CN117942384B - Preparation method of ginger oil with high biological activity and supercritical carbon dioxide extraction - Google Patents

Abstract

The invention relates to a preparation method of high-bioactivity ginger oil and supercritical carbon dioxide extraction, wherein 6-gingerol in the ginger oil is more than 50%, 8-Jiang Fenxiao% and 10-Jiang Fenxiao% of the ginger oil. The preparation method of the ginger oil comprises the following steps: filling dried ginger powder into an extraction tank of a supercritical CO2 system, extracting with supercritical carbon dioxide, separating out the extracted ginger oil in a separation tank through graded decompression and graded cooling, adding purified water to wash the separation tank, combining the separated matter and the washing liquid into a separating funnel, standing, separating the liquid and discarding the water phase to obtain the ginger oil. The ginger oil with high biological activity obtained by the invention has unique chemical composition distribution, the whole method avoids using toxic organic solvents, and the preparation process is environment-friendly. The ginger oil disclosed by the invention has excellent biological performance of inhibiting inflammation, and can inhibit mice ear swelling induced by dimethylbenzene, inhibit mice egg white foot swelling and inhibit delayed hypersensitivity of mice caused by DNCB.

Description

Preparation method of high biological activity ginger oil and supercritical carbon dioxide extraction thereof

Technical Field

The present invention belongs to the field of biomedicine and relates to a ginger oil with significantly higher biological activity, such as ginger oil made from fresh ginger or dried ginger. The ginger oil with high biological activity has a unique chemical composition distribution and exhibits excellent biological effects. The present invention also relates to a preparation method of the ginger oil with high biological activity, which uses a supercritical carbon dioxide extraction process, does not use toxic or harmful organic solvents, and has a green and environmentally friendly preparation process.

Background technique

Ginger ( Zingiber officinale Roscoe), also known as ginger, is a perennial herbaceous plant of the genus Zingiber in the family Zingiberaceae. It has rhizomes with yellow-green flowers and a pungent aroma. The plant is 0.5-1 meter tall; the rhizomes are thick, branched, and aromatic and spicy. The leaves are lanceolate or linear-lanceolate, glabrous, and sessile; the ligule is membranous. The peduncle is up to 25 cm long; the spike inflorescence is cone-shaped; the bracts are ovate, light green or light yellow on the edges, with a small tip at the top. The calyx tube is about 1 cm long; the corolla is yellow-green, with lanceolate lobes; the central lobe of the lip is oblong-obovate. Ginger is widely cultivated in central, southeastern and southwestern China. The rhizomes are used for medicinal purposes, and the fresh or dried products can be used as cooking ingredients or made into pickles and sugar ginger. Aromatic oils can be extracted from the stems, leaves, and rhizomes, which are used in food, beverages, and cosmetic spices.

The aliases of ginger include ginger root, Bai Layun, hook-shaped finger, Yindixin, Yanliang boy, and fresh ginger. The rhizome (dried ginger), cork (ginger peel), and leaves (ginger leaves) of ginger can all be used as medicine. It has the effects of dispelling cold, warming the middle and stopping vomiting, warming the lungs and stopping coughs, and detoxification. It is often used for colds, spleen and stomach cold syndrome, stomach cold vomiting, lung cold cough, and detoxification of fish and crabs. Ginger and dried ginger are pungent and warm in nature, and belong to the lung, stomach, and spleen meridians; clinically, they are mainly used to dispel cold, warm the middle and stop vomiting, and warm the lungs and stop coughs. It is often used for spleen and stomach deficiency and cold, loss of appetite, nausea and vomiting, or vomiting with phlegm and fluid, vomiting due to stomach disharmony, cold or cold phlegm cough, cold and wind, aversion to wind and fever, nasal congestion and headache. It can also relieve drug poisoning such as raw pinellia and raw arisaema, as well as food poisoning such as fish and crabs. Modern pharmacological studies have shown that ginger has antibacterial, anti-cancer, antioxidant and anti-aging effects. Its unique "gingerol" can effectively treat abdominal distension, abdominal pain, diarrhea, vomiting and other symptoms caused by overeating cold food. In addition, ginger can increase appetite and promote the secretion of digestive juices; gingerol in ginger also has a strong choleretic effect. In addition, pharmacological studies have shown that methanol or ether extracts of ginger have sedative, analgesic, anti-inflammatory, antiemetic and transient hypertension effects; water extracts or volatile oils can significantly prolong the time of thrombosis; alcohol extracts and the gingerols and gingerolene ketones they contain have significant snail-killing and anti-schistosomiasis effects. The functions and indications in traditional Chinese medicine are: warming the meridians and dispersing cold, restoring yang and unblocking the meridians, and drying dampness and eliminating phlegm. It is used for cold pain in the abdomen, vomiting and diarrhea, cold limbs and weak pulse, phlegm and cough. Dried ginger can guide blood-related medicines into the blood, and qi-related medicines into the qi. It can also remove evil and nourish new things, which means that yang gives birth to yin and yin grows. Therefore, it can be used by people with blood deficiency, and it is also suitable for symptoms such as vomiting blood, epistaxis, and bleeding.

The 2020 edition of the Chinese Pharmacopoeia contains two entries: dried ginger and fresh ginger. Dried ginger is the dried rhizome of ginger, a plant of the ginger family. It is dug in winter, with the fibrous roots and mud removed, and then sun-dried or low-temperature dried. The sliced slices are dried in the sun or low-temperature dried, and are called "dried ginger slices". Fresh ginger is the fresh rhizome of ginger, a plant of the ginger family. It is dug in autumn and the fibrous roots and mud are removed. Ginger oil can be obtained from dried ginger and fresh ginger through steam distillation or supercritical carbon dioxide extraction.

Ginger Oil, also known as ginger oil, is a light yellow to yellow oily liquid extracted from fresh or dried ginger. It has a special smell and spicy taste, with the characteristic aroma of ginger. The main components of ginger oil are gingerol (also known as gingerol), zingiberene, gingerol, gingerone, citral, phellandrene, borneol, etc.

Gingerol is a typical bioactive component found in dried ginger, fresh ginger and ginger oil. It is a yellow oily liquid with a spicy and bitter taste. It is reported to have a relative density of 1.0713, a refractive index of 1.5212, and a boiling point of 235-240°C (2.39 kPa). It is believed that the total gingerol (collectively known as gingerol) content in dried ginger is as high as 9.6%. The chemical structural formulas of several typical gingerol compounds are shown in Formula I below:

Formula I

Among them: n=4 is 6-gingerol (C17H26O4), n=6 is 8-gingerol (C19H30O4), n=8 is 10-gingerol (C21H34O4), n=8 is 12-gingerol (C23H38O4), 6-gingerol is also called 6-gingerol, and the names of other gingerols are also expressed by analogy.

Among them, the chemical name of 6-gingerol is (5S)-5-hydroxy-1-(4-hydroxy-3-methoxyphenyl) decan-3-one, the English chemical name is (5S)-5-Hydroxy-1-(4-hydroxy-3-methoxy-phenyl) decan-3-one, the molecular formula is C17H26O4, and the molecular weight is 294.39. It is known that 6-gingerol has multiple biological activities such as anticoagulant, antimutagenic, antirheumatic, cold-dispelling, antioxidant, antitumor, cardiotonic, hypolipidemic, hypoglycemic, anti-atherosclerotic, gastric mucosal protection, liver protection and gallbladder promotion, anti-inflammatory, antitussive, anti-dizziness and anti-vomiting, and central nervous system inhibition. It also has insecticidal, anti-pathogenic microorganism and bactericidal and preservative effects. Among them, the anti-tumor effect of 6-gingerol is the most concerned.

6-Gingerol is the main phenolic compound and the most important irritant component of ginger oil isolated from the rhizome of the ginger family (Thresh, Pharm. J. [3] 10, 171 (1879); 12, 721 (1881); 14, 798(1883); 15, 208 (1884); Garnett, Grier, Pharm. J. [4] 25, 118 (1907); Nelson, J. Am. Chem. Soc. 39, 1466 (1917)). For an earlier structural study of 6-gingerol, see Lapworth et al., J. Chem. Soc. 111, 777 (1917). For early review literature, see Redgrove, Pharm. J. 125, 54 (1930) and Jacobs, Am. Perfum. 48, no. 7, 60, 62 (1946). For evidence that there are a series of phenolic ketone homologues in the pungent components of ginger and that 6-gingerol is the main component, see DW Connell, MD Sutherland, Aust. J. Chem. 22, 1033 (1969). For the synthesis of the (±)-configuration of 6-gingerol, see: Hirao et al., Chem. Pharm. Bull. 20, 2287 (1972); K. Banno, T. Mukaiyama, Bull. Chem. Soc. Jpn. 49, 1453 (1976); P. Denniff, DA Whiting, Chem. Commun. 1976, 712; P.Denniff et al., J. Chem. Soc. Perkin Trans. 1 1981, 82. For the stereoselective synthesis of the S (+)-configuration, see: D. Enders et al., Ber. 112, 3703 (1979). For the biosynthesis of the (±)-configuration of 6-gingerol, see: P. Denniff, DA Whiting, Chem. Commun. 1976, 711; I. Macleod, DA Whiting, ibid. 1979, 1152; P. Denniff et al., J. Chem. Soc. Perkin Trans. 1 1980, 2637. For the physical properties and cardiotonic effects of gingerol, see: N. Shoji et al., J. Pharm. Sci. 71, 1174 (1982).

The prior art discloses some methods for preparing ginger oil, especially methods for preparing ginger oil by supercritical carbon dioxide extraction, but the products obtained by these methods have complex components, for example, contain a large amount of ketone compounds, and the method for preparing ginger oil mainly containing gingerol compounds has not been reported, especially the method for preparing ginger oil mainly containing 6-gingerol has not been reported. Therefore, the art still expects to provide a method for providing ginger oil mainly containing gingerol compounds, especially mainly containing 6-gingerol, with excellent biological activity.

Summary of the invention

The present invention aims to provide a method for preparing ginger oil, and in particular to provide a method for preparing ginger oil having excellent biological activity, mainly comprising gingerol compounds, and in particular to provide ginger oil having excellent biological activity, mainly comprising 6-gingerol. Alternatively, the present invention aims to provide ginger oil, and in particular to provide ginger oil having excellent biological activity, mainly comprising gingerol compounds, and in particular to provide ginger oil having excellent biological activity, mainly comprising 6-gingerol. It has been unexpectedly found that ginger oil having excellent biological activity, mainly comprising gingerol compounds, and in particular to provide ginger oil having excellent biological activity, mainly comprising 6-gingerol can be prepared using the method of the present invention, and the present invention is completed based on such a finding.

