CN114657023A

CN114657023A - Extraction method and application of juniper essential oil

Info

Publication number: CN114657023A
Application number: CN202111052237.0A
Authority: CN
Inventors: 朱小龙; 韦世松
Original assignee: Guangzhou Dongzhimeng Cosmetics Co ltd
Current assignee: Guangzhou Dongzhimeng Cosmetics Co ltd
Priority date: 2021-09-08
Filing date: 2021-09-08
Publication date: 2022-06-24

Abstract

The invention provides a method for extracting cypress essential oil, which comprises the following steps: crushing Chinese juniper wood; distilling with water vapor, condensing, separating, and collecting organic phase to obtain crude oil; separating the crude oil by normal phase silica gel column chromatography, eluting the eluent by ethyl acetate and petroleum ether according to the content of 0-100% ethyl acetate, wherein the mass ratio of the crude oil to the silica gel is 1: 7-1: 12; collecting the components within 2-95%, collecting the components capable of developing color by potassium permanganate, testing the boiling point of each component, and mixing and concentrating the components below 300 deg.C to obtain the essential oil of Chinese juniper. The extraction method of the cypress essential oil adopts column chromatography separation and potassium permanganate for color development, the silica gel can completely adsorb and remove the large-polarity impurities and pigment impurities, the price of the silica gel is very low, the cost is greatly reduced compared with rectification, and the purity is also ensured due to the screening of the potassium permanganate and the boiling point. Therefore, the method for extracting the cypress essential oil has the characteristics of low cost and high quality.

Description

Extraction method and application of juniper essential oil

Technical Field

The invention belongs to the field of medicine extraction, and particularly relates to a method for extracting cypress essential oil and application thereof.

Background

The cypress essential oil has higher added value, stable price and continuous high trend. Most of the existing methods for extracting the juniper essential oil adopt a steam distillation method, the extracted essential oil has complex components, more impurities and poor texture, and if further purification is needed, the distillation treatment with higher temperature is also involved. The quality of the cypress essential oil is directly influenced by the amount of the active ingredients.

And the rectification is energy-consuming and has higher cost.

Therefore, it is necessary to find a method for extracting the essential oil of juniper wood which can retain the active ingredients as much as possible.

Disclosure of Invention

The invention aims to provide a cypress essential oil and an extraction method thereof, and aims to solve the technical problems that the existing cypress essential oil extraction method is insufficient in retention of active substances and low in cost.

In order to solve the technical problem, the invention provides a method for extracting cypress essential oil, which comprises the following steps:

crushing Chinese juniper wood;

distilling with water vapor, condensing, separating, and collecting organic phase to obtain crude oil;

separating the crude oil by normal phase silica gel column chromatography, eluting the eluent by ethyl acetate and petroleum ether according to the content of 0-100% ethyl acetate, wherein the mass ratio of the crude oil to the silica gel is 1: 7-1: 12;

collecting the components within 2-95%, collecting the components capable of developing color by potassium permanganate, testing the boiling point of each component, and mixing and concentrating the components below 300 deg.C to obtain the essential oil of Chinese juniper.

Preferably, the temperature of the steam distillation is 100-110 ℃.

Preferably, a low-frequency pulse molecular refining operation is further included between the water vapor distillation and the condensation operation.

Preferably, the silica gel is 200-300 mesh silica gel.

Preferably, the mass ratio of the crude oil to the silica gel is 1: 9.

preferably, the pulverization treatment is to pulverize the cypress into powder with a particle size of less than 1 mm.

In another aspect, the invention provides the cypress essential oil extracted by the cypress essential oil extraction method.

The invention further provides a whitening and freckle-removing composition which comprises the cypress essential oil extracted by the cypress essential oil extraction method, ascorbyl tetraisopalmitate, phenethyl resorcinol and bisabolol.

Preferably, the whitening and freckle-removing composition further comprises one or more of a humectant, a skin feel regulator, a preservative, an emulsifier and deionized water;

preferably, the whitening and freckle-removing composition comprises 0.3-0.6% of the cypress essential oil, 0.2-1% of ascorbyl tetraisopalmitate, 0.1-0.3% of the phenethyl resorcinol and 0.2-0.6% of the bisabolol by mass.

Compared with the prior art, the method for extracting the cypress essential oil has the advantages that steam distillation is adopted for primary extraction, the cost is low, the extraction is sufficient, the extracted essential oil is mixed, and as the active ingredients of the cypress essential oil mainly comprise beta-cedrene, thujopside, longifolene, cedrol, flavonoids and tannin, the steam distillation cannot avoid bringing some large-polarity impurities, and the large-polarity impurities need to be further rectified for removal. The extraction method of the cypress essential oil adopts column chromatography separation subsequently, potassium permanganate develops color, and all active substances can be traced. And the silica gel can adsorb and remove all the large-polarity impurities and pigment impurities, and in addition, the silica gel has very low price, compared with rectification, the cost is greatly reduced, and the purity is also ensured due to the screening of potassium permanganate and the boiling point. Therefore, the method for extracting the cypress essential oil has the characteristics of low cost and high quality.

