CN114642713A - High-permeability compound agilawood essential oil and preparation method thereof - Google Patents
High-permeability compound agilawood essential oil and preparation method thereof Download PDFInfo
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- CN114642713A CN114642713A CN202210322628.8A CN202210322628A CN114642713A CN 114642713 A CN114642713 A CN 114642713A CN 202210322628 A CN202210322628 A CN 202210322628A CN 114642713 A CN114642713 A CN 114642713A
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- essential oil
- agilawood
- oil
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Abstract
The invention provides high-permeability compound agilawood essential oil and a preparation method thereof, wherein the high-permeability compound agilawood essential oil comprises the following raw materials in percentage by weight: 0.3-3% of agilawood essential oil, 1-3% of bay leaf essential oil, 1.5-3% of eucalyptus camphor and romantic nutgrass leaf essential oil, 1.5-4% of mint essential oil, 1-3% of eucalyptus leaf essential oil, 0.7-2% of cardamom essential oil, 2-4% of lemon essential oil, 2-4% of roman chamomile essential oil, 1-3% of tea tree essential oil and 75-85% of fractionated coconut oil; the invention compounds natural plant essential oil, adjusts the formula, has scientific proportion and adopts a specific mixing process, solves the problems that various essential oils are easy to generate flocculent suspended matters and layering is caused by different specific gravities after blending, and achieves high penetration, high absorption, high volatilization and high metabolism effect.
Description
Technical Field
The invention relates to the field of essential oil extraction, and in particular relates to high-permeability compound agilawood essential oil and a preparation method thereof.
Background
Aquilaria sinensis is wood containing resin of Aquilaria sinensis of Thymelaeaceae, and is a very rare spice and Chinese medicinal material in ancient and modern times. Although aloeswood is widely distributed in Guangdong, Hainan, Guangxi, Fujian and the like since a long time ago, wild aloeswood is almost cut down in the last thirty years, so that the resource of the aquilaria wood in China needs to be protected urgently, and the severe situation reaches a state of inequality. In all the applications of the agilawood, the agilawood essential oil is an application form with the highest scientific and technological content and application value of agilawood tree resources.
The essential oil is composed of a plurality of very small molecules, and the high volatile substances can be absorbed by nasal mucosa tissues to enter the body, so that messages are directly sent to the brain, and the emotion and the physiological function of the body are regulated through the peripheral system of the brain. Therefore, in the aromatherapy, the essential oil can strengthen the physiological and psychological functions, well regulate the skin function, nourish skin cells, repair damaged skin, and has the positive effects of calming the nerves, relieving and the like, and certain components in the essential oil also have the function of regulating the internal secretion of a human body.
The compound essential oil is prepared by blending various plant essential oils according to different properties, and is mainly used for improving the potential focus of human body and the like. According to the specific symptoms of human body, the expected effect can be achieved by making certain compound matching with proper single-component essential oil, base oil and dosage control. Compounding the agilawood essential oil with other essential oil can achieve the purpose of simultaneously using agilawood for the maintenance of a respiratory system, a skin system and a muscle system, but compounding of the agilawood essential oil with other essential oil is unstable, easy to delaminate and poor in stability, and effective components of the agilawood essential oil cannot be effectively utilized.
Disclosure of Invention
Therefore, the invention provides high-permeability compound agilawood essential oil and a preparation method thereof, and aims to solve the problems.
The technical scheme of the invention is realized as follows: a high-permeability compound agilawood essential oil comprises the following raw materials in percentage by weight: 0.3-3% of agilawood essential oil, 1-3% of bay leaf essential oil, 1.5-3% of eucalyptus camphor and romantic nutgrass leaf essential oil, 1.5-4% of mint essential oil, 1-3% of eucalyptus leaf essential oil, 0.7-2% of cardamom essential oil, 2-4% of lemon essential oil, 2-4% of roman chamomile essential oil, 1-3% of tea tree essential oil and 75-85% of fractionated coconut oil.
Further, the high-permeability compound agilawood essential oil comprises the following raw materials in percentage by weight: 1.6% of agilawood essential oil, 2% of bay leaf essential oil, 2% of eucalyptus camphor and romantic nutgrass leaf essential oil, 3% of mint essential oil, 2% of eucalyptus leaf essential oil, 1.4% of cardamom essential oil, 3% of lemon essential oil, 3% of roman chamomile essential oil, 2% of tea tree essential oil and 80% of fractionated coconut oil.