To this end, the first aspect of the present invention provides a ginger oil, which contains 550-650 mg/g of 6-gingerol, 55-65 mg/g of 8-gingerol, and 35-45 mg/g of 10-gingerol. The relative density of the ginger oil at 20° C. is in the range of 0.941±0.01, and the refractive index is in the range of 1.438±0.02.

The ginger oil according to the first aspect of the present invention comprises 580-650 mg/g of 6-gingerol, 58-62 mg/g of 8-gingerol and 38-44 mg/g of 10-gingerol. The relative density of the ginger oil at 20° C. is 0.941 and the refractive index is 1.438.

The ginger oil according to the first aspect of the present invention is prepared according to any method described in the third aspect of the present invention.

Furthermore, the second aspect of the present invention provides use of the ginger oil described in any one of the first aspects of the present invention in preparing a product for inhibiting inflammation.

Furthermore, the third aspect of the present invention provides a method for preparing the ginger oil according to any one of the first aspects of the present invention, comprising the following steps:

(1) A supercritical carbon dioxide extraction system is provided, which includes an extraction tank, and also includes a first separation tank, a second separation tank and a third separation tank connected in series in sequence according to the flow direction of carbon dioxide, wherein the second separation tank is filled with a plurality of glass balls with a diameter of 2 to 10 mm, and the surfaces of the glass balls are coated with a propylene glycol-acetic acid mixture with a volume ratio of 10 to 15:1;

(2) The extraction tank of the supercritical carbon dioxide extraction system is pre-filled with dried ginger powder that has been crushed to a particle size of 20-30 meshes. After the carbon dioxide enters the extraction tank, the gas temperature in the tank is adjusted to 32-40° C. and the pressure is adjusted to 40-50 mPa. Extraction is performed under supercritical conditions of temperature and pressure for 2-8 hours;

(3) After the extraction is completed, the carbon dioxide in the extraction tank is pumped into the first separation tank, and the temperature and pressure in the tank are adjusted to 38±3°C and 15±4mPa respectively and maintained for 1 hour; then,

The carbon dioxide in the first separation tank is pumped into the second separation tank, and the temperature and pressure in the tank are adjusted to 33±2°C and 8±1mPa respectively and maintained for 2 hours; then,

The carbon dioxide in the second separation tank is pumped into the third separation tank, and the temperature and pressure in the tank are adjusted to 29±2°C and 2±0.5mPa respectively and maintained for 1 hour, and then the carbon dioxide is discharged;

(4) Discharge the separated product in the second separation tank, wash it with purified water added to the second separation tank, combine the separated product and the washing liquid into a separatory funnel, let it stand, separate and discard the water phase, and obtain ginger oil.

According to the method of the first aspect of the present invention, in the supercritical carbon dioxide extraction system, the following devices are connected through a high-pressure fluid pipeline according to the flow direction of carbon dioxide:

A carbon dioxide gas storage tank, which is used to provide a carbon dioxide gas source;

A gas storage tank, which is used to temporarily store the carbon dioxide gas source from the carbon dioxide gas storage tank and optionally the carbon dioxide recovery gas recovered from the system;

A plurality of high-pressure pumps, which are arranged on the high-pressure fluid pipelines between the devices downstream of the gas storage tank, and each high-pressure pump is used to transmit and adjust the pressure of carbon dioxide to the next device;

A heat exchanger for adjusting the temperature of the pressurized carbon dioxide gas to the level required by the extraction process;

An extraction tank, which is used to extract the material dosed therein with supercritical carbon dioxide;

A separation tank, comprising a first separation tank, a second separation tank and a third separation tank connected in series in sequence according to the flow direction of carbon dioxide, a discharge valve being arranged at the bottom of the separation tank, wherein the second separation tank is filled with a plurality of glass balls with a diameter of 2 to 10 mm, a high-pressure fluid pipeline entering the second separation tank is inserted into the glass ball group, and the surface of the glass ball is coated with a propylene glycol-acetic acid mixture with a volume ratio of 10 to 15:1;

a flow meter installed downstream of the third separation tank and used to measure the flow rate of carbon dioxide derived from the third separation tank;

The condenser is installed downstream of the flow meter and is used to cool the carbon dioxide after the extraction and recover it into the gas storage tank.

According to the method described in the first aspect of the present invention, after the glass balls are filled into the second separation tank, a propylene glycol-acetic acid mixture is added to the tank to soak the glass balls, and then excess mixture in the tank is discharged to allow the surface of the glass balls to be coated with the propylene glycol-acetic acid mixture.

According to the method described in the first aspect of the present invention, the glass balls are pre-soaked in a propylene glycol-acetic acid mixture before being filled into the second separation tank, and then the glass balls are filled into the second separation tank.

According to the method described in the first aspect of the present invention, the glass ball group occupies 30-90% of the inner volume of the second separation tank.

According to the method described in the first aspect of the present invention, the glass ball group occupies 50-80% of the inner volume of the second separation tank.

According to the method described in the first aspect of the present invention, the material to be extracted filled in the extraction tank occupies 60-100% of the inner volume of the extraction tank.

According to the method described in the first aspect of the present invention, the volume of the separation tank is 5% to 50% of the volume of the extraction tank.

According to the method described in the first aspect of the present invention, the volume of the separation tank is 20% to 30% of the volume of the extraction tank.

According to the method of the first aspect of the present invention, the high-pressure fluid pipeline is a straight pipe or a flexible pipe, which can withstand a pressure of up to 100 mPa.

According to the method of the first aspect of the present invention, the carbon dioxide gas extracted from the gas storage tank is pressurized by a high-pressure pump and transported to a heat exchanger, where the gas is temperature-adjusted and then introduced into the extraction tank.

According to the method of the first aspect of the present invention, the high-pressure pump is capable of providing required pressure for its downstream devices such as an extraction tank and a separation tank.

According to the method of the first aspect of the present invention, a shut-off valve is provided between the devices connected via the high-pressure fluid pipeline as required.

According to the method of the first aspect of the present invention, the high-pressure fluid pipeline is used to transport gaseous carbon dioxide or liquid carbon dioxide.

According to the method of the first aspect of the present invention, the pressure in various types of tanks is precisely regulated by a high-pressure pump in combination with an additional pressure reducing valve.

According to the method described in the first aspect of the present invention, step (3) is performed as follows:

After the extraction is completed, the carbon dioxide in the extraction tank 5 is pumped into the first separation tank, and the temperature and pressure in the tank are adjusted to 38±3°C and 15±4mPa respectively and maintained for 1 hour; then,

The carbon dioxide in the first separation tank is pumped into the second separation tank, and the temperature and pressure in the tank are adjusted to 33±2°C and 8±1mPa respectively and maintained for 2 hours; then,

The carbon dioxide in the second separation tank is pumped into the third separation tank, and the temperature and pressure in the tank are adjusted to 29±2°C and 2±0.5mPa respectively and maintained for 1 hour, and then the carbon dioxide is exported to the flow meter, condenser and gas storage tank;

According to the method of the first aspect of the present invention, step (4) is performed as follows:

The separated product in the second separation tank was discharged, and purified water was added to the second separation tank for washing, 250 ml each time, and the separated product and the washing liquid were combined into a separating funnel, allowed to stand, separated and the water phase was discarded to obtain ginger oil.

The method according to the first aspect of the present invention comprises the following steps:

(1) A supercritical carbon dioxide extraction system is provided, which connects the following devices through a high-pressure fluid pipeline according to the flow direction of carbon dioxide:

A carbon dioxide gas storage tank, which is used to provide a carbon dioxide gas source;

A gas storage tank, which is used to temporarily store the carbon dioxide gas source from the carbon dioxide gas storage tank and optionally the carbon dioxide recovery gas recovered from the system;

A plurality of high-pressure pumps, which are arranged on the high-pressure fluid pipelines between the devices downstream of the gas storage tank, and each high-pressure pump is used to transmit and adjust the pressure of carbon dioxide to the next device;

A heat exchanger for adjusting the temperature of the pressurized carbon dioxide gas to the level required by the extraction process;

An extraction tank, which is used to extract the material dosed therein with supercritical carbon dioxide;

A separation tank, comprising a first separation tank, a second separation tank and a third separation tank connected in series in sequence according to the flow direction of carbon dioxide, a discharge valve being arranged at the bottom of the separation tank, wherein the second separation tank is filled with a plurality of glass balls with a diameter of 5 mm, a high-pressure fluid pipeline entering the second separation tank is inserted into the glass ball group, and the surface of the glass ball is coated with a propylene glycol-acetic acid mixture;

a flow meter installed downstream of the third separation tank and used to measure the flow rate of carbon dioxide derived from the third separation tank;

A condenser installed downstream of the flow meter to cool the carbon dioxide after extraction and recover it into a gas storage tank;

in,

After the glass balls are filled into the second separation tank, a propylene glycol-acetic acid mixture is added to the tank to soak the glass balls, and then excess mixture in the tank is discharged, so that the surface of the glass balls is coated with the propylene glycol-acetic acid mixture in a volume ratio of 12.5:1;

The glass ball group occupies 70% of the inner volume of the second separation tank;

The gas storage tank receives both the initial carbon dioxide gas from the carbon dioxide gas storage tank and the recovered carbon dioxide gas after the extraction work is completed. The two sources of gas are mixed in the gas storage tank and then used again in the next batch of extraction process;

The volume of the extraction tank is 10L, and the dried ginger powder is pre-filled therein. After the carbon dioxide enters the extraction tank, the temperature of the gas in the tank is adjusted to 38±1°C and the pressure is adjusted to 46±2mPa. Extraction is performed under supercritical conditions of this temperature and pressure;

The volume of each separation tank is 25% of the volume of the extraction tank;

(2) pre-filling the extraction tank of the supercritical carbon dioxide extraction system of step (1) with 4 kg of dried ginger powder crushed to a particle size of 20-30 mesh, and extracting for 4 hours under the operating conditions of step (1);

(3) After the extraction is completed, the carbon dioxide in the extraction tank is pumped into the first separation tank, and the temperature and pressure in the tank are adjusted to 38±1°C and 15±2mPa respectively and maintained for 1 hour; then,

The carbon dioxide in the first separation tank is pumped into the second separation tank, and the temperature and pressure in the tank are adjusted to 33±1°C and 8±0.5mPa respectively and maintained for 2 hours; then,

The carbon dioxide in the second separation tank is pumped into the third separation tank, and the temperature and pressure in the tank are adjusted to 29±1°C and 2±0.2mPa respectively and maintained for 1 hour, and then the carbon dioxide is exported to the flow meter, condenser and gas storage tank;

(4) Discharge the separated product in the second separation tank, wash it three times with purified water added to the second separation tank, 250 ml each time, combine the separated product and the washing liquid into a separatory funnel, let it stand, separate and discard the water phase, and obtain ginger oil.