The cypress essential oil has the characteristics of high purity, high abundance of active ingredients and low cost due to the adoption of the extraction method of the cypress essential oil. Better efficacy can be obtained at lower cost in application.

The whitening and freckle-removing composition disclosed by the invention adopts active skin-care and whitening components such as ascorbyl tetraisopalmitate, phenethyl resorcinol and bisabolol to form a basic effect, and in addition, the cypress essential oil is added, and the cypress essential oil contains a large amount of beta-cedrene, thujoram, longifolene, cedrol, flavonoid compounds and tannin, and the components can resist free radicals, so that the whitening and freckle-removing composition has the functions of resisting oxidation and ageing. In addition, cedarwood brain, such as active alcohol, flavonoid compounds and tannin, also have certain biological activity, can lubricate skin, activate the functions of muscle base inflammation diminishing and bacteria resisting, and further has the functions of whitening and protecting skin. Finally, the Chinese juniper essential oil extracted by the extraction method provided by the invention is high in purity and abundance of active ingredients, and the whitening and freckle-removing composition is better in effect and smaller in side effect after price adjustment. The Chinese juniper essential oil also has the functions of eliminating insomnia, headache and anxiety, benefiting respiratory organs and lung function, promoting blood circulation and heart activity, relieving hypertension, preventing angiosclerosis, promoting metabolism of whole body cells, activating collaterals, and regulating whole body, and has effects of whitening and caring skin.

Drawings

Fig. 1 is a flow chart of the method for extracting the cypress essential oil according to the embodiment of the invention.

Detailed Description

In order that the invention may be more readily understood, reference will now be made to the following more particular description of the invention, examples of which are set forth below. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. These embodiments are provided so that this disclosure will be thorough and complete. The various starting materials used in the examples are, unless otherwise indicated, conventional commercial products.

Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.

The numerical values set forth in the examples of the present invention are approximations, not necessarily values. All values within the error range may be included without limiting to the specific values disclosed in the embodiments of the present invention, where the error or experimental conditions allow.

The numerical ranges disclosed in the examples of the present invention are intended to indicate the relative amounts of the components in the mixture and the ranges of temperatures or other parameters recited in the other method examples.

The embodiment of the invention provides a method for extracting cypress essential oil, which comprises the following steps:

s101: crushing Chinese juniper wood;

s102: distilling with water vapor, condensing, separating, and collecting organic phase to obtain crude oil;

s103: separating the crude oil by normal phase silica gel column chromatography, eluting the eluent by ethyl acetate and petroleum ether according to the content of 0-100% ethyl acetate, wherein the mass ratio of the crude oil to the silica gel is 1: 7-1: 12;

s104: collecting the components within 2-95%, collecting the components capable of developing color by potassium permanganate, testing the boiling point of each component, and mixing and concentrating the components below 300 deg.C to obtain the essential oil of Chinese juniper.

Preferably, the pulverizing process in the step S101 is to pulverize sabina chinensis into powder having a particle size of less than 1 mm. The content of active ingredients in the cypress is low, and the wood structure of the cypress is compact, so that the extraction efficiency can be high only by pulverizing the powder more carefully.

Preferably, in the step S102, the temperature of the steam distillation is 100-110 ℃. The extraction can be carried out in a milder way by adopting the boiling point of water and the temperature slightly higher than the boiling point, and the extraction is thorough by adopting a separation type extraction means generally. In a further preferred embodiment, a low-frequency pulse molecular refining operation is also included between the water vapor distillation and condensation operations. The low-frequency pulse molecular refining operation can mix and emulsify water and oil components in advance, part of impurities can be removed by water washing, and the residual oil phase can be primarily purified.

Preferably, in the step S103, the silica gel is 200-300 mesh silica gel, and the silica gel with this mesh is selected because the oily compound is more easily eluted, so that a larger mesh is selected instead of 100-200 mesh silica gel, and some flavonoid tannin compounds have a larger polarity and contain hydroxyl groups, and are easily adsorbed by the silica gel, and the large mesh easily wastes the solvent, so that the mesh range is selected.

Preferably, in step S103, the mass ratio of the crude oil to the silica gel is 1: 9. since some active ingredients are liquid due to their low boiling point, a larger proportion of silica gel is required to prevent the active ingredients from falling down too quickly, thereby improving the purity of the juniper essential oil. But not too much silica gel, which causes unnecessary waste and material loss caused by silica gel adsorption.