Further, a preparation method of the high-permeability compound agilawood essential oil comprises the following steps:
s1, preparing agilawood essential oil: crushing roots, stems and branches of agilawood into agilawood powder with the average particle size of 50-80 meshes, adding absolute ethyl alcohol, mixing, performing ultrasonic treatment, collecting oily matters, adding cellulase with the enzyme activity of 2000-4000U/g into the oily matters, and performing enzyme hydrolysis, wherein the volume ratio of the oily matters to the cellulase is 1: 3-5, performing enzyme inactivation treatment after enzymolysis is finished to obtain an enzymolysis product, performing suction filtration, extracting the obtained filtrate I with absolute ethyl alcohol, wherein the volume ratio of the filtrate I to the absolute ethyl alcohol is 2-6: 10, the extraction temperature is 120-150 ℃, the extraction time is 3-8 hours, taking an organic phase, performing suction filtration again, distilling the obtained filtrate II to remove ethanol, the distillation temperature is 90-120 ℃, and the pressure is 0.1-10 MPa, and obtaining agilawood essential oil for later use;
s2, preparation of fractionated coconut oil: cleaning coconut meat, crushing, sieving with a 70-90-mesh sieve, carrying out cold pressing to obtain crude oil and a cold pressed cake, carrying out supercritical extraction on the cold pressed cake, wherein an extracted solvent is n-butane, the mass-volume ratio g/mL of the cold pressed cake to the n-butane is 1-3: 5, obtaining an extract, carrying out fractional extraction for 70-100 min at the temperature of 40-80 ℃ and under the pressure of 0.5-1.2 MPa, and collecting a fractional liquid with the lauric acid content of 50-70%, namely fractionated coconut oil;
s3, preparing compound essential oil: mixing the agilawood essential oil with cardamom essential oil, Roman chamomile essential oil, bay leaf essential oil, eucalyptus camphor and Rovinsa leaf essential oil, mint essential oil, Eucalyptus leaf essential oil, tea tree essential oil and lemon essential oil respectively in sequence, stirring and mixing, performing primary homogenization at 24-30 ℃ for 5-10 min, heating to 40-60 ℃ for secondary homogenization for 20-30 min, continuously stirring for 1-3 h after homogenization is finished, and taking out to obtain composite essential oil;
and S4, adding the compound essential oil into the fractionated coconut oil of S2, mixing for 20-30 min at the rotating speed of 100-300 rpm, and standing for 20-30 h to obtain the high-permeability compound agilawood essential oil.
Further, the mass volume g/mL ratio of the S1 agilawood powder to the absolute ethyl alcohol is 3-10: 25.
Furthermore, the ultrasonic power of S1 is 800-1200W, and the ultrasonic time is 40-80 min.
Further, the S1 is subjected to enzymatic hydrolysis at the temperature of 30-50 ℃ for 3-6 h.
Further, the temperature of the supercritical extraction in the S2 is 28-45 ℃, the pressure is 0.3-0.6 MPa, and the extraction time is 40-80 min.
Further, the temperature of the supercritical extraction in the S2 is 28-45 ℃, the pressure is 0.3-0.6 MPa, and the extraction time is 40-80 min.
Furthermore, in the S3, the first homogenizing rotation speed is 1000-3000 rpm, and the second homogenizing rotation speed is 8000-12000 rpm.
Compared with the prior art, the invention has the beneficial effects that:
the invention compounds natural plant essential oil, adjusts the formula, has scientific proportion, and adopts a specific mixing process, thereby solving the problems that various essential oils are easy to generate flocculent suspended matters and layering is caused by different specific gravities after blending, and achieving the effects of high permeability, high absorption, high volatilization and high metabolism; the agilawood essential oil is prepared by adopting a specific extraction method and adjusting the extraction process, so that the obtained agilawood essential oil is high in effective component, and various essential oils have anti-inflammatory and bacteriostatic effects and can keep the skin clean and transparent for a long time. The coconut oil can keep skin moist for a long time, and has the effects of smooth circulation of capillary vessels and better inhibiting various problems caused by unsmooth blood circulation under the action of high permeability of the agilawood essential oil.
All the materials in the formula are pure plant organic raw materials, herbal essential oil compounding is carried out in a physical mode, effective substances of the essential oil are not lost, and the agilawood is simultaneously used for maintaining a respiratory system, a skin system and a muscle system.
Detailed Description
In order to better understand the technical content of the invention, specific examples are provided below to further illustrate the invention.
The experimental methods used in the examples of the present invention are all conventional methods unless otherwise specified.
The materials, reagents and the like used in the examples of the present invention can be obtained commercially without specific description.
Agilawood essential oil: the ingredients include sesquiterpene, 2- (2-phenylethyl) chromone, triterpenes, etc.; the agilawood recorded in Ben Cao gang mu has the effects of promoting the circulation of qi, regulating qi and calming the nerves. Because of fragrant smell, the pillow can purify air and soothe nerves and help sleep. Modern pharmacological research shows that the volatile oil contained in the agilawood has the effects of promoting secretion of digestive juice, anaesthetizing, relieving pain, relaxing muscles, resisting bacteria and the like.
Bay leaf essential oil: the components: 1.8 eucalyptol, alpha-vinyl acetate; has antibacterial and antifungal properties, and helps relieve asthma, trachea, and viral infection. The laurel leaf essential oil is obtained by extracting the leaves and the branches at high temperature.
Essential oil of eucalyptus camphor and romantic nutgrass: the components: 1.8-eucalyptol-sabinene alpha-terpineol, etc.; effective against virus and bacteria, can relieve respiratory discomfort, and can help to expand and strengthen respiratory system. The essential oil of eucalyptus camphor and the roxburgh rose leaves is obtained by using the roxburgh rose leaves and distilling the high temperature in a distillation kettle.