The method according to the first aspect of the present invention comprises the following steps:

(1) A supercritical carbon dioxide extraction system is provided, which connects the following devices through a high-pressure fluid pipeline according to the flow direction of carbon dioxide:

A carbon dioxide gas storage tank, which is used to provide a carbon dioxide gas source;

A gas storage tank, which is used to temporarily store the carbon dioxide gas source from the carbon dioxide gas storage tank and optionally the carbon dioxide recovery gas recovered from the system;

A plurality of high-pressure pumps, which are arranged on the high-pressure fluid pipelines between the devices downstream of the gas storage tank, and each high-pressure pump is used to transmit and adjust the pressure of carbon dioxide to the next device;

A heat exchanger for adjusting the temperature of the pressurized carbon dioxide gas to the level required by the extraction process;

An extraction tank, which is used to extract the material dosed therein with supercritical carbon dioxide;

A separation tank, comprising a first separation tank, a second separation tank and a third separation tank connected in series in sequence according to the flow direction of carbon dioxide, a discharge valve being arranged at the bottom of the separation tank, wherein the second separation tank is filled with a plurality of glass balls with a diameter of 8 mm, a high-pressure fluid pipeline entering the second separation tank is inserted into the glass ball group, and the surface of the glass ball is coated with a propylene glycol-acetic acid mixture;

a flow meter installed downstream of the third separation tank and used to measure the flow rate of carbon dioxide derived from the third separation tank;

A condenser installed downstream of the flow meter to cool the carbon dioxide after extraction and recover it into a gas storage tank;

in,

After the glass balls are filled into the second separation tank, a propylene glycol-acetic acid mixture is added to the tank to soak the glass balls, and then excess mixture in the tank is discharged, so that the surface of the glass balls is coated with the propylene glycol-acetic acid mixture in a volume ratio of 10:1;

The glass ball group occupies 75% of the inner volume of the second separation tank;

The gas storage tank receives both the initial carbon dioxide gas from the carbon dioxide gas storage tank and the recovered carbon dioxide gas after the extraction work is completed. The two sources of gas are mixed in the gas storage tank and then used again in the next batch of extraction process;

The volume of the extraction tank is 10L, and the dried ginger powder is pre-filled therein. After the carbon dioxide enters the extraction tank, the temperature of the gas in the tank is adjusted to 38±1°C and the pressure is adjusted to 46±2mPa. Extraction is performed under supercritical conditions of this temperature and pressure;

The volume of each separation tank is 30% of the volume of the extraction tank;

(2) pre-filling the extraction tank of the supercritical carbon dioxide extraction system of step (1) with 4 kg of dried ginger powder crushed to a particle size of 20-30 mesh, and extracting for 3.5 hours under the operating conditions of step (1);

(3) After the extraction is completed, the carbon dioxide in the extraction tank is pumped into the first separation tank, and the temperature and pressure in the tank are adjusted to 38±1°C and 15±2mPa respectively and maintained for 1 hour; then,

The carbon dioxide in the first separation tank is pumped into the second separation tank, and the temperature and pressure in the tank are adjusted to 33±1°C and 8±0.5mPa respectively and maintained for 2 hours; then,

The carbon dioxide in the second separation tank is pumped into the third separation tank, and the temperature and pressure in the tank are adjusted to 29±1°C and 2±0.2mPa respectively and maintained for 1 hour, and then the carbon dioxide is exported to the flow meter, condenser and gas storage tank;

(4) Discharge the separated product in the second separation tank, wash it three times with purified water added to the second separation tank, 250 ml each time, combine the separated product and the washing liquid into a separatory funnel, let it stand, separate and discard the water phase, and obtain ginger oil.

The method according to the first aspect of the present invention comprises the following steps:

(1) A supercritical carbon dioxide extraction system is provided, which connects the following devices through a high-pressure fluid pipeline according to the flow direction of carbon dioxide:

A carbon dioxide gas storage tank, which is used to provide a carbon dioxide gas source;

A gas storage tank, which is used to temporarily store the carbon dioxide gas source from the carbon dioxide gas storage tank and optionally the carbon dioxide recovery gas recovered from the system;

A plurality of high-pressure pumps, which are arranged on the high-pressure fluid pipelines between the devices downstream of the gas storage tank, and each high-pressure pump is used to transmit and adjust the pressure of carbon dioxide to the next device;

A heat exchanger for adjusting the temperature of the pressurized carbon dioxide gas to the level required by the extraction process;

An extraction tank, which is used to extract the material dosed therein with supercritical carbon dioxide;

A separation tank, comprising a first separation tank, a second separation tank and a third separation tank connected in series in sequence according to the flow direction of carbon dioxide, a discharge valve being arranged at the bottom of the separation tank, wherein the second separation tank is filled with a plurality of glass balls with a diameter of 3 mm, a high-pressure fluid pipeline entering the second separation tank is inserted into the glass ball group, and the surface of the glass ball is coated with a propylene glycol-acetic acid mixture;

a flow meter installed downstream of the third separation tank and used to measure the flow rate of carbon dioxide derived from the third separation tank;

A condenser installed downstream of the flow meter to cool the carbon dioxide after extraction and recover it into a gas storage tank;

in,

After the glass balls are filled into the second separation tank, a propylene glycol-acetic acid mixture is added to the tank to soak the glass balls, and then excess mixture in the tank is discharged, so that the surface of the glass balls is coated with the propylene glycol-acetic acid mixture in a volume ratio of 15:1;

The glass ball group occupies 65% of the inner volume of the second separation tank;

The gas storage tank receives both the initial carbon dioxide gas from the carbon dioxide gas storage tank and the recovered carbon dioxide gas after the extraction work is completed. The two sources of gas are mixed in the gas storage tank and then used again in the next batch of extraction process;

The volume of the extraction tank is 10L, and the dried ginger powder is pre-filled therein. After the carbon dioxide enters the extraction tank, the temperature of the gas in the tank is adjusted to 38±1°C and the pressure is adjusted to 46±2mPa. Extraction is performed under supercritical conditions of this temperature and pressure;

The volume of each separation tank is 20% of the volume of extraction tank 5;

(2) pre-filling the extraction tank of the supercritical carbon dioxide extraction system of step (1) with 4 kg of dried ginger powder crushed to a particle size of 20-30 mesh, and extracting for 5 hours under the operating conditions of step (1);

(3) After the extraction is completed, the carbon dioxide in the extraction tank is pumped into the first separation tank, and the temperature and pressure in the tank are adjusted to 38±1°C and 15±2mPa respectively and maintained for 1 hour; then,

The carbon dioxide in the first separation tank is pumped into the second separation tank, and the temperature and pressure in the tank are adjusted to 33±1°C and 8±0.5mPa respectively and maintained for 2 hours; then,

The carbon dioxide in the second separation tank is pumped into the third separation tank, and the temperature and pressure in the tank are adjusted to 29±1°C and 2±0.2mPa respectively and maintained for 1 hour, and then the carbon dioxide is exported to the flow meter, condenser and gas storage tank;

(4) Discharge the separated product in the second separation tank, wash it three times with purified water added to the second separation tank, 250 ml each time, combine the separated product and the washing liquid into a separatory funnel, let it stand, separate and discard the water phase, and obtain ginger oil.

The technical principle of supercritical extraction, generally speaking, is to use the relationship between the solubility of supercritical fluid (SCF, using carbon dioxide as supercritical fluid) and its density, that is, to use the influence of pressure and temperature on the solubility of supercritical fluid. In the supercritical state, the supercritical fluid is contacted with the substance to be separated, so that it can selectively extract the relevant components in sequence. Of course, the extract obtained corresponding to each pressure range cannot be single, but the conditions can be controlled to obtain the best proportion of mixed components, and then the supercritical fluid is turned into ordinary gas by means of decompression and temperature increase, and the extracted substance is completely or basically precipitated, thereby achieving the purpose of separation and purification. Therefore, the supercritical fluid extraction process is a combination of extraction and separation processes.

Supercritical CO ₂ refers to a compressible high-density fluid that is above the critical temperature and critical pressure (called the critical point). It is the fourth state besides the three states of gas, liquid and solid. Its intermolecular force is very small, similar to gas, but its density is very large, close to liquid. Therefore, it has the dual properties of gas and liquid between gas and liquid. At the same time, it has higher solubility of liquid and higher fluidity of gas. Its mass transfer rate is higher than that of ordinary liquid solvents, and its diffusion coefficient is between that of liquid and gas. It has good permeability and no interphase effect, so it helps to improve the extraction efficiency and can save energy significantly. The physical and chemical properties of supercritical CO ₂ are very different from those of liquids and gases in non-critical states. Since density is the solubility, viscosity is the fluid resistance, and diffusion coefficient is the main parameter of mass transfer rate, the special properties of supercritical CO ₂ determine that supercritical CO ₂ extraction technology has a series of important characteristics.

It has been found that the ginger oil prepared by the method of the present invention has certain excellent properties, such as excellent physical and chemical properties and biological properties.

BRIEF DESCRIPTION OF THE DRAWINGS

Figure 1: Schematic diagram of supercritical fluid extraction equipment process.

Fig. 2: HPLC chart of ginger oil b obtained in Example 2, in which the retention time of 6-gingerol is 17.14 min, the retention time of 8-gingerol is 25.86 min (relative retention time 1.509), and the retention time of 10-gingerol is 41.62 min (relative retention time 2.428).

Some structural devices involved in the supercritical carbon dioxide extraction system mentioned in the present invention and their figure marks are summarized as follows: carbon dioxide gas storage tank 1, gas storage tank 2, high-pressure pump 3, heat exchanger 4, extraction tank 5, separation tank 6, first separation tank 6a, second separation tank 6b, third separation tank 6c, flow meter 7, condenser 8, high-pressure fluid pipeline 9, shut-off valve 10.

Detailed ways

The present invention can be further described by the following examples, however, the scope of the present invention is not limited to the following examples. It will be appreciated by those skilled in the art that various changes and modifications may be made to the present invention without departing from the spirit and scope of the present invention. The present invention provides general and/or specific descriptions of the materials and test methods used in the test. Although many materials and operating methods used to achieve the purpose of the present invention are well known in the art, the present invention is still described in as much detail as possible at this point.

