Supercritical extraction process of perilla seed oil

Abstract

The invention is suitable for the technical field of perilla seed oil extraction, and provides a perilla seed oil supercritical extraction process, which comprises the following steps: step (1), drying perilla seeds, weighing the perilla seeds, crushing, and grinding into powder; (2) dissolving the purple perilla seed powder with a proper amount of absolute ethyl alcohol, performing ultrasonic oscillation, filtering and separating to obtain filtrate A; (3) adding the filter paper in the step (2) into a Soxhlet extractor, and performing reflux extraction by taking absolute ethyl alcohol and petroleum ether as solvents to obtain an extracting solution A; (4) heating and concentrating the extracting solution A, and removing redundant petroleum ether to obtain an extracting solution B; and step (5), mixing the filtrate A and the extracting solution B, adding the mixture into an extraction kettle, setting the flow rate of CO2 to be 20L / h and the extraction time to be 2-3h, and extracting the purple perilla seed oil. According to the method, the oil yield of the perilla seed oil is remarkably improved, the oil yield is obviously improved by optimizing the technological process and parameters, and the method has wide application prospects.

Description

Technical Field

[0001] The invention relates to the technical field of perilla seed oil extraction, in particular to a supercritical extraction process of perilla seed oil. Background Art

[0002] Perilla frutescens (L.) Britt., also known as guiren, white perilla, red perilla, etc., is an annual herbaceous plant of the Lamiaceae family. Perilla has strong adaptability and is not strict on soil. It has good drainage and grows well on sandy loam, loam, clay loam, in front of and behind houses, by ditches, and on fertile soil.

[0003] Perilla seed oil is a vegetable oil extracted from the seeds of Perilla frutescens, which is rich in nutrients and health functions. It has a long history of use in traditional Chinese medicine and is increasingly used in food, cosmetics and health products. Perilla seed oil is rich in linolenic acid (ω-3 fatty acid) and some natural ingredients that are beneficial to the skin.

[0004] Perilla extraction refers to the process of extracting active ingredients from the leaves, seeds or other parts of the perilla plant, which often include essential oils, perilla seed oil and other nutrients. Common methods of perilla extraction include cold pressing (pressing), solvent extraction, steam distillation and supercritical CO2 extraction. Among them, supercritical CO2 extraction has been widely used in the extraction of perilla seed oil due to its advantages of high efficiency, environmental protection and large-scale production. This method uses supercritical CO2 as an extractant, and by adjusting the pressure and temperature, CO2 reaches a supercritical state, thereby effectively extracting the active ingredients in perilla seed oil. Compared with other extraction methods, supercritical CO2 extraction has higher extraction efficiency and better product quality, while avoiding the use of organic solvents and reducing environmental pollution.

[0005] However, the oil yield of the existing supercritical CO2 extraction method still has a lot of room for improvement. In this regard, the present application proposes a supercritical extraction process for perilla seed oil. Summary of the invention

[0006] The invention aims to provide a supercritical extraction process for perilla seed oil, so as to solve the problem that the oil yield of the supercritical CO2 extraction method in the prior art still has a large room for improvement.

[0007] To achieve the above object, the present invention provides the following technical solution: a supercritical extraction process of perilla seed oil, comprising the following steps:

[0008] Step (1), drying the perilla seeds, weighing the perilla seeds, crushing them, and grinding them into powder;

[0009] Step (2), dissolving the perilla seed powder with an appropriate amount of anhydrous ethanol, ultrasonically vibrating, filtering, and separating to obtain a filtrate A;

[0010] Step (3), adding the filter paper in step (2) into a Soxhlet extractor, using anhydrous ethanol and petroleum ether as solvents, and reflux extraction to obtain an extract A;

[0011] Step (4), heating and concentrating the extract A, removing excess petroleum ether, and obtaining an extract B;

[0012] Step (5), mixing the filtrate A and the extract B, adding them into an extraction kettle, setting the CO2 flow rate to 20 L / h, the extraction time to 2-3 h, and extracting perilla seed oil;

[0013] Step (6), transferring the CO2 dissolved with perilla seed oil into separation kettle I, reducing the pressure, precipitating the solute, and depositing it at the bottom of separation kettle I, then transferring the CO2 into separation kettle II, reducing the pressure, continuing to precipitate the solute, and depositing it at the bottom of separation kettle II, and collecting the perilla seed oil.

[0014] Preferably, the temperature of ultrasonic oscillation in step (2) is 30-40° C., and the ultrasonic oscillation time is 25-45 min.

