CN108659957A - The method that jujube extracts essential oil - Google Patents

Abstract

The present invention provides a kind of methods that jujube extracts essential oil comprising step：(1) jujube is immersed in liquid nitrogen, it is cooling, obtain super cold jujube；(2) the super cold jujube is subjected to liquid nitrogen frozen pulverization process, obtains super cold jujube powder；(3) the super cold jujube powder is subjected to frozen dried, obtains super cold extra dry red wine date powder end；(4) by the super cold extra dry red wine date powder end, Soxhlet extraction is carried out, jujube essential oil solution is obtained；(5) the jujube essential oil solution is evaporated in vacuo, obtains jujube essential oil.The present invention has extraction of essential oil rate high, and the dense advantage of characteristic perfume can make full use of the jujube core, fructus corni and jujube meat of jujube, greatly improve the recovery rate of essential oil under the premise of not reducing jujube essential oil quality.

Description

Method for extracting essential oil from jujube

technical field

The invention relates to the field of plant essential oil extraction, more specifically, to a method for extracting essential oil from jujube.

Background technique

Jujube is rich in vitamins A, B, C and other essential vitamins and 18 kinds of amino acids and minerals, among which the content of vitamin C (ascorbic acid) is as high as 70 to 80 times that of grapes and apples. However, the storage capacity of red dates is less than about 20% of the total output, the cold storage capacity is about 7%, and the fresh fruit rot rate reaches 20% to 25%. The deep processing technology research of red dates has become an urgent problem to be solved in the industrialization of red dates. Extracting essential oil from jujube is a major development direction at present.

Jujube essential oil is a substance with a special smell and is volatile at room temperature. It is a precious liquid with high medicinal value and health care performance. It can increase the oxygen content in the blood and nourish the cells of the whole body. It is a mild tonic. Jujube essential oil has the functions of antitussive, wind-dispelling, preventing cardiovascular disease, improving immunity, and strengthening the stomach.

At present, jujube essential oil is mainly extracted by steam distillation, supercritical _CO2 extraction, microwave extraction and so on. The extraction rates of these methods are all low, and the extraction of jujube core and jujube skin, which are more beneficial components in red dates, is not sufficient enough. In addition, most of the existing methods require high-temperature treatment, which easily causes the loss of fragrance and flavor. At present, there is a need for a method that does not reduce the quality of the essential oil, and can fully extract the essential oil of the whole jujube and has a high extraction rate.

Contents of the invention

The purpose of the present invention is to provide a method for extracting essential oil from jujube, which can make full use of the core, skin and flesh of jujube without reducing the quality of essential oil of jujube, and greatly increase the extraction rate of essential oil.

In order to achieve the above object, the present invention provides a method for extracting essential oil from jujube, which comprises the steps of: (1) immersing jujube in liquid nitrogen and cooling to obtain ultra-cold jujube; (2) freezing the super-cold jujube in liquid nitrogen Pulverizing to obtain ultra-cold jujube powder; (3) freeze-drying the ultra-cold jujube powder to obtain ultra-cold-dried jujube powder; (4) performing Soxhlet extraction on the ultra-cold-dried jujube powder to obtain jujube essential oil solution; (5) vacuum distilling the jujube essential oil solution to obtain the jujube essential oil.

Optionally, the red dates are fresh red dates or naturally dried red dates.

Optionally, immerse the jujube in liquid nitrogen for 10 to 30 minutes for cooling

Optionally, the process of the liquid nitrogen freezing and crushing treatment is as follows: the ultra-cold jujube is put into the crushing chamber from the hopper of the liquid nitrogen freezing and crushing machine, the temperature of the crushing chamber is adjusted to -190 to -100°C, and the crushing time is 0.5 to 100°C. 2 hours, sieve and collect.

Optionally, the process of the freeze-drying treatment is: after cooling the freeze-drying box to -50～-20°C, putting the ultra-cold jujube powder into a glass dish and placing it in the freeze-drying box; The vacuum degree is 0.7-1MPa, and it is kept for 5-10 hours; it is heated to 40-50° C., and it is kept for 5-8 hours; it is returned to normal pressure, and taken out to obtain ultra-cooled dried jujube powder.