Example 1: Providing a general supercritical carbon dioxide extraction system

The various components and equipment of the supercritical carbon dioxide extraction system of the present invention can be easily obtained from commercial sources or designed and purchased according to the production scale. The supercritical carbon dioxide extraction system provided by the present invention is generally similar to the existing supercritical carbon dioxide extraction system in structure, but some components or devices are modified. For example, a schematic embodiment of the present invention shown in FIG. 1 connects the following typical (necessary) devices through a high-pressure fluid pipeline 9 according to the flow direction of carbon dioxide:

A carbon dioxide gas storage tank 1, which is used to provide a carbon dioxide gas source;

A gas storage tank 2, which is used to temporarily store the carbon dioxide gas source from the carbon dioxide gas storage tank 1 and optionally the carbon dioxide recovery gas recovered from the system;

A plurality of high-pressure pumps 3, which are arranged on the high-pressure fluid pipeline 9 between the devices downstream of the gas storage tank 2, and each high-pressure pump 3 is used to transmit and adjust the pressure of carbon dioxide to the next device;

A heat exchanger 4, which is used to adjust the temperature of the pressurized carbon dioxide gas to the degree required by the extraction process;

An extraction tank 5, which is used to extract the material dosed therein with supercritical carbon dioxide;

The separation tank 6 comprises a first separation tank 6a, a second separation tank 6b and a third separation tank 6c which are connected in series in sequence according to the flow direction of carbon dioxide, and a discharge valve is provided at the bottom of the separation tank, wherein the second separation tank 6b is filled with a plurality of glass balls with a diameter of 2 to 10 mm, and a high-pressure fluid pipeline 9 entering the second separation tank 6b is inserted into the glass ball group, and the surface of the glass ball is coated with a propylene glycol-acetic acid mixture with a volume ratio of 10 to 15:1;

A flow meter 7, which is installed downstream of the third separation tank 6c and is used to measure the flow rate of carbon dioxide derived from the third separation tank 6c;

The condenser 8 is installed downstream of the flow meter 7 and is used to cool the carbon dioxide after the extraction and recover it into the gas storage tank 2.

In one embodiment of the above-mentioned supercritical carbon dioxide extraction system, after the glass balls are filled into the second separation tank 6b, a propylene glycol-acetic acid mixture is added into the tank to soak the glass balls, and then the excess mixture in the tank is discharged to make the surface of the glass balls coated with the propylene glycol-acetic acid mixture; alternatively, the glass balls are soaked in the propylene glycol-acetic acid mixture before being filled into the second separation tank 6b, and then the glass balls are filled into the second separation tank 6b.

In one embodiment of the above supercritical carbon dioxide extraction system, the glass ball group occupies 30-90% of the inner volume of the second separation tank 6b, preferably 50-80%.

In one embodiment of the above-mentioned supercritical carbon dioxide extraction system, the carbon dioxide storage tank 1 is a conventional carbon dioxide storage cylinder, and the carbon dioxide gas stored therein can be exported to subsequent devices through a high-pressure fluid pipeline 9. In one embodiment, after the carbon dioxide comes out of the carbon dioxide storage tank 1, it temporarily enters the gas storage tank 2.

The gas storage tank 2 receives both the initial carbon dioxide gas from the carbon dioxide storage tank 1 and optionally the carbon dioxide recovery gas after the extraction work is completed. After the initial carbon dioxide gas and the carbon dioxide recovery gas are mixed in the gas storage tank 2, they can be used again in the next extraction process.

In one embodiment of the above-mentioned supercritical carbon dioxide extraction system, the volume of the extraction tank 5 can be determined according to the scale of production, for example, the volume can be in the range of 1L to 1000L or even wider. In view of the fact that carbon dioxide can be recycled, a smaller volume can also be designed to achieve the extraction of ginger oil by multi-batch extraction. In addition, the maximum tolerable pressure of the extraction tank 5 can be easily designed to reach a working pressure of up to 100mPa. The pressure in the extraction tank 5 can also be easily changed according to the process. In addition, the material to be extracted filled in the extraction tank 5 occupies 60 to 100% of the inner volume of the extraction tank 5.

In one embodiment of the above-mentioned supercritical carbon dioxide extraction system, the volume of the separation tank 6 can be determined according to the production scale, and can usually be smaller than the volume of the extraction tank 5, for example, it can be 5% to 50% of the volume of the extraction tank 5. Preferably, in the present invention, the volume of each separation tank 6 is 20% to 30% of the volume of the extraction tank 5. In addition, the maximum tolerable pressure of the separation tank 6 can be easily designed to reach a working pressure of up to 80mPa. The pressure in the separation tank 6 can also be easily changed according to the process.

In one embodiment of the above-mentioned supercritical carbon dioxide extraction system, the extraction tank 5 is pre-filled with ginger powder crushed to a particle size of 20-30 mesh. After the carbon dioxide enters the extraction tank 5, the gas temperature in the tank is adjusted to 32-40°C and the pressure is adjusted to 40-50 mPa. Extraction is performed under supercritical conditions of this temperature and pressure for 2-8 hours.

In one embodiment of the supercritical carbon dioxide extraction system, the high-pressure fluid pipeline 9 can be a straight pipe or a flexible pipe. These high-pressure fluid pipelines can withstand a pressure of up to 100 mPa.

In one embodiment of the above-mentioned supercritical carbon dioxide extraction system, the carbon dioxide gas extracted from the gas storage tank 2 is pressurized by a high-pressure pump 3 and transported to a heat exchanger 4, where the gas is temperature-adjusted and then introduced into an extraction tank 5.

In one embodiment of the above-mentioned supercritical carbon dioxide extraction system, a condenser 8 is further included, which is installed downstream of the flow meter 7, and is used to cool the carbon dioxide after the extraction and recover it to the gas storage tank 2. Of course, in another embodiment, the condenser 8 may not be provided, or the carbon dioxide after the extraction may not be recovered.

In one embodiment of the supercritical carbon dioxide extraction system, the high-pressure pump 3 is capable of providing required pressure to its downstream devices such as the extraction tank 5 and the separation tank 6 .

In one embodiment of the supercritical carbon dioxide extraction system, a shutoff valve 10 is provided between the devices connected via the high-pressure fluid pipeline 9 as required.

In one embodiment of the above-mentioned supercritical carbon dioxide extraction system, the high-pressure fluid pipeline 9 is used to transport carbon dioxide in various forms or states, such as gaseous carbon dioxide or liquid carbon dioxide.

In one embodiment of the above-mentioned supercritical carbon dioxide extraction system, the pressure in various types of tanks can be accurately regulated by a high-pressure pump 3 in combination with an additional pressure reducing valve (which can be easily set by a person skilled in the art, and is not shown in FIG. 1 of the present invention).

According to the supercritical carbon dioxide extraction system provided in Example 1, ginger oil can be prepared in the present invention by including the following general operations and exemplary material ratios and amounts and equipment scales (material ratios and amounts and equipment scales can be easily adjusted according to production requirements):

(1) providing the supercritical carbon dioxide extraction system described above in this embodiment;

(2) The extraction tank 5 of the supercritical carbon dioxide extraction system is pre-filled with dried ginger powder crushed to a particle size of 20-30 meshes, and after the carbon dioxide enters the extraction tank 5, the gas temperature in the tank is adjusted to 32-40° C. and the pressure is adjusted to 40-50 mPa, and extraction is performed under the supercritical conditions of temperature and pressure for 2-8 hours;

(3) After the extraction is completed, the carbon dioxide in the extraction tank 5 is pumped into the first separation tank 6a, and the temperature and pressure in the tank are adjusted to 38±3°C and 15±4mPa respectively and maintained for 1 hour; then

The carbon dioxide in the first separation tank 6a is pumped into the second separation tank 6b, and the temperature and pressure in the tank are adjusted to 33±2°C and 8±1mPa respectively and maintained for 2 hours; then

The carbon dioxide in the second separation tank 6b is pumped into the third separation tank 6c, and the temperature and pressure in the tank are adjusted to 29±2°C and 2±0.5mPa respectively and maintained for 1 hour, and then the carbon dioxide is led out to the flow meter 7, the condenser 8 and the gas storage tank 2;

(4) Discharge the separated product in the second separation tank 6b, add purified water to the second separation tank 6b and wash it three times, 250 ml each time, combine the separated product and the washing liquid into a separatory funnel, let it stand, separate and discard the water phase, and obtain ginger oil b.

Example 2: Extraction of ginger oil using a supercritical carbon dioxide extraction system

The basic configuration of the supercritical carbon dioxide extraction system for extracting ginger oil in this embodiment is as shown in Example 1. The size or scale of each component device can be adjusted appropriately. The extraction process steps are as follows:

(1) A supercritical carbon dioxide extraction system is provided, which connects the following devices through a high-pressure fluid pipeline 9 according to the flow direction of carbon dioxide:

A carbon dioxide gas storage tank 1, which is used to provide a carbon dioxide gas source;

A gas storage tank 2, which is used to temporarily store the carbon dioxide gas source from the carbon dioxide gas storage tank 1 and optionally the carbon dioxide recovery gas recovered from the system;

A plurality of high-pressure pumps 3, which are arranged on the high-pressure fluid pipeline 9 between the devices downstream of the gas storage tank 2, and each high-pressure pump 3 is used to transmit and adjust the pressure of carbon dioxide to the next device;

A heat exchanger 4, which is used to adjust the temperature of the pressurized carbon dioxide gas to the degree required by the extraction process;

An extraction tank 5, which is used to extract the material dosed therein with supercritical carbon dioxide;

The separation tank 6 comprises a first separation tank 6a, a second separation tank 6b and a third separation tank 6c which are connected in series in sequence according to the flow direction of carbon dioxide, and a discharge valve is provided at the bottom of the separation tank, wherein the second separation tank 6b is filled with a plurality of glass balls with a diameter of 5 mm, and a high-pressure fluid pipeline 9 entering the second separation tank 6b is inserted into the glass ball group, and the surface of the glass ball is coated with a propylene glycol-acetic acid mixture;

A flow meter 7, which is installed downstream of the third separation tank 6c and is used to measure the flow rate of carbon dioxide derived from the third separation tank 6c;

A condenser 8 installed downstream of the flow meter 7 is used to cool the carbon dioxide after extraction and recover it into the gas storage tank 2;

in,

After the glass balls are filled into the second separation tank 6b, a propylene glycol-acetic acid mixture is added to the tank to soak the glass balls, and then the excess mixture in the tank is discharged, so that the surface of the glass balls is coated with the propylene glycol-acetic acid mixture with a volume ratio of 12.5:1;

The glass ball group occupies 70% of the inner volume of the second separation tank 6b;

The gas storage tank 2 receives both the initial carbon dioxide gas from the carbon dioxide gas storage tank 1 and the recovered carbon dioxide gas after the extraction work is completed. The gases from the two sources are mixed in the gas storage tank 2 and then used again in the next batch of extraction process.