According to the extraction method of the cypress essential oil, firstly, water vapor distillation is adopted, the cost is low, the extraction effect is good, the subsequent silica gel column separation is adopted to assist the color development of potassium permanganate, the cost can be well reduced on the basis of ensuring the purity, and compared with rectification, the low-temperature purification of the column chromatography means can retain most of active ingredients which are easy to oxidize and degrade, and only a small sample is needed to test the boiling point, so that the technical effect same as that of rectification can be achieved. Therefore, the abundance of the active ingredients can be finally improved, and the quality of the cypress essential oil is greatly improved.

In another aspect, the present invention provides the cypress essential oil extracted by the cypress essential oil extraction method. Due to the adoption of the extraction method of the cypress essential oil, the cypress essential oil disclosed by the embodiment of the invention has the advantages of high active component porosity, high purity, good quality and low cost.

The embodiment of the invention also provides a whitening and freckle-removing composition, which comprises the Chinese juniper essential oil extracted by the Chinese juniper essential oil extraction method, ascorbyl tetraisopalmitate, phenethyl resorcinol and bisabolol.

In a preferred embodiment, the whitening and freckle-removing composition further comprises one or more of a moisturizing agent, a skin feeling regulator, a preservative, an emulsifier and deionized water;

further in a preferred embodiment the moisturizer comprises at least one of panthenol, 1, 3-butylene glycol, glycerin, butylene glycol, 1, 3-propylene glycol, betaine, dipropylene glycol, glyceryl polyether-26, erythritol, methyl propylene glycol, hydroxyethyl urea, sodium polyglutamate, panthenol, fructan, trehalose poly, ethylene glycol, xylitol, sorbitol, pyrrolidone carboxylic acid, sodium lactate, urea, methyl glucose polyether, chitin derivatives, trehalose, tremella polysaccharides, sodium hyaluronate, panthenol, ceramide; further, the mass fraction of the moisturizer of the present invention is in the range of 0.1 to 30% from the viewpoint of moisturizing effect and cost.

In a preferred embodiment, the skin feel modifier comprises at least one of dextran, polymethyl methacrylate, polyethylene, ethylene/acrylic acid copolymer, silicone, composite material microspheres, silicon dioxide, oat flour, nylon-12, biosugar gum and aqueous polyurethane. Furthermore, the mass fraction of the skin feel regulator in the formula of the invention is 0.1-20%.

In a preferred embodiment the preservative comprises at least one of chlorphenesin, methyl ester, phenoxyethanol, methylparaben, propylparaben, chlorphenesin, ethylhexylglycerol, hexamidine dihydrochloride, benzyl alcohol, p-hydroxyacetophenone, sorbic acid/potassium sorbate, phenoxyethanol, parabens, polyols, chlorphenesin, glyceryl caprylate, glyceryl caprate, sodium diacetate, calcium propionate, sodium lactate, polylysine, diethylhexyl syringylidenemalonate, dehydroacetic acid and its salts, salicylic acid/sodium salicylate, benzoic acid, iodopropynyl butylcarbamate, sorbitan caprylate, anisic acid. Furthermore, the mass fraction of the preservative in the formula is 0.1-20%.

In a preferred embodiment, the whitening and freckle-removing composition comprises 0.3-0.6% of the cypress essential oil, 0.2-1% of ascorbyl tetraisopalmitate, 0.1-0.3% of the phenethyl resorcinol and 0.2-0.6% of the bisabolol. The content of the active ingredients is tested by biological activity and experience, and the range is selected, so that the activity is ensured, and simultaneously, no waste or side effect is generated.

On one hand, the whitening and freckle-removing composition adopts ascorbyl tetraisopalmitate and phenethyl resorcinol L-tyrosine as substrates, and inhibits the generation of melanin by inhibiting the activity of tyrosinase; the bisabolol is an active ingredient extracted from chamomile flowers, has extremely strong anti-inflammatory effect and antibacterial activity, and can relieve the phenomenon of pigmentation caused by inflammation in the formula of the invention; the source of melanogenesis of the melanine can be blocked, the self-healing force can be improved, and the melanine can be matched with various types of whitening products for use, so that the whitening effect can be improved; the cypress essential oil mainly contains beta-cedrene, thujopside, longifolene, cedrol, flavonoid compounds and tannin. Beta-cedrene, thujolene, longifolene and cedrol contain unsaturated bonds, so that free radicals can be eliminated, and the cedrol is resistant to oxidation. The flavonoids and tannins can be oxidized into quinone because of phenolic hydroxyl groups, and have the function of eliminating active oxygen. The ketone compound and tannin also have certain functions of sterilization and anti-inflammation, and can cooperate with the bisabolol to relieve the pigmentation phenomenon caused by inflammation. Therefore, the combined use can obtain good whitening effect. In addition, the skin-whitening and skin-protecting tea also has the functions of eliminating insomnia, headache and anxiety, benefiting the functions of respiratory organs and lungs, improving blood circulation and heart activity, relieving hypertension, preventing angiosclerosis, promoting the metabolism and activating collaterals of cells of the whole body and achieving the effects of whitening and protecting skin from the aspect of regulating the whole body.