Mint essential oil: the component is menthol; has antiviral, analgesic, antipruritic, anti-irritant, antitussive, antibacterial, and choleretic effects. Peppermint leaf was used to obtain peppermint essential oil using high temperature distillation through a still.
Eucalyptus leaf essential oil: the components: eucalyptol, linalool, citronellal, camphor, anethole and terpineol; strong antibacterial power, and can relieve inflammation; promoting relaxation and improving emotion. The eucalyptus leaf essential oil is obtained by using eucalyptus leaf and distilling the eucalyptus leaf at high temperature through a distillation kettle.
Cardamom essential oil: the components: limonene, zingiberene, terpineol, eucalyptol; relieving asthma, invigorating stomach, and expelling pathogenic wind. The cardamom fruit is picked up, crushed and extracted by supercritical carbon dioxide.
Lemon essential oil: the components: limonene, citral, geranic acid, citronella oil, camphene; has effects of dispelling flatulence, promoting digestion, and clearing blood and resisting septicemia. The lemon peel is picked and extracted twice by microwave assistance.
Roman chamomile essential oil: component (b), methyl tyrosine, methacrylic acid, azulene; detoxicating, healing sore, regulating qi-flowing, invigorating stomach, dredging channels, and relieving pain. Chamomile flowers are extracted continuously and circularly by supercritical carbon dioxide fluid.
Tea tree essential oil: the components: terpineol, pinene and eucalyptol; healing sore, promoting granulation, relieving cough and asthma, relieving pain, killing virus, and invigorating body. And (3) picking the leaves and branches, performing continuous cyclic extraction by using supercritical carbon dioxide fluid, and adding ultrasonic waves for treatment in the extraction process to obtain the tea tree essential oil.
Example 1
A high-permeability compound agilawood essential oil comprises the following raw materials in percentage by weight: agilawood essential oil 0.3%, cardamom essential oil 0.7%, Roman chamomile essential oil 3%, bay leaf essential oil 2%, mint essential oil 1.5%, eucalyptus camphor-luwensha leaf essential oil 1.5%, eucalyptus leaf essential oil 2%, tea tree essential oil 1%, lemon essential oil 3%, fractionated coconut oil: 85 percent.
Example 2
A high-permeability compound agilawood essential oil comprises the following raw materials in percentage by weight: 0.5% of agilawood essential oil, 1% of cardamom essential oil, 3% of Roman chamomile essential oil, 2% of bay leaf essential oil, 1.5% of mint essential oil, 1% of eucalyptus camphor and nutgrass flatsedge leaf essential oil, 2% of Eucalyptus globulus leaf essential oil, 1% of tea tree essential oil, 3% of lemon essential oil and 85% of fractionated coconut oil.
Example 3
A high-permeability compound agilawood essential oil comprises the following raw materials in percentage by weight: 1.6% of agilawood essential oil, 2% of bay leaf essential oil, 2% of eucalyptus camphor and romantic nutgrass leaf essential oil, 3% of mint essential oil, 2% of eucalyptus leaf essential oil, 1.4% of cardamom essential oil, 3% of lemon essential oil, 3% of roman chamomile essential oil, 2% of tea tree essential oil and 80% of fractionated coconut oil;
the preparation method of the above examples 1 to 3 is as follows:
s1, preparing agilawood essential oil: the roots and the stems of the Chinese eaglewood are dried, crushing branches into agilawood powder with the average particle size of 70 meshes, adding absolute ethyl alcohol, mixing, adding cellulose with enzyme activity of 3000U/g into the oily matter for enzyme hydrolysis, wherein the mass volume g/mL ratio of the agilawood powder to the absolute ethyl alcohol is 7:25, performing ultrasonic treatment with the ultrasonic power of 1000W and the ultrasonic time of 60min, collecting the oily matter, adding the cellulose with the enzyme activity of 3000U/g into the oily matter for enzyme hydrolysis, performing enzyme hydrolysis for 5h at the enzyme hydrolysis temperature of 40 ℃, performing enzyme inactivation after the enzymatic hydrolysis is completed to obtain an enzymatic hydrolysate, performing suction filtration, extracting the obtained filtrate I with the absolute ethyl alcohol, wherein the volume ratio of the filtrate I to the absolute ethyl alcohol is 4:10, the extraction temperature is 140 ℃, the extraction time is 5h, performing suction filtration again on an organic phase, distilling the obtained filtrate II to remove the ethyl alcohol, and obtaining agilawood essential oil for later use, wherein the distillation temperature is 110 ℃, and the pressure is 5 MPa;
s2, preparation of fractionated coconut oil: cleaning coconut meat, crushing, sieving with a 80-mesh sieve, performing cold pressing to obtain crude oil and a cold pressed cake, performing supercritical extraction on the cold pressed cake at 38 ℃, under the pressure of 0.5MPa, for 60min, wherein the extracted solvent is n-butane, the mass volume ratio g/mL of the cold pressed cake to the n-butane is 2:5 to obtain an extract, performing fractional extraction at 60 ℃ and under the pressure of 0.8MPa for 85min, and collecting a fractional liquid with the lauric acid content of 60%, namely fractional coconut oil;
s3, preparing compound essential oil: mixing the above lignum Aquilariae Resinatum essential oil with fructus Amomi rotundus essential oil, Roman flos Matricariae Chamomillae essential oil, laurel leaf essential oil, Eucalyptus globulus Labill leaf essential oil, herba Menthae essential oil, Eucalyptus globulus Labill leaf essential oil, tea tree essential oil, and fructus Citri Limoniae essential oil, respectively, stirring, homogenizing at 28 deg.C and 2000rpm for 8min, heating to 50 deg.C and 10000rpm for 25min, stirring for 2h, and taking out to obtain composite essential oil;
s4, adding the compound essential oil into the fractionated coconut oil of S2, mixing for 25min at the rotation speed of 200rpm, and standing for 24h to obtain the high-permeability compound agilawood essential oil.
