, the extraction pressure is 0.9-1.1MPa, and the extraction time is 5-8 h;
the crushing in the step (1) is carried out at a low temperature of-50 to-90 ℃, and the particle size after crushing is 30 to 50 meshes.
2. The extraction process of perilla oil as claimed in claim 1, wherein the extraction process comprises the following steps: the extraction step in the step (2) is as follows: maintaining for 1-3min when the pressure of the extraction kettle is increased to 0.9-1.1MPa, and then releasing the pressure to normal pressure; then continuously increasing the pressure to 0.9-1.1MPa, and extracting for 5-8 h.
3. The extraction process of perilla oil as claimed in claim 1, wherein the extraction process comprises the following steps: the water content of the perilla leaves in the step (1) is 7-9%.
4. The extraction process of perilla oil as claimed in claim 1, wherein the extraction process comprises the following steps: the crushing in the step (1) is that the temperature is firstly reduced to minus 50 to minus 90 ℃, the temperature is uniformly raised to the room temperature at the speed of 2 ℃/min, and then the low-temperature crushing is carried out at the temperature of minus 50 to minus 90 ℃, and the particle size after the crushing is 30 to 50 meshes.
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| CN111187671A (en) * | 2019-09-29 | 2020-05-22 | 郝兴群 | Extraction method of perilla leaf essential oil containing perilla flavone |
| CN114907910A (en) * | 2022-06-22 | 2022-08-16 | 中林油科技有限公司 | Extraction process for idesia polycarpa oil |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101905091A (en) * | 2010-07-12 | 2010-12-08 | 新疆大学 | Equipment and method for extracting biologically active ingredients from subcritical fluid |
| CN105505583A (en) * | 2015-11-24 | 2016-04-20 | 郑州雪麦龙食品香料有限公司 | A method of extracting bay leaf oil from bay leaves with subcritical n-butane fluid |
| CN106135466A (en) * | 2016-06-29 | 2016-11-23 | 贵州省油菜研究所 | A kind of perilla oil high efficiency extraction technique |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2017057178A (en) * | 2015-09-18 | 2017-03-23 | イビデン株式会社 | Extract of perilla frutescens var. crispa f. viridis. and production methods thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101905091A (en) * | 2010-07-12 | 2010-12-08 | 新疆大学 | Equipment and method for extracting biologically active ingredients from subcritical fluid |
| CN105505583A (en) * | 2015-11-24 | 2016-04-20 | 郑州雪麦龙食品香料有限公司 | A method of extracting bay leaf oil from bay leaves with subcritical n-butane fluid |
| CN106135466A (en) * | 2016-06-29 | 2016-11-23 | 贵州省油菜研究所 | A kind of perilla oil high efficiency extraction technique |
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