The volume of the extraction tank 5 is 10L, and the dried ginger powder is pre-filled therein. After the carbon dioxide enters the extraction tank 5, the temperature of the gas in the tank is adjusted to 38±1°C and the pressure is adjusted to 46±2mPa. Extraction is performed under supercritical conditions of this temperature and pressure.

The volume of each separation tank 6 is 25% of the volume of the extraction tank 5;

(2) pre-filling the extraction tank 5 of the supercritical carbon dioxide extraction system of step (1) with 4 kg of dried ginger powder crushed to a particle size of 20-30 mesh, and extracting for 4 hours under the operating conditions of step (1);

(3) After the extraction is completed, the carbon dioxide in the extraction tank 5 is pumped into the first separation tank 6a, and the temperature and pressure in the tank are adjusted to 38±1°C and 15±2mPa respectively and maintained for 1 hour; then

The carbon dioxide in the first separation tank 6a is pumped into the second separation tank 6b, and the temperature and pressure in the tank are adjusted to 33±1°C and 8±0.5mPa respectively and maintained for 2 hours; then

The carbon dioxide in the second separation tank 6b is pumped into the third separation tank 6c, and the temperature and pressure in the tank are adjusted to 29±1°C and 2±0.2mPa respectively and maintained for 1 hour, and then the carbon dioxide is led out to the flow meter 7, the condenser 8 and the gas storage tank 2;

(4) The separated material in the second separation tank 6b was discharged, and the separated material was washed three times with 250 ml of purified water added to the second separation tank 6b each time. The separated material and the washing liquid were combined into a separatory funnel, allowed to stand, separated and the aqueous phase was discarded to obtain 68.1 g of ginger oil b, which was a light yellow oily liquid with a relative density (20°C) of 0.941 and a refractive index (20°C) of 1.438 (the relative density of the ginger oil b in Example 3 and Example 4 was both within the range of 0.941±0.01, and the refractive index was both within the range of 1.438±0.02).

In addition, referring to the washing and liquid separation method in the above step (4), 17.4 g of ginger oil a was harvested from the first separation tank 6a, and 266.2 g of ginger oil c was harvested from the third separation tank 6c.

Ginger oil a, ginger oil b and ginger oil c refer to the oily substances separated from the first separation tank 6a, the second separation tank 6b and the third separation tank 6c respectively. This meaning is meant when ginger oil a, ginger oil b and ginger oil c are mentioned in the context of the present invention.

If not otherwise specified, the dried ginger powder used in preparing ginger oil in the present invention is from the same batch.

Example 3: Extraction of ginger oil using a supercritical carbon dioxide extraction system

The basic configuration of the supercritical carbon dioxide extraction system for extracting ginger oil in this embodiment is as shown in Example 1. The size or scale of each component device can be adjusted appropriately. The extraction process steps are as follows:

(1) A supercritical carbon dioxide extraction system is provided, which connects the following devices through a high-pressure fluid pipeline 9 according to the flow direction of carbon dioxide:

A carbon dioxide gas storage tank 1, which is used to provide a carbon dioxide gas source;

A gas storage tank 2, which is used to temporarily store the carbon dioxide gas source from the carbon dioxide gas storage tank 1 and optionally the carbon dioxide recovery gas recovered from the system;

A plurality of high-pressure pumps 3, which are arranged on the high-pressure fluid pipeline 9 between the devices downstream of the gas storage tank 2, and each high-pressure pump 3 is used to transmit and adjust the pressure of carbon dioxide to the next device;

A heat exchanger 4, which is used to adjust the temperature of the pressurized carbon dioxide gas to the degree required by the extraction process;

An extraction tank 5, which is used to extract the material dosed therein with supercritical carbon dioxide;

The separation tank 6 comprises a first separation tank 6a, a second separation tank 6b and a third separation tank 6c which are connected in series in sequence according to the flow direction of carbon dioxide, and a discharge valve is provided at the bottom of the separation tank, wherein the second separation tank 6b is filled with a plurality of glass balls with a diameter of 8 mm, and a high-pressure fluid pipeline 9 entering the second separation tank 6b is inserted into the glass ball group, and the surface of the glass ball is coated with a propylene glycol-acetic acid mixture;

A flow meter 7, which is installed downstream of the third separation tank 6c and is used to measure the flow rate of carbon dioxide derived from the third separation tank 6c;

A condenser 8 installed downstream of the flow meter 7 is used to cool the carbon dioxide after extraction and recover it into the gas storage tank 2;

in,

After the glass balls are filled into the second separation tank 6b, a propylene glycol-acetic acid mixture is added to the tank to soak the glass balls, and then the excess mixture in the tank is discharged, so that the surface of the glass balls is coated with the propylene glycol-acetic acid mixture in a volume ratio of 10:1;

The glass ball group occupies 75% of the inner volume of the second separation tank 6b;

The gas storage tank 2 receives both the initial carbon dioxide gas from the carbon dioxide gas storage tank 1 and the recovered carbon dioxide gas after the extraction work is completed. The gases from the two sources are mixed in the gas storage tank 2 and then used again in the next batch of extraction process.

The volume of the extraction tank 5 is 10L, and the dried ginger powder is pre-filled therein. After the carbon dioxide enters the extraction tank 5, the temperature of the gas in the tank is adjusted to 38±1°C and the pressure is adjusted to 46±2mPa. Extraction is performed under supercritical conditions of this temperature and pressure.

The volume of each separation tank 6 is 30% of the volume of the extraction tank 5;

(2) pre-filling the extraction tank 5 of the supercritical carbon dioxide extraction system of step (1) with 4 kg of dried ginger powder crushed to a particle size of 20-30 mesh, and extracting for 3.5 hours under the operating conditions of step (1);

(3) After the extraction is completed, the carbon dioxide in the extraction tank 5 is pumped into the first separation tank 6a, and the temperature and pressure in the tank are adjusted to 38±1°C and 15±2mPa respectively and maintained for 1 hour; then

The carbon dioxide in the first separation tank 6a is pumped into the second separation tank 6b, and the temperature and pressure in the tank are adjusted to 33±1°C and 8±0.5mPa respectively and maintained for 2 hours; then

The carbon dioxide in the second separation tank 6b is pumped into the third separation tank 6c, and the temperature and pressure in the tank are adjusted to 29±1°C and 2±0.2mPa respectively and maintained for 1 hour, and then the carbon dioxide is led out to the flow meter 7, the condenser 8 and the gas storage tank 2;

(4) The separated product in the second separation tank 6b was discharged and washed three times with 250 ml of purified water added to the second separation tank 6b each time. The separated product and the washing liquid were combined into a separatory funnel, allowed to stand, separated and the aqueous phase was discarded to obtain 69.2 g of ginger oil b as a light yellow oily liquid.

In addition, referring to the washing and liquid separation method in the above step (4), 17.1 g of ginger oil a was harvested from the first separation tank 6a, and 257.8 g of ginger oil c was harvested from the third separation tank 6c.

Example 4: Extraction of ginger oil using a supercritical carbon dioxide extraction system

The basic configuration of the supercritical carbon dioxide extraction system for extracting ginger oil in this embodiment is as shown in Example 1. The size or scale of each component device can be adjusted appropriately. The extraction process steps are as follows:

(1) A supercritical carbon dioxide extraction system is provided, which connects the following devices through a high-pressure fluid pipeline 9 according to the flow direction of carbon dioxide:

A carbon dioxide gas storage tank 1, which is used to provide a carbon dioxide gas source;

A gas storage tank 2, which is used to temporarily store the carbon dioxide gas source from the carbon dioxide gas storage tank 1 and optionally the carbon dioxide recovery gas recovered from the system;

A plurality of high-pressure pumps 3, which are arranged on the high-pressure fluid pipeline 9 between the devices downstream of the gas storage tank 2, and each high-pressure pump 3 is used to transmit and adjust the pressure of carbon dioxide to the next device;

A heat exchanger 4, which is used to adjust the temperature of the pressurized carbon dioxide gas to the degree required by the extraction process;

An extraction tank 5, which is used to extract the material dosed therein with supercritical carbon dioxide;

The separation tank 6 comprises a first separation tank 6a, a second separation tank 6b and a third separation tank 6c which are connected in series in sequence according to the flow direction of carbon dioxide, and a discharge valve is provided at the bottom of the separation tank, wherein the second separation tank 6b is filled with a plurality of glass balls with a diameter of 3 mm, and a high-pressure fluid pipeline 9 entering the second separation tank 6b is inserted into the glass ball group, and the surface of the glass ball is coated with a propylene glycol-acetic acid mixture;

A flow meter 7, which is installed downstream of the third separation tank 6c and is used to measure the flow rate of carbon dioxide derived from the third separation tank 6c;

A condenser 8 installed downstream of the flow meter 7 is used to cool the carbon dioxide after extraction and recover it into the gas storage tank 2;

in,

After the glass balls are filled into the second separation tank 6b, a propylene glycol-acetic acid mixture is added to the tank to soak the glass balls, and then the excess mixture in the tank is discharged, so that the surface of the glass balls is coated with the propylene glycol-acetic acid mixture in a volume ratio of 15:1;

The glass ball group occupies 65% of the inner volume of the second separation tank 6b;

The gas storage tank 2 receives both the initial carbon dioxide gas from the carbon dioxide gas storage tank 1 and the recovered carbon dioxide gas after the extraction work is completed. The gases from the two sources are mixed in the gas storage tank 2 and then used again in the next batch of extraction process.

The volume of the extraction tank 5 is 10L, and the dried ginger powder is pre-filled therein. After the carbon dioxide enters the extraction tank 5, the temperature of the gas in the tank is adjusted to 38±1°C and the pressure is adjusted to 46±2mPa. Extraction is performed under supercritical conditions of this temperature and pressure.