Example 4
A high-permeability compound agilawood essential oil comprises the following raw materials in percentage by weight: 1.6% of agilawood essential oil, 2% of bay leaf essential oil, 2% of eucalyptus camphor and romantic nutgrass leaf essential oil, 3% of mint essential oil, 2% of eucalyptus leaf essential oil, 1.4% of cardamom essential oil, 3% of lemon essential oil, 3% of roman chamomile essential oil, 2% of tea tree essential oil and 80% of fractionated coconut oil;
the preparation method comprises the following steps:
s1, preparing agilawood essential oil: crushing roots, stems and branches of agilawood into agilawood powder with an average particle size of 50 meshes, adding absolute ethyl alcohol, mixing, wherein the mass volume g/mL ratio of the agilawood powder to the absolute ethyl alcohol is 3:25, performing ultrasonic treatment, the ultrasonic power is 800W, the ultrasonic time is 40min, collecting oily matters, adding cellulase with the enzyme activity of 2000U/g into the oily matters, performing enzymatic hydrolysis, wherein the enzymatic hydrolysis temperature is 30 ℃, performing enzymatic hydrolysis for 3h, and the volume ratio of the oily matters to the cellulase is 1: 3, carrying out enzyme inactivation treatment after enzymolysis is finished to obtain an enzymolysis product, carrying out suction filtration, extracting the obtained filtrate I with absolute ethyl alcohol, wherein the volume ratio of the filtrate I to the absolute ethyl alcohol is 2:10, the extraction temperature is 120 ℃, the extraction time is 3 hours, taking an organic phase for carrying out suction filtration again, distilling the obtained filtrate II to remove the ethyl alcohol, and obtaining agilawood essential oil for later use, wherein the distillation temperature is 90 ℃, and the pressure is 0.1 MPa;
s2, preparation of fractionated coconut oil: cleaning coconut meat, crushing, sieving with a 70-mesh sieve, performing cold pressing to obtain crude oil and a cold pressed cake, performing supercritical extraction on the cold pressed cake at the temperature of 28 ℃, under the pressure of 0.3MPa, for 40min, wherein the extracted solvent is n-butane, the mass volume ratio g/mL of the cold pressed cake to the n-butane is 1:5 to obtain an extract, performing fractional extraction at the temperature of 40 ℃ and under the pressure of 0.5MPa for 70min, and collecting a fractional liquid with the lauric acid content of 50%, namely fractional coconut oil;
s3, preparing compound essential oil: mixing the above lignum Aquilariae Resinatum essential oil with fructus Amomi rotundus essential oil, Roman flos Matricariae Chamomillae essential oil, laurel leaf essential oil, Eucalyptus globulus Labill leaf essential oil, herba Menthae essential oil, Eucalyptus globulus Labill leaf essential oil, tea tree essential oil, and fructus Citri Limoniae essential oil, respectively, stirring, homogenizing at 24 deg.C and 1000rpm for 5min, heating to 40 deg.C and 8000rpm for 20min, stirring for 1h, and taking out to obtain composite essential oil;
s4, adding the compound essential oil into the fractionated coconut oil of S2, mixing for 20min at the rotation speed of 400rpm, and standing for 20h to obtain the high-permeability compound agilawood essential oil.