Optionally, the process of the Soxhlet extraction is as follows: the ultra-cold dried jujube powder is placed in a cylindrical filter paper tube, and put into the extraction tube of the Soxhlet extractor together; in the extraction bottle of the Soxhlet extractor Ethanol is put in, and the mass ratio of ethanol to the ultra-cold-dried jujube powder is 1:1-15; the Soxhlet extractor is opened, and the extraction time is 3-5 hours.

Optionally, the extraction tube of the Soxhlet extractor is subjected to one or a combination of microwave irradiation and ultrasonic waves.

Optionally, the process of vacuum distillation is as follows: placing the jujube essential oil solution in a beaker and placing it in the box of a vacuum drying oven; connecting the cylinder of inert gas to the inlet valve of the vacuum drying oven through a pipeline , open the valve of the gas cylinder, adjust the output valve of the decompression gauge, and keep the output pressure at 0.1-0.2MPa; open the vacuum pump, draw a vacuum, adjust the intake valve, and keep the vacuum degree at 0.4-0.75Mpa; set the vacuum The temperature of the drying box is 55-75°C, keep the jujube essential oil solution in a slightly boiling state; after the distillation, turn off the vacuum pump, and after the box body of the vacuum drying box is naturally cooled to room temperature, restore the pressure in the box to normal pressure and close Cylinder valve, take out the beaker, airtight preservation, obtain red date essential oil.

Optionally, the inert gas is one of argon and nitrogen.

The present invention preliminarily freezes jujube with liquid nitrogen, and then freezes and pulverizes jujube with liquid nitrogen to obtain superfine jujube powder with a small particle size. Wall, which is more conducive to the subsequent extraction process, essential oil substances diffuse into the solvent, greatly improving the extraction rate of essential oils. Heating and vacuum distillation of jujube essential oil solution can reduce the distillation temperature and reduce the contact between air and solution, and avoid the oxidative inactivation of active ingredients in jujube essential oil to a certain extent, thereby maintaining the medicinal value of jujube essential oil.

Other features and advantages of the present invention will be described in detail in the detailed description that follows.

Description of drawings

The above and other objects, features and advantages of the present invention will become more apparent by describing the exemplary embodiments of the present invention in more detail with reference to the accompanying drawings, wherein, in the exemplary embodiments of the present invention, the same reference numerals generally represent same parts.

Fig. 1 shows the flow chart of the method for extracting essential oil from jujube according to the present invention.

Figure 2 shows the equipment diagram for vacuum distillation.

Detailed ways

Preferred embodiments of the present invention will be described in more detail below with reference to the accompanying drawings. Although preferred embodiments of the invention are shown in the drawings, it should be understood that the invention may be embodied in various forms and should not be limited to the embodiments set forth herein.

With reference to Fig. 1, the method for extracting essential oil from jujube according to the present invention comprises steps: (1) immerse jujube in liquid nitrogen, cool, obtain ultra-cold jujube; (2) carry out liquid nitrogen freezing and pulverizing treatment to described super-cold jujube, obtain Ultra-cold jujube powder; (3) freeze-drying the super-cold jujube powder to obtain ultra-cold-dried jujube powder; (4) performing Soxhlet extraction on the ultra-cold jujube powder to obtain jujube essential oil solution; ( 5) Vacuum distilling the jujube essential oil solution to obtain the jujube essential oil.

In the method for extracting essential oil from red dates according to the present invention, the red dates are fresh red dates or naturally dried red dates.

In the method for extracting essential oil from jujube according to the present invention, the time for immersing jujube in liquid nitrogen to cool is 10-30min

In the method for extracting essential oil from jujube according to the present invention, the process of the liquid nitrogen freezing and crushing treatment is as follows: the ultra-cold jujube is put into the crushing chamber from the feed bin of the liquid nitrogen freezing crushing machine, and the temperature of the crushing chamber is adjusted to be -190 ~-100°C, pulverize for 0.5-2 hours, sieve and collect.

In the method for extracting essential oil from jujube according to the present invention, the freeze-drying process is as follows: after the freeze-drying box is cooled to -50--20°C, the ultra-cold jujube powder is put into a glass dish and placed in a In a freeze-drying box; evacuate to a vacuum degree of 0.7-1 MPa, and keep for 5-10 hours; heat to 40-50° C., and keep for 5-8 hours; return to normal pressure, and take out to obtain ultra-cold-dried jujube powder.