[0015] Preferably, the volume ratio of anhydrous ethanol to petroleum ether in step (3) is (5-10):1.

[0016] Preferably, the reflux extraction time in step (3) is 8-15h.

[0017] Preferably, the temperature is raised to 70° C. in step (4).

[0018] Preferably, the extraction pressure in step (5) is 35-40 MPa.

[0019] Preferably, in step (6), the pressure of the separation kettle I is reduced to 8 MPa and the temperature is 36°C.

[0020] Preferably, in step (6), the pressure of separation kettle II is reduced to 5 MPa and the temperature is 32°C.

[0021] The present invention has at least the following beneficial effects:

[0022] The invention provides a supercritical extraction process for perilla seed oil. Before supercritical CO2 extraction, ultrasonic oscillation and Soxhlet extraction are first performed, which significantly improves the oil yield of perilla seed oil. The oil yield is significantly improved by optimizing the process flow and parameters, and the invention has broad application prospects. DETAILED DESCRIPTION

[0023] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0024] Example 1

[0025] This embodiment provides a supercritical extraction process for perilla seed oil, comprising the following steps:

[0026] Step (1), drying the perilla seeds, weighing the perilla seeds, crushing them, and grinding them into powder;

[0027] Step (2), dissolving the perilla seed powder with an appropriate amount of anhydrous ethanol, ultrasonically oscillating for 25 minutes at a temperature of 30° C., filtering, and separating to obtain filtrate A;

[0028] Step (3), adding the filter paper in step (2) into a Soxhlet extractor, using anhydrous ethanol and petroleum ether as solvents, with the volume ratio of anhydrous ethanol to petroleum ether being 5:1, and reflux extraction for 8 hours to obtain an extract A;

[0029] Step (4), heating the extract A to 70° C., concentrating, and removing excess petroleum ether to obtain an extract B;

[0030] Step (5), mixing the filtrate A and the extract B, adding them into an extraction kettle, setting the CO2 flow rate to 20 L / h, the extraction time to 2 h, the extraction pressure to 35 MPa, and extracting perilla seed oil;

[0031] Step (6), transferring the CO2 dissolved with perilla seed oil into separation kettle I, reducing the pressure to 8 MPa, the temperature to 36°C, precipitating the solute, and depositing it at the bottom of separation kettle I, then transferring the CO2 into separation kettle II, reducing the pressure to 5 MPa, the temperature to 32°C, continuing to precipitate the solute, and depositing it at the bottom of separation kettle II, and collecting the perilla seed oil.

[0032] Example 2

[0033] This embodiment provides a supercritical extraction process for perilla seed oil, comprising the following steps:

[0034] Step (1), drying the perilla seeds, weighing the perilla seeds, crushing them, and grinding them into powder;

[0035] Step (2), dissolving the perilla seed powder with an appropriate amount of anhydrous ethanol, ultrasonically oscillating for 35 minutes at a temperature of 35° C., filtering, and separating to obtain filtrate A;

[0036] Step (3), adding the filter paper in step (2) into a Soxhlet extractor, using anhydrous ethanol and petroleum ether as solvents, with the volume ratio of anhydrous ethanol to petroleum ether being 8:1, and reflux extraction for 12 hours to obtain an extract A;

[0037] Step (4), heating the extract A to 70° C., concentrating, and removing excess petroleum ether to obtain an extract B;

[0038] Step (5), mixing the filtrate A and the extract B, adding them into an extraction kettle, setting the CO2 flow rate to 20 L / h, the extraction time to 2.5 h, the extraction pressure to 37 MPa, and extracting perilla seed oil;

[0039] Step (6), transferring the CO2 dissolved with perilla seed oil into separation kettle I, reducing the pressure to 8 MPa, the temperature to 36°C, precipitating the solute, and depositing it at the bottom of separation kettle I, then transferring the CO2 into separation kettle II, reducing the pressure to 5 MPa, the temperature to 32°C, continuing to precipitate the solute, and depositing it at the bottom of separation kettle II, and collecting the perilla seed oil.