Example 5
A high-permeability compound agilawood essential oil comprises the following raw materials in percentage by weight: 1.6% of agilawood essential oil, 2% of bay leaf essential oil, 2% of eucalyptus camphor and romantic nutgrass leaf essential oil, 3% of mint essential oil, 2% of eucalyptus leaf essential oil, 1.4% of cardamom essential oil, 3% of lemon essential oil, 3% of roman chamomile essential oil, 2% of tea tree essential oil and 80% of fractionated coconut oil;
the preparation method comprises the following steps:
s1, preparing agilawood essential oil: the roots and the stems of the Chinese eaglewood are dried, crushing branches into agilawood powder with the average particle size of 80 meshes, adding absolute ethyl alcohol, mixing, wherein the mass volume g/mL ratio of the agilawood powder to the absolute ethyl alcohol is 10:25, performing ultrasonic treatment, the ultrasonic power is 1200W, the ultrasonic time is 80min, collecting oily matters, adding cellulase with the enzyme activity of 4000U/g into the oily matters, performing enzyme hydrolysis at the enzyme hydrolysis temperature of 50 ℃ for 6h, performing enzyme inactivation after the enzymatic hydrolysis is completed to obtain an enzymatic hydrolysate, performing suction filtration, extracting the obtained filtrate I with the absolute ethyl alcohol, wherein the volume ratio of the filtrate I to the absolute ethyl alcohol is 6:10, the extraction temperature is 150 ℃, the extraction time is 8h, performing suction filtration again on the obtained filtrate II, distilling to remove the ethyl alcohol, wherein the distillation temperature is 120 ℃, and the pressure is 10MPa, and obtaining agilawood essential oil for later use;
s2, preparation of fractionated coconut oil: cleaning coconut meat, crushing, sieving with a 90-mesh sieve, carrying out cold pressing to obtain crude oil and a cold pressed cake, carrying out supercritical extraction on the cold pressed cake, wherein the temperature of the supercritical extraction is 45 ℃, the pressure is 0.6MPa, the extraction time is 80min, the extracted solvent is n-butane, the mass-to-volume ratio g/mL of the cold pressed cake to the n-butane is 3:5, obtaining an extract, carrying out fractional extraction for 100min at the temperature of 80 ℃ and the pressure of 1.2MPa, and collecting a fractional liquid with the lauric acid content of 70%, namely the fractional coconut oil;
s3, preparing compound essential oil: mixing the above lignum Aquilariae Resinatum essential oil with fructus Amomi rotundus essential oil, Roman flos Matricariae Chamomillae essential oil, laurel leaf essential oil, Eucalyptus globulus Labill leaf essential oil, herba Menthae essential oil, Eucalyptus globulus Labill leaf essential oil, tea tree essential oil, and fructus Citri Limoniae essential oil, respectively, stirring, homogenizing at 30 deg.C and 3000rpm for 10min, heating to 60 deg.C and 12000rpm for 30min, stirring for 3h, and taking out to obtain composite essential oil;
s4, adding the compound essential oil into the fractionated coconut oil of S2, mixing for 30min at the rotation speed of 600rpm, and standing for 30h to obtain the high-permeability compound agilawood essential oil.
Comparative example 1
The difference between the comparative example and the example 3 is that the high-permeability compound agilawood essential oil comprises the following raw materials in percentage by weight: 5% of agilawood essential oil, 0.3% of laurel leaf essential oil, 1% of eucalyptus camphor and romantic nutgrass leaf essential oil, 5% of mint essential oil, 4% of eucalyptus leaf essential oil, 0.2% of cardamom essential oil, 1% of lemon essential oil, 5% of roman chamomile essential oil, 0.1% of tea tree essential oil and 78.4% of fractionated coconut oil;
the preparation method comprises the following steps:
s1, preparing agilawood essential oil: the roots and the stems of the Chinese eaglewood are dried, crushing branches into agilawood powder with the average particle size of 80 meshes, adding absolute ethyl alcohol, mixing, wherein the mass volume g/mL ratio of the agilawood powder to the absolute ethyl alcohol is 10:25, performing ultrasonic treatment, the ultrasonic power is 1200W, the ultrasonic time is 80min, collecting oily matters, adding cellulase with the enzyme activity of 4000U/g into the oily matters, performing enzyme hydrolysis at the enzyme hydrolysis temperature of 50 ℃ for 6h, performing enzyme inactivation after the enzymatic hydrolysis is completed to obtain an enzymatic hydrolysate, performing suction filtration, extracting the obtained filtrate I with the absolute ethyl alcohol, wherein the volume ratio of the filtrate I to the absolute ethyl alcohol is 6:10, the extraction temperature is 150 ℃, the extraction time is 8h, performing suction filtration again on the obtained filtrate II, distilling to remove the ethyl alcohol, wherein the distillation temperature is 120 ℃, and the pressure is 10MPa, and obtaining agilawood essential oil for later use;
s2, preparation of fractionated coconut oil: cleaning coconut meat, crushing, sieving with a 90-mesh sieve, carrying out cold pressing to obtain crude oil and a cold pressed cake, carrying out supercritical extraction on the cold pressed cake, wherein the temperature of the supercritical extraction is 45 ℃, the pressure is 0.6MPa, the extraction time is 80min, the extracted solvent is n-butane, the mass-to-volume ratio g/mL of the cold pressed cake to the n-butane is 3:5, obtaining an extract, carrying out fractional extraction for 100min at the temperature of 80 ℃ and the pressure of 1.2MPa, and collecting a fractional liquid with the lauric acid content of 70%, namely the fractional coconut oil;
s3, preparing compound essential oil: mixing the above lignum Aquilariae Resinatum essential oil with fructus Amomi rotundus essential oil, Roman flos Matricariae Chamomillae essential oil, laurel leaf essential oil, Eucalyptus globulus Labill leaf essential oil, herba Menthae essential oil, Eucalyptus globulus Labill leaf essential oil, tea tree essential oil, and fructus Citri Limoniae essential oil, respectively, stirring, homogenizing at 28 deg.C and 2000rpm for 8min, heating to 50 deg.C and 10000rpm for 25min, stirring for 2h, and taking out to obtain composite essential oil;
s4, adding the compound essential oil into the fractionated coconut oil of S2, mixing for 30min at the rotation speed of 600rpm, and standing for 30h to obtain the high-permeability compound agilawood essential oil.