In the method for extracting essential oil from jujube according to the present invention, the process of the Soxhlet extraction is: the ultra-cold dried jujube powder is placed in a cylindrical filter paper tube, and put into the extraction tube of the Soxhlet extractor together; Ethanol is put into the extraction bottle of the Soxhlet extractor, and the mass ratio of ethanol to the ultra-cold dried jujube powder is 1:1-15; the Soxhlet extractor is opened, and the extraction time is 3-5 hours.

In the method for extracting essential oil from jujube according to the present invention, the extraction tube of the Soxhlet extractor accepts one or a combination of microwave irradiation and ultrasonic waves.

In the method for extracting essential oil from jujube according to the present invention, with reference to Fig. 2, the process of the vacuum distillation is as follows: placing the jujube essential oil solution in a beaker and placing it in the box of a vacuum drying oven; Connect the intake valve of the vacuum drying box through a pipeline, open the valve of the gas cylinder, adjust the output valve of the decompression gauge, and keep the output pressure at 0.1 to 0.2 MPa; open the vacuum pump, draw vacuum, adjust the intake valve, and keep Vacuum degree 0.4～0.75Mpa; The temperature of setting described vacuum drying box is 55～75 ℃, keeps described red jujube essential oil solution to be in slight boiling state; After distillation finishes, close vacuum pump, wait for the box body of vacuum drying box to cool naturally to After room temperature, restore the pressure in the box to normal pressure, close the valve of the gas cylinder, take out the beaker, and keep it airtight to obtain the jujube essential oil.

In the method for extracting essential oil from jujube according to the present invention, the inert gas is one of argon and nitrogen.

Below, the method for extracting essential oil from jujube of the present invention is described in detail in conjunction with specific examples.

Example 1

(1) Liquid nitrogen cooling: immerse fresh jujubes in liquid nitrogen for 10 minutes to obtain ultra-cold jujubes.

(2) Liquid nitrogen freezing and crushing: Put the ultra-cold jujube into the crushing chamber from the hopper of the liquid nitrogen freezing and crushing machine, adjust the temperature of the crushing chamber to be -100°C, crush for 0.5 hours, sieve, collect, and obtain ultra-cold jujube powder .

(3) Freeze-drying: After cooling the freeze-drying box to -50°C, put the ultra-cold jujube powder into a glass dish and place it in the freeze-drying box; vacuumize to a vacuum degree of 0.7 MPa and keep for 5 hours; heat to 40 ℃, and keep it for 5 hours; return to normal pressure, take out to obtain ultra-cold dried jujube powder.

(4) Soxhlet extraction: put the ultra-cold dried jujube powder in a cylindrical filter paper tube, and put them together in the extraction tube of the Soxhlet extractor, wherein the extraction tube accepts microwave irradiation; put it in the extraction bottle of the Soxhlet extractor Ethanol, the mass ratio of ethanol to ultra-cold-dried jujube powder is 1:1; the Soxhlet extractor is opened, and the extraction time is 3 hours to obtain the jujube essential oil solution.

(5) Vacuum distillation: red date essential oil solution is placed in the beaker, is placed in the casing of vacuum oven; The cylinder of argon is communicated with the intake valve of described vacuum oven by pipeline, opens the valve of cylinder, regulates The output valve of the decompression meter, keep the output pressure at 0.1MPa; turn on the vacuum pump, draw the vacuum, adjust the intake valve, and keep the vacuum degree at 0.4Mpa; set the temperature of the vacuum drying oven at 55°C, and keep the jujube essential oil solution in a slightly boiling state After the distillation finishes, close the vacuum pump, after the casing of the vacuum drying box is naturally cooled to room temperature, restore the pressure in the casing to normal pressure, close the gas cylinder valve, take out the beaker, and keep it in a sealed state to obtain the jujube essential oil.

Example 2

(1) Liquid nitrogen cooling: immerse the naturally dried red dates in liquid nitrogen for 30 minutes to obtain super-cooled red dates.

(2) Liquid nitrogen freezing and crushing: Put the ultra-cold red dates into the crushing chamber from the hopper of the liquid nitrogen freezing crushing machine, adjust the temperature of the crushing chamber to be -190°C, crush for 2 hours, sieve, collect, and obtain super-cold red dates powder .