The volume of each separation tank 6 is 20% of the volume of the extraction tank 5;

(2) pre-filling the extraction tank 5 of the supercritical carbon dioxide extraction system of step (1) with 4 kg of dried ginger powder crushed to a particle size of 20-30 mesh, and extracting for 5 hours under the operating conditions of step (1);

(3) After the extraction is completed, the carbon dioxide in the extraction tank 5 is pumped into the first separation tank 6a, and the temperature and pressure in the tank are adjusted to 38±1°C and 15±2mPa respectively and maintained for 1 hour; then

The carbon dioxide in the first separation tank 6a is pumped into the second separation tank 6b, and the temperature and pressure in the tank are adjusted to 33±1°C and 8±0.5mPa respectively and maintained for 2 hours; then

The carbon dioxide in the second separation tank 6b is pumped into the third separation tank 6c, and the temperature and pressure in the tank are adjusted to 29±1°C and 2±0.2mPa respectively and maintained for 1 hour, and then the carbon dioxide is led out to the flow meter 7, the condenser 8 and the gas storage tank 2;

(4) The separated product in the second separation tank 6b was discharged and washed three times with 250 ml of purified water added to the second separation tank 6b each time. The separated product and the washing liquid were combined into a separatory funnel, allowed to stand, separated and the aqueous phase was discarded to obtain 64.7 g of ginger oil b as a light yellow oily liquid.

In addition, referring to the washing and liquid separation method in the above step (4), 18.7 g of ginger oil a was harvested from the first separation tank 6a, and 275.4 g of ginger oil c was harvested from the third separation tank 6c.

Example 5: Extraction of ginger oil using a supercritical carbon dioxide extraction system

This example refers to the operations of Example 2 herein, except that the surface of the glass ball is coated with propylene glycol in the second separation tank instead of the propylene glycol-acetic acid mixture; 71.4 g of ginger oil b, 17.5 g of ginger oil a, and 268.2 g of ginger oil c are obtained.

Example 6: Extraction of ginger oil using a supercritical carbon dioxide extraction system

This example refers to the operations of Example 2 herein, except that in the second separation tank, the surface of the glass ball is coated with an ethanol-acetic acid mixture with a volume ratio of 12.5:1 instead of a propylene glycol-acetic acid mixture; 67.9 g of ginger oil b, 18.2 g of ginger oil a, and 273.3 g of ginger oil c are obtained.

Test Example 1: Determination of the content of 6-gingerol, 8-gingerol and 10-gingerol in ginger oil

This test example provides the following HPLC method for determining the content of 6-gingerol, 8-gingerol, and 10-gingerol in ginger oil (or ginger and dried ginger):

Determined by high performance liquid chromatography (Chinese Pharmacopoeia 2020 Edition, Part IV, General Rules 0512);

Chromatographic conditions and system suitability test: octadecylsilane bonded silica gel was used as filler (Waters brand chromatograph, 4.6 mm × 200 mm, 5 μm); acetonitrile was used as mobile phase A, 0.1% formic acid solution was used as mobile phase B, and gradient elution was performed according to the provisions in the following table; the flow rate was 0.5 ml per minute, and the detection wavelength was 282 nm; the theoretical plate number calculated based on the 6-gingerol peak should be no less than 5000;

Preparation of reference solution: Take an appropriate amount of 6-gingerol reference substance (6-gingerol, Lot111833-202007, purchased from China National Institute for Food and Drug Control), accurately weigh it, and add methanol to make a 100µg/ml solution;

Preparation of test solution:

Method for preparing test solution for determination of ginger or dried ginger: Cut ginger into small pieces of 1-2 mm and accurately weigh about 1 g or accurately weigh about 1 g of dried ginger powder that has been passed through a No. 3 sieve, place in a 100 ml round-bottom flask, accurately add 50 ml of methanol, seal, weigh, heat and reflux for 30 minutes, cool, weigh again, make up the lost weight with methanol, shake well, filter, and take the filtrate. If necessary, dilute the mixture of mobile phase A and mobile phase B with a volume ratio of 45:55 to a concentration of 6-gingerol of 10-300 µg/ml;

The method for preparing the test solution when measuring the ginger oil or related materials prepared by the present invention is as follows: accurately weigh about 100 mg of the test sample, place it in a 50 ml volumetric flask, add methanol to dissolve and dilute to the scale, accurately draw 5 ml and place it in a 50 ml volumetric flask, add a mixture of mobile phase A and mobile phase B in a volume ratio of 45:55 and dilute to the scale, and obtain;

Determination method: Accurately pipette 20 μl of reference solution and test solution respectively, inject into liquid chromatograph, determine, and calculate the content of 6-gingerol; take 6-gingerol as reference, and use correction factors to calculate the contents of 8-gingerol and 10-gingerol respectively;

In the chromatogram of the test sample, the relative retention time of the chromatographic peaks of 8-gingerol and 10-gingerol and the corresponding chromatographic peak of 6-gingerol reference substance should be within the specified value of ±5%; taking the relative retention time of 6-gingerol as 1.00 and the correction factor as 1.0000, the relative retention time of 8-gingerol is 1.51, the correction factor is 0.7708, and the relative retention time of 10-gingerol is 2.42, and the correction factor is 0.7823.

The above HPLC method was used to determine the contents of 6-gingerol (which can be abbreviated as 6-JF or 6JF in the present invention), 8-gingerol (which can be abbreviated as 8-JF or 8JF in the present invention) and 10-gingerol (which can be abbreviated as 10-JF or 10JF in the present invention) in the ginger oil obtained in various examples of the present invention and the raw material dried ginger powder used. The results are shown in Table 1. FIG. 2 provides a typical HPLC chart of ginger oil b obtained in Example 2, in which the retention time of 6-gingerol is 17.14 min, the retention time of 8-gingerol is 25.86 min (relative retention time 1.509), and the retention time of 10-gingerol is 41.62 min (relative retention time 2.428).

Table 1:

According to the results in Table 1 above, the ginger oil b obtained in Examples 2 to 4 of the present invention contains up to 59 to 64% of 6-gingerol, and most of the 6-gingerol extracted from the extraction tank by supercritical carbon dioxide extraction is enriched in ginger oil b, while the 6-gingerol content in ginger oil a and ginger oil c is very low; unexpectedly, as shown in the results of Examples 5 to 6, when the surface of the glass ball in the second separation tank is not coated with propylene glycol-acetic acid mixed solution, the extracted 6-gingerol is less enriched in ginger oil b, and most of it is enriched in ginger oil c, but because the collection capacity of ginger oil c is large, the concentration of 6-gingerol in ginger oil c is still significantly lower than that of ginger oil b in Examples 2 to 4. In this sense, Examples 2 to 4 of the present invention provide a method for preparing ginger oil with a high content of 6-gingerol, namely ginger oil b.

Example 7: Extraction of ginger oil using a supercritical carbon dioxide extraction system

This example refers to the operations of Example 2 herein, except that in the second separation tank, the surface of the glass ball is coated with a glycerol-acetic acid mixture with a volume ratio of 12.5:1 instead of a propylene glycol-acetic acid mixture; 153.6 g of ginger oil b (6-gingerol 187.41 mg/g), 17.6 g of ginger oil a (6-gingerol 18.38 mg/g), and 193.4 g of ginger oil c (6-gingerol 56.82 mg/g) are obtained, wherein the concentration of 6-gingerol in the three ginger oils is significantly lower than that of the ginger oil b obtained in Example 2.

Example 8: Extraction of ginger oil using a supercritical carbon dioxide extraction system

This example refers to the operations of Example 2 herein, except that in the second separation tank, the surface of the glass ball is coated with a propylene glycol-formic acid mixture with a volume ratio of 12.5:1 instead of a propylene glycol-acetic acid mixture; 98.8g of ginger oil b, 18.2g of ginger oil a, and 264.6g of ginger oil c are obtained, wherein the concentration of 6-gingerol in ginger oil b is 402.13mg/g, and the other two ginger oils contain only trace amounts of 6-gingerol, and the total yield of 6-gingerol in the three ginger oils is 89.8%. These results show that although most of the 6-gingerol is basically recovered in ginger oil b, its recovery volume is large, resulting in a significantly lower 6-gingerol concentration than that of ginger oil b obtained in Example 2. In addition, the production environment safety and labor protection of formic acid are significantly inferior to those of acetic acid.

Test Example 2: Study on the effect of ginger oil in inhibiting inflammation

Existing literature records that ginger oil has the effect of inhibiting inflammation, such as the method described in Zhang Zhuxin's literature (Zhang Zhuxin, et al., Research on the Anti-inflammatory Effect of Ginger Oil, Chinese Herbal Medicine, 1989, 20(12):18), etc. This test example refers to these relevant literature methods to investigate the anti-inflammatory effect of some ginger oils prepared by the present invention.

The weights of the three ginger oils obtained in Example 2 of the present invention, namely ginger oil a, ginger oil b, and ginger oil c, and the 6-gingerol concentrations thereof are 68.1 g (604.73 mg/g), 17.4 g (21.42 mg/g), and 266.2 g (1.46 mg/g), respectively. According to the weight ratio of the three, 6.81 g, 1.74 g, and 26.62 g of the three ginger oils are accurately weighed, and mixed uniformly to obtain 35.17 g of mixed ginger oil Ex2 (wherein the 6-gingerol concentration is 119.14 mg/g and the content is 4.19 g), which is used as the control reagent of this test example.

1. Test drugs: ginger oil b obtained in Example 2, mixed ginger oil Ex2, ibuprofen tablets (Teyi Pharmaceutical, L11220809, H44021099), dexamethasone acetate tablets (Zhejiang Xianju, L190905, H33020822).

2. Animals: Kunming mice weighing 18-21 g and male Wistar rats weighing 140-180 g were purchased from the Institute of Medical Laboratory Animals, Chinese Academy of Medical Sciences, license number SCXK (Beijing) 2019-0011.

3. Inhibitory effect of xylene on mouse ear swelling

60 mice, both male and female, were randomly divided into 6 groups. The test drug was dissolved, suspended or emulsified in distilled water to an appropriate concentration in advance, and 20 ml of the drug solution was administered by gavage per 1 kg of animal body weight. The control group was given distilled water with the same volume, once a day for 5 consecutive days. One hour after the last administration, 0.05 ml of xylene was applied to the front and back of the right ear of each group of mice to induce inflammation. Four hours later, the mice were killed by cervical dislocation, the ears were cut off, and a round ear piece was punched in the same part of the left and right ears using a puncher with a diameter of 8 mm. The weight was weighed on an electronic balance, and the difference between the weights of the left and right ear pieces was used as the swelling degree, and the swelling inhibition rate was calculated. The results (x±s, n=10) are shown in Table 2 below.