Comparative example 2
The difference between the comparative example and the example 3 is that absolute ethyl alcohol ultrasonic treatment is not carried out in the process of preparing the agilawood essential oil, and the specific steps are as follows:
a high-permeability compound agilawood essential oil comprises the following raw materials in percentage by weight: 1.6% of agilawood essential oil, 2% of bay leaf essential oil, 2% of eucalyptus camphor and romantic nutgrass leaf essential oil, 3% of mint essential oil, 2% of eucalyptus leaf essential oil, 1.4% of cardamom essential oil, 3% of lemon essential oil, 3% of roman chamomile essential oil, 2% of tea tree essential oil and 80% of fractionated coconut oil;
the preparation method comprises the following steps:
s1, preparing agilawood essential oil: crushing roots, stems and branches of agilawood into agilawood powder with the average particle size of 70 meshes, adding cellulase with the enzyme activity of 3000U/g into the agilawood powder for enzyme hydrolysis at the enzyme hydrolysis temperature of 40 ℃ for 5 hours, wherein the volume ratio of the agilawood powder to the cellulase is 1:4, performing enzyme inactivation treatment after the enzyme hydrolysis is finished to obtain an enzymolysis product, performing suction filtration, extracting the obtained filtrate I with absolute ethyl alcohol at the volume ratio of 4:10, the extraction temperature of 140 ℃, the extraction time of 5 hours, taking the organic phase for suction filtration again, distilling the obtained filtrate II to remove the ethanol, and obtaining agilawood essential oil for later use, wherein the distillation temperature is 110 ℃, and the pressure is 5 MPa;
s2, preparation of fractionated coconut oil: cleaning coconut meat, crushing, sieving with a 80-mesh sieve, carrying out cold pressing to obtain crude oil and a cold pressed cake, carrying out supercritical extraction on the cold pressed cake, wherein the temperature of the supercritical extraction is 38 ℃, the pressure is 0.5MPa, the extraction time is 60min, the extracted solvent is n-butane, the mass-to-volume ratio g/mL of the cold pressed cake to the n-butane is 2:5, obtaining an extract, carrying out fractional extraction for 85min under the conditions of 60 ℃ and 0.8MPa, and collecting a fractional liquid with the lauric acid content of 60%, namely the fractional coconut oil;
s3, preparing compound essential oil: mixing the above lignum Aquilariae Resinatum essential oil with fructus Amomi rotundus essential oil, Roman flos Matricariae Chamomillae essential oil, laurel leaf essential oil, Eucalyptus globulus Labill leaf essential oil, herba Menthae essential oil, Eucalyptus globulus Labill leaf essential oil, tea tree essential oil, and fructus Citri Limoniae essential oil, respectively, stirring, homogenizing at 28 deg.C and 2000rpm for 8min, heating to 50 deg.C and 10000rpm for 25min, stirring for 2h, and taking out to obtain composite essential oil;
s4, adding the compound essential oil into the fractionated coconut oil of S2, mixing for 25min at the rotation speed of 200rpm, and standing for 24h to obtain the high-permeability compound agilawood essential oil.
Comparative example 3
The difference between the comparative example and the example 3 is that the once homogenization is used in the mixing process of the composite essential oil, the rotating speed is 10000rpm, the temperature is 50 ℃, and the concrete steps are as follows:
the high-permeability compound agilawood essential oil comprises the following raw materials in percentage by weight: 1.6% of agilawood essential oil, 2% of bay leaf essential oil, 2% of eucalyptus camphor and romantic nutgrass leaf essential oil, 3% of mint essential oil, 2% of eucalyptus leaf essential oil, 1.4% of cardamom essential oil, 3% of lemon essential oil, 3% of roman chamomile essential oil, 2% of tea tree essential oil and 80% of fractionated coconut oil;
the preparation method comprises the following steps:
s1, preparing agilawood essential oil: the roots and the stems of the Chinese eaglewood are dried, crushing branches into agilawood powder with the average particle size of 70 meshes, adding absolute ethyl alcohol, mixing, adding cellulose with enzyme activity of 3000U/g into the oily matter for enzyme hydrolysis, wherein the mass volume g/mL ratio of the agilawood powder to the absolute ethyl alcohol is 7:25, performing ultrasonic treatment with the ultrasonic power of 1000W and the ultrasonic time of 60min, collecting the oily matter, adding the cellulose with the enzyme activity of 3000U/g into the oily matter for enzyme hydrolysis, performing enzyme hydrolysis for 5h at the enzyme hydrolysis temperature of 40 ℃, performing enzyme inactivation after the enzymatic hydrolysis is completed to obtain an enzymatic hydrolysate, performing suction filtration, extracting the obtained filtrate I with the absolute ethyl alcohol, wherein the volume ratio of the filtrate I to the absolute ethyl alcohol is 4:10, the extraction temperature is 140 ℃, the extraction time is 5h, performing suction filtration again on an organic phase, distilling the obtained filtrate II to remove the ethyl alcohol, and obtaining agilawood essential oil for later use, wherein the distillation temperature is 110 ℃, and the pressure is 5 MPa;