(3) Freeze-drying: After cooling the freeze-drying box to -20°C, put the ultra-cold jujube powder into a glass dish and place it in the freeze-drying box; evacuate to a vacuum of 1MPa and keep for 10 hours; heat to 50°C , and kept for 8 hours; returned to normal pressure, taken out to obtain ultra-cold dried jujube powder.

(4) Soxhlet extraction: put the ultra-cold dried jujube powder in a cylindrical filter paper tube, and put them together in the extraction tube of the Soxhlet extractor, wherein the extraction tube accepts microwave irradiation; put it in the extraction bottle of the Soxhlet extractor Ethanol, the mass ratio of ethanol to ultra-cold-dried jujube powder is 1:15; the Soxhlet extractor is opened, and the extraction time is 5 hours to obtain the jujube essential oil solution.

(5) Vacuum distillation: red jujube essential oil solution is placed in the beaker, is placed in the casing of vacuum oven; The cylinder of nitrogen is communicated with the inlet valve of described vacuum oven by pipeline, opens the valve of cylinder, adjusts the degassing With the output valve of the pressure gauge, keep the output pressure at 0.2MPa; turn on the vacuum pump, extract the vacuum, adjust the intake valve, and keep the vacuum degree at 0.75Mpa; set the temperature of the vacuum drying oven to 75°C, and keep the jujube essential oil solution in a slightly boiling state; After the distillation, turn off the vacuum pump, and after the box body of the vacuum drying box is naturally cooled to room temperature, restore the pressure in the box to normal pressure, close the valve of the gas cylinder, take out the beaker, and store it in an airtight manner to obtain the jujube essential oil.

Example 3

(1) Liquid nitrogen cooling: immerse fresh jujubes in liquid nitrogen for 20 minutes to obtain ultra-cold jujubes.

(2) Liquid nitrogen freezing and crushing: Put the ultra-cold red dates into the crushing chamber from the hopper of the liquid nitrogen freezing crushing machine, adjust the temperature of the crushing chamber to be -150°C, crush for 1 hour, sieve, collect, and obtain super-cold red dates powder .

(3) Freeze-drying: After cooling the freeze-drying box to -30°C, put the ultra-cold jujube powder into a glass dish and place it in the freeze-drying box; vacuumize to a vacuum degree of 0.8 MPa and keep for 8 hours; heat to 45 ℃, and keep it for 6.5 hours; return to normal pressure, take out to obtain ultra-cold dried jujube powder.

(4) Soxhlet extraction: put the ultra-cold dried jujube powder in a cylindrical filter paper tube, and put them together in the extraction tube of the Soxhlet extractor, wherein the extraction tube accepts ultrasonic waves; put ethanol in the extraction bottle of the Soxhlet extractor , the mass ratio of ethanol to ultra-cold-dried jujube powder is 1:8; the Soxhlet extractor is opened, and the extraction time is 4 hours to obtain the jujube essential oil solution.

(5) Vacuum distillation: red date essential oil solution is placed in the beaker, is placed in the casing of vacuum oven; The cylinder of argon is communicated with the intake valve of described vacuum oven by pipeline, opens the valve of cylinder, regulates The output valve of the decompression meter, keep the output pressure at 0.15MPa; turn on the vacuum pump, draw the vacuum, adjust the intake valve, and keep the vacuum degree at 0.6Mpa; set the temperature of the vacuum drying oven at 65°C, and keep the jujube essential oil solution in a slightly boiling state After the distillation finishes, close the vacuum pump, after the casing of the vacuum drying box is naturally cooled to room temperature, restore the pressure in the casing to normal pressure, close the gas cylinder valve, take out the beaker, and keep it in a sealed state to obtain the jujube essential oil.

Comparative example 1

Jujube does not go through the steps of liquid nitrogen cooling, liquid nitrogen freezing, crushing and freeze-drying, and the others are the same as in Example 3.

Comparative example 2

Except that jujube essential oil is distilled in natural environment, and vacuum distillation is not carried out, other is identical with embodiment 3.