Table 2:

Note: Compared with the control group, *P<0.05, **P<0.01 (the same below); #The dosage of the two test drugs, ginger oil b and mixed ginger oil Ex2, refers to the amount of 6-gingerol contained in the two test drugs administered per kg animal body weight. For example, when 600 mg/kg body weight of ginger oil b is administered, it means that 600 mg of 6-gingerol is administered to each 1 kg animal body weight, and when 600 mg/kg body weight of mixed ginger oil Ex2 is administered, it means that 600 mg of 6-gingerol is administered to each 1 kg animal body weight. Other similar expressions have similar meanings.

According to the results in the above table, although the dosages of the two test drugs, ginger oil b and mixed ginger oil Ex2, were the same in terms of 6-gingerol, their inhibitory effects on xylene-induced mouse ear swelling were significantly different. The possible reason is that although the animals orally took the same dose of 6-gingerol, the presence of a large amount of other ingredients in mixed ginger oil Ex2 may have a negative impact on the biological properties of 6-gingerol.

4. Inhibitory effect on egg white-induced foot swelling in rats

48 rats were randomly divided into 6 groups. The test drug was dissolved, suspended or emulsified into an appropriate concentration with distilled water in advance, and 10 ml of the drug solution was administered by gavage per 1 kg of animal body weight. The control group was given distilled water with the same volume, once a day, for 7 consecutive days. Before the last administration, the volume below the right hind ankle joint was measured with a small animal toe volume measuring instrument (Beijing Zhongshi Di Chuang Technology Co., Ltd.), and 10% egg white 0.9% saline solution was injected subcutaneously in the right hind foot 1 hour after administration. 0.05 ml/rat was injected to cause inflammation in the animal. The volume below the right hind ankle joint was measured by the same method at 0.5h, 1h, 2h, 4h, and 6h after inflammation, and the average toe volume of each group of animals at each time point was calculated, and the difference obtained by subtracting the average value before inflammation from the average value after inflammation was divided by the average value before inflammation and then multiplied by 100%, and the percentage was the swelling rate. The results are shown in Table 3 below.

table 3:

The dosages in the above table have similar meanings to those in Table 2. As can be seen from the results in the above table, a similar trend is shown as in the results in Table 2, that is, even when the same dose of 6-gingerol is given, the inhibitory effect of ginger oil b on egg white-induced paw swelling in rats is significantly better than that of mixed ginger oil Ex2 at various doses and time points.

5. Inhibitory effect on DNCB-induced delayed hypersensitivity reaction in mice

54 mice were randomly divided into 6 groups; the skin of about 1 square centimeter area of the abdomen was depilated, and 0.1 ml of 1% 2,4-dinitrochlorobenzene (DNCB) was evenly dripped on the depilated area of each animal to sensitize the animals; animals were given oral administration on the day of sensitization, and the test drug was dissolved, suspended or emulsified in distilled water to an appropriate concentration in advance, and 20 ml of the drug solution was administered by oral administration per 1 kg of animal body weight. The control group was given distilled water with the same volume, once a day for 7 consecutive days; 30 minutes after the last administration, 0.1 ml of 1% DNCB was applied to the front and back sides of each mouse's right ear, and the mice were killed by cervical dislocation 24 hours later, and both ears were cut off, and round ear pieces were punched at the same position with a 12mm puncher, and weighed with an electronic balance. The weight difference between the left and right ear pieces of each animal was used as the swelling degree; the thymus and spleen were removed, weighed, and the thymus index and spleen index were calculated. The results (x±s, n=9) are shown in Table 4 below.

Table 4:

The dosage in the above table has similar meanings to Table 2. As can be seen from the results in the above table, a similar trend is shown as in Table 2, that is, even when the same dose of 6-gingerol is given, the inhibitory effect of ginger oil b on DNCB-induced mouse ear swelling, DNCB-induced delayed hypersensitivity mice thymus and spleen index at various doses is significantly better than that of mixed ginger oil Ex2, and ginger oil b of the present invention can significantly reduce DNCB-induced mouse ear swelling, and significantly reduce the thymus and spleen index of DNCB-induced delayed hypersensitivity mice. From the above preparation of mixed ginger oil Ex2, its essence is a mixture of all ginger oils extracted by supercritical carbon dioxide, and ginger oil b is essentially a special part of the above-mentioned mixed ginger oil Ex2, which is obtained by the construction method of the second separation tank in Examples 2 to 4 of the present invention. It has been found that the construction method of the second separation tank and the physical and chemical properties and biological properties of the ginger oil b obtained therefrom are not foreseeable at all in the prior art.

The present invention illustrates the detailed method of the present invention through the above-mentioned embodiments, but the present invention is not limited to the above-mentioned detailed method, that is, it does not mean that the present invention must rely on the above-mentioned detailed method to be implemented. Those skilled in the art should understand that any improvement of the present invention, equivalent replacement of various raw materials of the product of the present invention, addition of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

Claims (11)

1. The ginger oil comprises 550-650 mg/g of 6-gingerol, 55-65 mg/g of 8-gingerol and 35-45 mg/g of 10-gingerol, wherein the relative density of the ginger oil at 20 ℃ is within the range of 0.941+/-0.01, and the refractive index is within the range of 1.438+/-0.02; the ginger oil is prepared by a method comprising the following steps:

(1) The supercritical carbon dioxide extraction system comprises an extraction tank, and further comprises a first separation tank, a second separation tank and a third separation tank which are sequentially connected in series according to the flowing direction of carbon dioxide, wherein the second separation tank is filled with a plurality of glass balls with diameters of 2-10 mm, and the surfaces of the glass balls are coated with propylene glycol-acetic acid mixed solution with the volume ratio of 10-15:1;

(2) Pre-filling dried ginger powder which is crushed to 20-30 meshes in a supercritical carbon dioxide extraction system into an extraction tank, regulating the temperature of gas in the tank to 32-40 ℃ after carbon dioxide enters the extraction tank, regulating the pressure to 40-50 mPa, and extracting for 2-8 hours under the supercritical conditions of the temperature and the pressure;

(3) After extraction is finished, pumping carbon dioxide in the extraction tank into a first separation tank, and regulating the temperature and the pressure in the tank to be respectively: 38+ -3 ℃, 15+ -4 mPa and maintained for 1 hour; next to this, the process is carried out,

Pumping carbon dioxide in the first separation tank into the second separation tank, and adjusting the temperature and the pressure in the tank to be respectively: 33+ -2 ℃, 8+ -1 mPa and held for 2 hours; next to this, the process is carried out,

Pumping carbon dioxide in the second separation tank into a third separation tank, and regulating the temperature and the pressure in the tank to be respectively: 29+ -2 ℃, 2+ -0.5 mPa and held for 1 hour, and then carbon dioxide is exported;

(4) Discharging the separated matter in the second separating tank, adding purified water into the second separating tank for washing, combining the separated matter and the washing liquid into a separating funnel, standing, separating liquid and discarding the water phase to obtain ginger oil.

2. The ginger oil according to claim 1, comprising 580-650 mg/g of 6-gingerol, 58-62 mg/g of 8-gingerol and 38-44 mg/g of 10-gingerol, the ginger oil having a relative density of 0.941 and a refractive index of 1.438 at 20 ℃.

3. Ginger oil according to claim 1, wherein in the supercritical carbon dioxide extraction system, the following are connected by high pressure fluid lines depending on the direction of carbon dioxide flow:

a carbon dioxide reservoir for providing a source of carbon dioxide;

a gas storage tank for temporarily storing a carbon dioxide gas source from a carbon dioxide gas storage tank and optionally a carbon dioxide recovery gas from a system recovery;

The high-pressure pumps are arranged on a high-pressure fluid pipeline between devices downstream of the gas storage groove, and each high-pressure pump is used for transmitting and adjusting the pressure of carbon dioxide to the next device;

a heat exchanger for regulating the temperature of the pressurized carbon dioxide gas to a level required for the extraction process;

an extraction tank for extracting the material fed therein with supercritical carbon dioxide;

The separation tank comprises a first separation tank, a second separation tank and a third separation tank which are sequentially connected in series according to the flowing direction of carbon dioxide, wherein a discharge valve is arranged at the bottom of the separation tank, a plurality of glass balls with the diameter of 2-10 mm are filled in the second separation tank, a high-pressure fluid pipeline entering the second separation tank is inserted into a glass ball group, and the surfaces of the glass balls are coated with propylene glycol-acetic acid mixed liquid with the volume ratio of 10-15:1;

A flow meter installed downstream of the third separation tank for measuring a flow rate of carbon dioxide discharged from the third separation tank;

A condenser installed downstream of the flowmeter for cooling and recovering the extracted carbon dioxide into the gas storage tank;

The high pressure fluid line is a straight tube or a flexible tube, which is capable of withstanding pressures up to 100 mPa.

4. Ginger oil according to claim 1, wherein after the glass balls are filled into the second separation tank, adding the propylene glycol-acetic acid mixture into the tank to soak the glass balls, and then discharging the excess mixture in the tank to make the surfaces of the glass balls be coated with the propylene glycol-acetic acid mixture.

5. Ginger oil according to claim 1, wherein the glass spheres occupy 30-90% of the inner volume of the second separator tank.

6. Ginger oil according to claim 1, wherein the material to be extracted filled in the extraction tank occupies 60-100% of the internal volume of the extraction tank.

7. Ginger oil according to claim 1, wherein the volume of the separator tank is 5% -50% of the volume of the extraction tank.