s2, preparation of fractionated coconut oil: cleaning coconut meat, crushing, sieving with a 80-mesh sieve, carrying out cold pressing to obtain crude oil and a cold pressed cake, carrying out supercritical extraction on the cold pressed cake, wherein the temperature of the supercritical extraction is 38 ℃, the pressure is 0.5MPa, the extraction time is 60min, the extracted solvent is n-butane, the mass-to-volume ratio g/mL of the cold pressed cake to the n-butane is 2:5, obtaining an extract, carrying out fractional extraction for 85min under the conditions of 60 ℃ and 0.8MPa, and collecting a fractional liquid with the lauric acid content of 60%, namely the fractional coconut oil;
s3, preparing compound essential oil: mixing the above lignum Aquilariae Resinatum essential oil with fructus Amomi rotundus essential oil, Roman flos Matricariae Chamomillae essential oil, laurel leaf essential oil, Eucalyptus globulus Labill leaf essential oil, herba Menthae essential oil, Eucalyptus globulus Labill leaf essential oil, tea tree essential oil, and fructus Citri Limoniae essential oil, respectively, stirring, homogenizing at 50 deg.C and 10000rpm for 25min, stirring for 2h after homogenizing, and taking out to obtain compound essential oil;
s4, adding the compound essential oil into the fractionated coconut oil of S2, mixing for 25min at the rotation speed of 200rpm, and standing for 24h to obtain the high-permeability compound agilawood essential oil.
First, performance test
The compound agilawood essential oil prepared in the above examples 1-5 and comparative examples 1-3 is measured for the total oil yield, stability and permeability;
(1) the total oil yield is as follows: m1/(M2-M3)×100；
In the formula, M1Is the content of compound lignum Aquilariae Resinatum essential oil, M2Is prepared from lignum Aquilariae Resinatum, laurel leaf, folium Eucalypti Globueli Camphora leaf, herba Menthae, folium Eucalypti Globueli, fructus Amomi rotundus essential oil, fructus Citri Limoniae, Roman flos Matricariae Chamomillae,Total mass of tea plant and coconut, M3Is the mass of the impurity.
(2) Stability: dividing the prepared compound agilawood essential oil into 8 groups, measuring the number of each group for three times, firstly rotating the essential oil at 0 ℃ and 1000rpm of a centrifugal machine for 20-40 min, then rotating at 100 ℃ and 1500rpm for 10-30 min, and observing the state of the essential oil.
(3) Permeability: dipping a glass rod with the essential oil according to a one-drop permeation method by using the essential oil to form a small water drop, gently placing the water drop on standard cloth to be detected, calculating the time from dipping the cloth cover to disappearing and permeating the cloth cover, and judging the standard: less than 3s is high penetration, 3-6 s is normal penetration, and more than 6s is low penetration.
(4) And (3) testing results:
| total oil yield (%) | Stability of | Permeability of | |
| Example 1 | 0.085 | Without delamination | High permeability |
| Example 2 | 0.083 | Without delamination | High permeability |
| Example 3 | 0.089 | Without delamination | High permeability |
| Example 4 | 0.086 | Without delamination | High permeability |
| Example 5 | 0.084 | Without delamination | High permeability |
| Comparative example 1 | 0.075 | Micro layering | General penetration |
| Comparative example 2 | 0.071 | Micro layering | General penetration |
| Comparative example 3 | 0.073 | Micro layering | General penetration |
According to the results, the natural plant essential oil is compounded, the formula of the natural plant essential oil is adjusted, the proportion is scientific, and a specific mixing process is adopted, so that the problems that various essential oils are easy to generate flocculent suspended matters after being blended and are layered due to different specific gravities are solved, high permeability, high absorption, high volatilization and high metabolism are achieved, compared with the comparative example 1, the proportion has better stability and permeability, compared with the comparative example 2, the extraction process of the agilawood is adjusted, the effective oily matter is obtained by using absolute ethyl alcohol ultrasound firstly, and then the enzymatic hydrolysis and extraction are carried out, so that the oil yield of the agilawood essential oil obtained by ultrasound is higher, and the total oil yield of the integral compound essential oil is higher; compared with the comparative example 3, the stability of the essential oil is effectively improved by mixing, homogenizing twice and adjusting the parameters of the homogenizing twice.
Second, typical case
1. The IT practitioner, 25-35 years old, 15 men and 18 women, uses 2-3 times a day; the application is continued for 6 days; the using method comprises the following steps: smelling and applying; the symptoms of palpitation, chest distress, muscle and joint soreness caused by sedentary sitting, space closure and the like basically disappear.
2. Applying and massaging for people with mobility disabilities, more than 50-65 years old, 1 man and 1 woman for 2 times every day; after the continuous use for 15 days, the conditions such as muscle swelling, joint stiffness and the like are obviously reduced; it can enhance blood circulation and reduce tissue degeneration.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
1. The high-permeability compound agilawood essential oil is characterized in that: comprises the following raw materials in percentage by weight: 0.3-3% of agilawood essential oil, 1-3% of bay leaf essential oil, 1.5-3% of eucalyptus camphor and romantic nutgrass leaf essential oil, 1.5-4% of mint essential oil, 1-3% of eucalyptus leaf essential oil, 0.7-2% of cardamom essential oil, 2-4% of lemon essential oil, 2-4% of roman chamomile essential oil, 1-3% of tea tree essential oil and 75-85% of fractionated coconut oil.