Performance Testing

1. Weigh the quality of jujube essential oil and the quality of jujube, and calculate the extraction rate of essential oil

Essential oil extraction rate=(quality of jujube essential oil/quality of jujube)×100%

2. Sensory evaluation of the aroma of the essential oil and whether the aroma is strong.

Performance comparison table

Example Essential oil extraction rate/% characteristic aroma Example 1 18 Yes, strong Example 2 19 Yes, strong Example 3 20 Yes, strong Comparative example 1 4 Yes, light Comparative example 2 7 none

It can be seen from the above examples that the jujube essential oil prepared by the present invention has the advantages of high extraction rate of essential oil and strong characteristic aroma relative to the comparative examples, and can make full use of the jujube pit and jujube without reducing the quality of the jujube essential oil. The skin and jujube meat can greatly increase the extraction rate of essential oils.

Having described various embodiments of the present invention, the foregoing description is exemplary, not exhaustive, and is not limited to the disclosed embodiments. Many modifications and alterations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments.

Claims (9)

1. a kind of method of jujube extraction essential oil, which is characterized in that including step：

(1) jujube is immersed in liquid nitrogen, it is cooling, obtain super cold jujube；

(2) the super cold jujube is subjected to liquid nitrogen frozen pulverization process, obtains super cold jujube powder；

(3) the super cold jujube powder is subjected to frozen dried, obtains super cold extra dry red wine date powder end；

(4) by the super cold extra dry red wine date powder end, Soxhlet extraction is carried out, jujube essential oil solution is obtained；

(5) the jujube essential oil solution is evaporated in vacuo, obtains jujube essential oil.

2. the method for jujube extraction essential oil as described in claim 1, which is characterized in that the jujube is for fresh jujube or certainly The jujube so dried.

3. the method for jujube as described in claim 1 extraction essential oil, which is characterized in that when jujube is immersed cooling in liquid nitrogen Between be 10~30min.

4. the method for jujube extraction essential oil as described in claim 1, which is characterized in that the mistake of the liquid nitrogen frozen pulverization process Cheng Wei：The super cold jujube puts into pulverizing chamber by the feed bin of liquid nitrogen frozen pulverizer, adjust pulverizing chamber temperature be -190~- It 100 DEG C, crushes 0.5~2 hour, is sieved, collect.

5. the method for jujube as described in claim 1 extraction essential oil, which is characterized in that the process of the frozen dried is：It will After freeze drying box is cooled to -50~-20 DEG C, the super cold jujube powder is fitted into glass dish, is positioned in freeze drying box；It vacuumizes To 0.7~1MPa of vacuum degree, kept for 5~10 hours；40~50 DEG C are heated to, and is kept for 5~8 hours；Restore to normal pressure, takes out Obtain super cold extra dry red wine date powder end.

6. the method for jujube as described in claim 1 extraction essential oil, which is characterized in that the process of the Soxhlet extraction is：It will The super cold extra dry red wine date powder end is placed in cylindrical filtration paper cylinder, is put into the extraction tube of Soxhlet extractor jointly；In the Soxhlet Ethyl alcohol is put into the extraction flask of extractor, ethyl alcohol is 1 with the super cold extra dry red wine date powder end mass ratio:1~15；Open the Soxhlet Extractor, extraction time are 3~5 hours.

7. the method for jujube extraction essential oil as claimed in claim 6, which is characterized in that the extraction tube of the Soxhlet extractor, Receive one kind in microwave irradiation and ul-trasonic irradiation or combination.

8. the method for jujube as described in claim 1 extraction essential oil, which is characterized in that the process of the vacuum distillation is：It will The jujube essential oil solution is placed in beaker, is positioned in the babinet of vacuum drying chamber；The gas cylinder of inert gas is passed through into pipeline It is connected to the air intake valve of the vacuum drying chamber, opens the valve of the gas cylinder, adjusts the output valve of decompression table, keeps output Pressure is 0.1~0.2MPa；Vacuum pump is opened, vacuum is extracted, adjusts air intake valve, keeps 0.4~0.75Mpa of vacuum degree；Setting The temperature of the vacuum drying chamber is 55~75 DEG C, and the jujube essential oil solution is kept to be in slight boiling condition；After distillation, close Vacuum pump is closed, after the babinet cooled to room temperature of vacuum drying chamber, restores pressure in babinet and closes bottle valve to normal pressure Door, takes out beaker, and closed preservation obtains jujube essential oil.

9. the method for jujube extraction essential oil as claimed in claim 8, which is characterized in that the inert gas is argon gas and nitrogen In one kind.