[0040] Example 3

[0041] This embodiment provides a supercritical extraction process for perilla seed oil, comprising the following steps:

[0042] Step (1), drying the perilla seeds, weighing the perilla seeds, crushing them, and grinding them into powder;

[0043] Step (2), dissolving the perilla seed powder with an appropriate amount of anhydrous ethanol, ultrasonically oscillating for 45 minutes at a temperature of 40° C., filtering, and separating to obtain filtrate A;

[0044] Step (3), adding the filter paper in step (2) into a Soxhlet extractor, using anhydrous ethanol and petroleum ether as solvents, with the volume ratio of anhydrous ethanol to petroleum ether being 10:1, and reflux extraction for 15 hours to obtain an extract A;

[0045] Step (4), heating the extract A to 70° C., concentrating, and removing excess petroleum ether to obtain an extract B;

[0046] Step (5), mixing the filtrate A and the extract B, adding them into an extraction kettle, setting the CO2 flow rate to 20 L / h, the extraction time to 3 h, the extraction pressure to 40 MPa, and extracting perilla seed oil;

[0047] Step (6), transferring the CO2 dissolved with perilla seed oil into separation kettle I, reducing the pressure to 8 MPa, the temperature to 36°C, precipitating the solute, and depositing it at the bottom of separation kettle I, then transferring the CO2 into separation kettle II, reducing the pressure to 5 MPa, the temperature to 32°C, continuing to precipitate the solute, and depositing it at the bottom of separation kettle II, and collecting the perilla seed oil.

[0048] The oil yield of the products obtained in the above examples 1-3 was tested, and the results are shown in the following table:

[0049] Example 1 Example 2 Example 3 Oil yield 43.9％ 44.7％ 45.4％

[0050] The invention performs ultrasonic oscillation and Soxhlet extraction before supercritical CO2 extraction, thereby significantly improving the oil yield of perilla seed oil, and by optimizing the process flow and parameters, compared with the traditional supercritical CO2 extraction method, the process of the invention has significantly improved the oil yield while ensuring product quality, which not only improves production efficiency but also reduces production costs, making large-scale production of perilla seed oil possible. The invention has broad application prospects in the production field of perilla seed oil.

[0051] The above shows and describes the basic principles, main features and advantages of the present invention. It is obvious to those skilled in the art that the present invention is not limited to the details of the above exemplary embodiments, and that the present invention can be implemented in other specific forms without departing from the spirit or basic features of the present invention. Therefore, no matter from which point of view, the embodiments should be regarded as exemplary and non-restrictive. The scope of the present invention is defined by the appended claims rather than the above description, and it is intended that all changes falling within the meaning and scope of the equivalent elements of the claims are included in the present invention.

[0052] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A supercritical extraction process for perilla seed oil, characterized in that: The following steps are involved: Step (1), drying the perilla seeds, weighing the perilla seeds, crushing them, and grinding them into powder; Step (2), dissolving the perilla seed powder with an appropriate amount of anhydrous ethanol, ultrasonically vibrating, filtering, and separating to obtain a filtrate A; Step (3), adding the filter paper in step (2) into a Soxhlet extractor, using anhydrous ethanol and petroleum ether as solvents, and reflux extraction to obtain an extract A; Step (4), heating and concentrating the extract A, removing excess petroleum ether, and obtaining an extract B; Step (5), mixing the filtrate A and the extract B, adding them into an extraction kettle, setting the CO2 flow rate to 20 L / h, the extraction time to 2-3 h, and extracting perilla seed oil; Step (6), transferring the CO2 dissolved with perilla seed oil into separation kettle I, reducing the pressure, precipitating the solute, and depositing it at the bottom of separation kettle I, then transferring the CO2 into separation kettle II, reducing the pressure, continuing to precipitate the solute, and depositing it at the bottom of separation kettle II, and collecting the perilla seed oil.

2. A supercritical extraction process for perilla seed oil according to claim 1, characterized in that: The temperature of the ultrasonic oscillation in the step (2) is 30-40° C., and the ultrasonic oscillation time is 25-45 min.

3. A supercritical extraction process for perilla seed oil according to claim 1, characterized in that: The volume ratio of anhydrous ethanol to petroleum ether in step (3) is (5-10):

1.

4. A supercritical extraction process for perilla seed oil according to claim 1, characterized in that: The reflux extraction time of step (3) is 8-15h.

5. The supercritical extraction process of perilla seed oil according to claim 1, characterized in that: In the step (4), the temperature is raised to 70°C.

6. The supercritical extraction process of perilla seed oil according to claim 1, characterized in that: The extraction pressure in step (5) is 35-40 MPa.

7. The supercritical extraction process of perilla seed oil according to claim 1, characterized in that: In step (6), the pressure in the separation kettle I is reduced to 8 MPa and the temperature is 36°C.

8. The supercritical extraction process of perilla seed oil according to claim 1, characterized in that: In step (6), the pressure in separation kettle II is reduced to 5 MPa and the temperature is 32°C.