The following embodiments are further described

Example 1

Crushing Chinese juniper wood to be less than 1 mm;

distilling with water vapor, condensing, refining low-frequency pulse molecules, separating liquid, and taking an organic phase to obtain crude oil;

separating the crude oil obtained by normal phase silica gel column chromatography, eluting the eluent by adopting ethyl acetate and petroleum ether according to the content of 0-100% ethyl acetate, and selecting 200-mesh and 300-mesh silica gel, wherein the mass ratio of the crude oil to the silica gel is 1: 9;

Example 2

Crushing Chinese juniper wood to less than 1 mm;

separating the crude oil obtained by normal phase silica gel column chromatography, eluting the crude oil by ethyl acetate and petroleum ether according to the content of 0-100% ethyl acetate, and selecting 300-400-mesh silica gel, wherein the mass ratio of the crude oil to the silica gel is 1: 7;

Example 3

Crushing Chinese juniper wood to less than 1 mm;

separating the crude oil by normal phase silica gel column chromatography, eluting the eluent by adopting ethyl acetate and petroleum ether according to the content of 0-100 percent ethyl acetate, and selecting 100-200-mesh silica gel, wherein the mass ratio of the crude oil to the silica gel is 1: 12;

The extraction amounts for the respective examples were measured as shown in table 1:

TABLE 1

	Silica gel mesh number	Mass multiple of silica gel	Temperature of extraction steam distillation/. degree.C	Color developing agent	Extracting relative amount
						Example 1	200-300	7	105	Potassium permanganate	1
Example 2	300-400	9	110	Potassium permanganate	0.88
						Example 3	100-200	12	130	Potassium permanganate	0.77

By comparing the contents obtained at the end, it was found that example 1 is the best and extracts more active ingredients, being the best example.

The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, and all equivalent structural changes made by using the content of the present specification or other related technical fields within the spirit of the present invention are included in the scope of the present invention.

The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.

The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. The extraction method of the cypress essential oil is characterized by comprising the following steps:

crushing Chinese juniper wood powder;

2. The method for extracting hinoki essential oil of claim 1, wherein the temperature of the steam distillation is 100-110 ℃.

3. The method for extracting essential oil of juniper chinensis as claimed in claim 1, further comprising a low frequency pulse molecular refining operation between the steam distillation and the condensation operation.

4. The method for extracting hinoki essential oil as claimed in claim 1, wherein the silica gel is 200-300 mesh silica gel.

5. The method for extracting hinoki essential oil according to claim 1, wherein the mass ratio of the crude oil to the silica gel is 1: 9.

6. the method for extracting essential oil of juniper wood according to claim 1, wherein the pulverization is carried out by pulverizing juniper wood into powder having a particle size of less than 1 mm.

7. A cypress essential oil extracted by the cypress essential oil extraction method of claims 1-6.

8. A whitening and freckle-removing composition, which is characterized by comprising the cypress essential oil extracted by the cypress essential oil extraction method of claim 7, ascorbyl tetraisopalmitate, phenethyl resorcinol and bisabolol.

9. The whitening spot-removing composition of claim 8, further comprising one or more of a humectant, a skin feel modifier, a preservative, an emulsifier, and deionized water;

the humectant comprises at least one of panthenol, 1, 3-butanediol, glycerol, butanediol, 1, 3-propylene glycol, betaine, dipropylene glycol, glyceryl polyether-26, erythritol, methyl propylene glycol, hydroxyethyl urea, sodium polyglutamate, panthenol, levan and trehalose;

the antiseptic comprises at least one of chlorphenesin, methyl ester, phenoxyethanol, methylparaben, propylparaben, chlorphenesin, ethylhexyl glycerol, hexamidine dihydrochloride and benzyl alcohol.

10. The whitening spot-removing composition of claim 8, wherein the composition comprises 0.3 to 0.6 mass% of cypress essential oil, 0.2 to 1 mass% of ascorbyl tetraisopalmitate, 0.1 to 0.3 mass% of phenethylresorcinol, and 0.2 to 0.6 mass% of bisabolol.