2. The high-permeability compound agilawood essential oil as claimed in claim 1, wherein: comprises the following raw materials in percentage by weight: 1.6% of agilawood essential oil, 2% of bay leaf essential oil, 2% of eucalyptus camphor and romantic nutgrass leaf essential oil, 3% of mint essential oil, 2% of eucalyptus leaf essential oil, 1.4% of cardamom essential oil, 3% of lemon essential oil, 3% of roman chamomile essential oil, 2% of tea tree essential oil and 80% of fractionated coconut oil.
3. The preparation method of the high-permeability compound agilawood essential oil as claimed in claim 1 or 2, wherein the preparation method comprises the following steps: the method comprises the following steps:
s1, preparing agilawood essential oil: crushing roots, stems and branches of agilawood into agilawood powder with the average particle size of 50-80 meshes, adding absolute ethyl alcohol, mixing, performing ultrasonic treatment, collecting oily matters, adding cellulase with the enzyme activity of 2000-4000U/g into the oily matters, and performing enzyme hydrolysis, wherein the volume ratio of the oily matters to the cellulase is 1: 3-5, performing enzyme inactivation treatment after enzymolysis is finished to obtain an enzymolysis product, performing suction filtration, extracting the obtained filtrate I with absolute ethyl alcohol, wherein the volume ratio of the filtrate I to the absolute ethyl alcohol is 2-6: 10, the extraction temperature is 120-150 ℃, the extraction time is 3-8 hours, taking an organic phase, performing suction filtration again, distilling the obtained filtrate II to remove ethanol, the distillation temperature is 90-120 ℃, and the pressure is 0.1-10 MPa, and obtaining agilawood essential oil for later use;
s2, preparation of fractionated coconut oil: cleaning coconut meat, crushing, sieving with a 70-90-mesh sieve, performing cold pressing to obtain crude oil and a cold pressed cake, performing supercritical extraction on the cold pressed cake, wherein an extracted solvent is n-butane, the mass volume ratio g/mL of the cold pressed cake to the n-butane is 1-3: 5, obtaining an extract, performing fractional extraction for 70-100 min at the temperature of 40-80 ℃ and under the pressure of 0.5-1.2 MPa, and collecting a fractional liquid with the lauric acid content of 50-70%, namely fractionated coconut oil;
s3, preparing compound essential oil: mixing the agilawood essential oil with cardamom essential oil, Roman chamomile essential oil, bay leaf essential oil, eucalyptus camphor and Rovinsa leaf essential oil, mint essential oil, Eucalyptus leaf essential oil, tea tree essential oil and lemon essential oil respectively in sequence, stirring and mixing, performing primary homogenization at 24-30 ℃ for 5-10 min, heating to 40-60 ℃ for secondary homogenization for 20-30 min, continuously stirring for 1-3 h after homogenization is finished, and taking out to obtain composite essential oil;
and S4, adding the compound essential oil into the fractionated coconut oil of S2, mixing for 20-30 min at the rotating speed of 100-300 rpm, and standing for 20-30 h to obtain the high-permeability compound agilawood essential oil.
4. The preparation method of the high-permeability compound agilawood essential oil as claimed in claim 3, wherein the preparation method comprises the following steps: the mass volume g/mL ratio of the S1 agilawood powder to the absolute ethyl alcohol is 3-10: 25.
5. The preparation method of the high-permeability compound agilawood essential oil as claimed in claim 3, wherein the preparation method comprises the following steps: the ultrasonic power of the S1 is 800-1200W, and the ultrasonic time is 40-80 min.
6. The preparation method of the high-permeability compound agilawood essential oil as claimed in claim 3, wherein the preparation method comprises the following steps: and (3) carrying out enzymatic hydrolysis for 3-6 h at the S1 enzyme hydrolysis temperature of 30-50 ℃.
7. The preparation method of the high-permeability compound agilawood essential oil as claimed in claim 3, wherein the preparation method comprises the following steps: the temperature of the supercritical extraction in the S2 is 28-45 ℃, the pressure is 0.3-0.6 MPa, and the extraction time is 40-80 min.
8. The preparation method of the high-permeability compound agilawood essential oil as claimed in claim 3, wherein the preparation method comprises the following steps: in the S3, the first homogenizing rotation speed is 1000-3000 rpm, and the second homogenizing rotation speed is 8000-12000 rpm.
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| CN103923749A (en) * | 2014-04-30 | 2014-07-16 | 海口蜜香树科技有限公司 | Method for extracting Chinese eaglewood essential oil |
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| CN111481450A (en) * | 2019-01-25 | 2020-08-04 | 广东轻工职业技术学院 | Preparation of plant essential oil microcapsule and application of plant essential oil microcapsule in hair product with lasting fragrance |
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