8. Ginger oil according to claim 1, the method of preparing the ginger oil comprising the steps of:

(1) A supercritical carbon dioxide extraction system is provided that connects the following devices via high pressure fluid lines depending on the direction of carbon dioxide flow:

a carbon dioxide reservoir for providing a source of carbon dioxide;

a gas storage tank for temporarily storing a carbon dioxide gas source from a carbon dioxide gas storage tank and optionally a carbon dioxide recovery gas from a system recovery;

The high-pressure pumps are arranged on a high-pressure fluid pipeline between devices downstream of the gas storage groove, and each high-pressure pump is used for transmitting and adjusting the pressure of carbon dioxide to the next device;

a heat exchanger for regulating the temperature of the pressurized carbon dioxide gas to a level required for the extraction process;

an extraction tank for extracting the material fed therein with supercritical carbon dioxide;

The separating tank comprises a first separating tank, a second separating tank and a third separating tank which are sequentially connected in series according to the flowing direction of carbon dioxide, wherein a discharge valve is arranged at the bottom of the separating tank, a plurality of glass balls with the diameter of 5mm are filled in the second separating tank, a high-pressure fluid pipeline entering the second separating tank is inserted into a glass ball group, and the surfaces of the glass balls are coated with propylene glycol-acetic acid mixed solution;

A flow meter installed downstream of the third separation tank for measuring a flow rate of carbon dioxide discharged from the third separation tank;

A condenser installed downstream of the flowmeter for cooling and recovering the extracted carbon dioxide into the gas storage tank;

Wherein,

After the glass balls are filled into the second separation tank, adding propylene glycol-acetic acid mixed solution into the tank to soak the glass balls, and then discharging redundant mixed solution in the tank to make the surfaces of the glass balls be coated with the propylene glycol-acetic acid mixed solution with the volume ratio of 12.5:1;

the glass ball group occupies 70% of the inner volume of the second separation tank;

the gas storage tank receives carbon dioxide initial gas from the carbon dioxide gas storage tank and carbon dioxide recovery gas after the extraction work is finished, and the two sources of gas are mixed in the gas storage tank and then are reused in the extraction process of the next batch;

the volume of the extraction tank is 10L, the dry ginger powder is filled in the extraction tank in advance, the temperature of the gas in the tank is regulated to 38+/-1 ℃ after carbon dioxide enters the extraction tank, the pressure is regulated to 46+/-2 mPa, and the extraction is carried out under the supercritical conditions of the temperature and the pressure;

each separator tank volume is 25% of the extraction tank volume;

(2) Pre-filling 4kg of dried ginger powder which is crushed to 20-30 meshes in an extraction tank of the supercritical carbon dioxide extraction system in the step (1), and extracting for 4 hours under the operation condition of the step (1);

(3) After extraction is finished, pumping carbon dioxide in the extraction tank into a first separation tank, and regulating the temperature and the pressure in the tank to be respectively: 38+ -1deg.C, 15+ -2mPa and held for 1 hour; next to this, the process is carried out,

Pumping carbon dioxide in the first separation tank into the second separation tank, and adjusting the temperature and the pressure in the tank to be respectively: 33+ -1 deg.C, 8+ -0.5 mPa and held for 2 hours; next to this, the process is carried out,

Pumping carbon dioxide in the second separation tank into a third separation tank, and regulating the temperature and the pressure in the tank to be respectively: 29+ -1deg.C, 2+ -0.2 mPa and maintained for 1 hr, and then carbon dioxide was led out to a flow meter, a condenser and a gas storage tank;

(4) Discharging the separated matter in the second separating tank, adding purified water into the second separating tank for washing for 3 times, 250ml each time, combining the separated matter and the washing liquid into a separating funnel, standing, separating liquid and discarding water phase to obtain ginger oil;

The high pressure fluid line is a straight tube or a flexible tube, which is capable of withstanding pressures up to 100 mPa.

9. Ginger oil according to claim 1, the method of preparing the ginger oil comprising the steps of:

(1) A supercritical carbon dioxide extraction system is provided that connects the following devices via high pressure fluid lines depending on the direction of carbon dioxide flow:

a carbon dioxide reservoir for providing a source of carbon dioxide;

a gas storage tank for temporarily storing a carbon dioxide gas source from a carbon dioxide gas storage tank and optionally a carbon dioxide recovery gas from a system recovery;

The high-pressure pumps are arranged on a high-pressure fluid pipeline between devices downstream of the gas storage groove, and each high-pressure pump is used for transmitting and adjusting the pressure of carbon dioxide to the next device;

a heat exchanger for regulating the temperature of the pressurized carbon dioxide gas to a level required for the extraction process;

an extraction tank for extracting the material fed therein with supercritical carbon dioxide;

The separating tank comprises a first separating tank, a second separating tank and a third separating tank which are sequentially connected in series according to the flowing direction of carbon dioxide, wherein a discharge valve is arranged at the bottom of the separating tank, a plurality of glass balls with the diameter of 8mm are filled in the second separating tank, a high-pressure fluid pipeline entering the second separating tank is inserted into a glass ball group, and the surfaces of the glass balls are coated with propylene glycol-acetic acid mixed solution;

A flow meter installed downstream of the third separation tank for measuring a flow rate of carbon dioxide discharged from the third separation tank;

A condenser installed downstream of the flowmeter for cooling and recovering the extracted carbon dioxide into the gas storage tank;

Wherein,

After the glass balls are filled into the second separation tank, adding propylene glycol-acetic acid mixed solution into the tank to soak the glass balls, and then discharging redundant mixed solution in the tank to make the surfaces of the glass balls be coated with the propylene glycol-acetic acid mixed solution with the volume ratio of 10:1;

the glass ball group occupies 75% of the inner volume of the second separation tank;

the gas storage tank receives carbon dioxide initial gas from the carbon dioxide gas storage tank and carbon dioxide recovery gas after the extraction work is finished, and the two sources of gas are mixed in the gas storage tank and then are reused in the extraction process of the next batch;

the volume of the extraction tank is 10L, the dry ginger powder is filled in the extraction tank in advance, the temperature of the gas in the tank is regulated to 38+/-1 ℃ after carbon dioxide enters the extraction tank, the pressure is regulated to 46+/-2 mPa, and the extraction is carried out under the supercritical conditions of the temperature and the pressure;

Each separator tank volume is 30% of the extraction tank volume;

(2) 4kg of dried ginger powder with the particle size of 20-30 meshes is pre-filled into an extraction tank of the supercritical carbon dioxide extraction system in the step (1), and extraction is carried out for 3.5 hours under the operation condition of the step (1);

(3) After extraction is finished, pumping carbon dioxide in the extraction tank into a first separation tank, and regulating the temperature and the pressure in the tank to be respectively: 38+ -1deg.C, 15+ -2mPa and held for 1 hour; next to this, the process is carried out,

Pumping carbon dioxide in the first separation tank into the second separation tank, and adjusting the temperature and the pressure in the tank to be respectively: 33+ -1 deg.C, 8+ -0.5 mPa and held for 2 hours; next to this, the process is carried out,

Pumping carbon dioxide in the second separation tank into a third separation tank, and regulating the temperature and the pressure in the tank to be respectively: 29+ -1deg.C, 2+ -0.2 mPa and maintained for 1 hr, and then carbon dioxide was led out to a flow meter, a condenser and a gas storage tank;

(4) Discharging the separated matter in the second separating tank, adding purified water into the second separating tank for washing for 3 times, 250ml each time, combining the separated matter and the washing liquid into a separating funnel, standing, separating liquid and discarding water phase to obtain ginger oil;

The high pressure fluid line is a straight tube or a flexible tube, which is capable of withstanding pressures up to 100 mPa.

10. Ginger oil according to claim 1, the method of preparing the ginger oil comprising the steps of:

(1) A supercritical carbon dioxide extraction system is provided that connects the following devices via high pressure fluid lines depending on the direction of carbon dioxide flow:

a carbon dioxide reservoir for providing a source of carbon dioxide;

a gas storage tank for temporarily storing a carbon dioxide gas source from a carbon dioxide gas storage tank and optionally a carbon dioxide recovery gas from a system recovery;

The high-pressure pumps are arranged on a high-pressure fluid pipeline between devices downstream of the gas storage groove, and each high-pressure pump is used for transmitting and adjusting the pressure of carbon dioxide to the next device;

a heat exchanger for regulating the temperature of the pressurized carbon dioxide gas to a level required for the extraction process;

an extraction tank for extracting the material fed therein with supercritical carbon dioxide;

The separating tank comprises a first separating tank, a second separating tank and a third separating tank which are sequentially connected in series according to the flowing direction of carbon dioxide, wherein a discharge valve is arranged at the bottom of the separating tank, a plurality of glass balls with the diameter of 3mm are filled in the second separating tank, a high-pressure fluid pipeline entering the second separating tank is inserted into a glass ball group, and the surfaces of the glass balls are coated with propylene glycol-acetic acid mixed solution;

A flow meter installed downstream of the third separation tank for measuring a flow rate of carbon dioxide discharged from the third separation tank;

A condenser installed downstream of the flowmeter for cooling and recovering the extracted carbon dioxide into the gas storage tank;

Wherein,

After the glass balls are filled into the second separation tank, adding propylene glycol-acetic acid mixed solution into the tank to soak the glass balls, and then discharging redundant mixed solution in the tank to make the surfaces of the glass balls be coated with the propylene glycol-acetic acid mixed solution with the volume ratio of 15:1;

The glass ball group occupies 65% of the inner volume of the second separation tank;

the gas storage tank receives carbon dioxide initial gas from the carbon dioxide gas storage tank and carbon dioxide recovery gas after the extraction work is finished, and the two sources of gas are mixed in the gas storage tank and then are reused in the extraction process of the next batch;

the volume of the extraction tank is 10L, the dry ginger powder is filled in the extraction tank in advance, the temperature of the gas in the tank is regulated to 38+/-1 ℃ after carbon dioxide enters the extraction tank, the pressure is regulated to 46+/-2 mPa, and the extraction is carried out under the supercritical conditions of the temperature and the pressure;

each separator tank volume is 20% of the extraction tank volume;

(2) Pre-filling 4kg of dried ginger powder which is crushed to 20-30 meshes in an extraction tank of the supercritical carbon dioxide extraction system in the step (1), and extracting for 5 hours under the operation condition of the step (1);

(3) After extraction is finished, pumping carbon dioxide in the extraction tank into a first separation tank, and regulating the temperature and the pressure in the tank to be respectively: 38+ -1deg.C, 15+ -2mPa and held for 1 hour; next to this, the process is carried out,

Pumping carbon dioxide in the first separation tank into the second separation tank, and adjusting the temperature and the pressure in the tank to be respectively: 33+ -1 deg.C, 8+ -0.5 mPa and held for 2 hours; next to this, the process is carried out,

Pumping carbon dioxide in the second separation tank into a third separation tank, and regulating the temperature and the pressure in the tank to be respectively: 29+ -1deg.C, 2+ -0.2 mPa and maintained for 1 hr, and then carbon dioxide was led out to a flow meter, a condenser and a gas storage tank;

(4) Discharging the separated matter in the second separating tank, adding purified water into the second separating tank for washing for 3 times, 250ml each time, combining the separated matter and the washing liquid into a separating funnel, standing, separating liquid and discarding water phase to obtain ginger oil;

The high pressure fluid line is a straight tube or a flexible tube, which is capable of withstanding pressures up to 100 mPa.

11. Use of the ginger oil according to any one of claims 1 to 10 in the preparation of a medicament for inhibiting inflammation.