CN108524331B - Taxus chinensis solid perfume and preparation method thereof - Google Patents
Taxus chinensis solid perfume and preparation method thereof Download PDFInfo
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
- A61K8/922—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q13/00—Formulations or additives for perfume preparations
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/56—Compounds, absorbed onto or entrapped into a solid carrier, e.g. encapsulated perfumes, inclusion compounds, sustained release forms
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Abstract
The invention discloses a preparation method of taxus chinensis solid perfume, which comprises the steps of pretreatment of raw materials, extraction of volatile oil, post-treatment of leaching liquor and preparation of microcapsule solid perfume; the invention also discloses the solid perfume obtained according to the preparation method; the invention fully utilizes the taxus chinensis resources, has simple process and lower cost, and the obtained taxus chinensis solid perfume draws the essence of concentrated taxus chinensis, has the unique faint scent of the Youyou forest of the taxus chinensis, has good slow release effect, lasting fragrance and convenient carrying; the solvent aroma-extracting petroleum ether selected by the solvent extraction method has relatively large solubility and larger diffusion degree to the active ingredients of the taxus chinensis var mairei, and the aroma-extracting petroleum ether is easy to recover and has small elution amount to unnecessary ingredients so as to facilitate the concentration and purification of volatile oil; the composite wall material of beta-cyclodextrin and maltodextrin is adopted, so that the embedding rate of the taxus chinensis microcapsules can be improved, and the effect of improving the compactness of the taxus chinensis microcapsule membrane can be achieved.
Description
Technical Field
The invention relates to the technical field of cosmetics, and particularly relates to taxus chinensis solid perfume.
Background
The invention of perfume was originally derived from the ancient demand of people for masking and improving body odor. In order to meet the requirements, people can make the mixed substances of spice buds and the like into a purse and carry the purse with the people. Due to the limited amount, the aroma over a long time pocket will escape and require re-replenishment of the aroma source. Then, people extract or synthesize the perfume to prepare a liquid product with high content of single or multiple components, and only needs to spray or coat the liquid product when in use, so as to achieve the purpose of improving the smell. Since the liquid perfume is very volatile, has a good diffusion radius, the release is also very fast, but the persistence is not sufficient. With the emergence of new inventions, various solid fragrance-releasing products such as perfume cards, mosquito repelling patches, etc. have been proposed. The perfume component is attached to the solid product to achieve the purpose of convenient carrying. However, the above method does not effectively solve the problems of too fast release and insufficient endurance. For this reason, the development of perfumes as solids and the use of slow-release substances to delay the release of the ingredients is the direction of priority. The solid perfume is a rod-shaped and granular solid perfume product prepared by dissolving or adsorbing essence in a curing agent. The product consists of essence, solvent and curing agent. Its advantages are durable fragrance and convenient carrying about.
Comparison document 1: chinese patent with application number of CN201310226251.7, named as 'preparation method of solid perfume' discloses a preparation method of solid perfume, the solid perfume prepared by the method is convenient to carry and has lasting fragrance; however, the method does not aim at specific plant components and does not relate to leaching of plant active ingredients, and the method does not relate to how to improve the embedding rate and compactness effect of specific plants because plant volatile oil cannot be effectively embedded by using one wall material alone.
Taxus chinensis is a natural rare anti-cancer plant which is recognized in the world to be endangered to extinct, is an ancient tree species which is left over from the fourth glacier, and has a history of 250 ten thousand years on the earth. The medicinal value of the taxus is mainly embodied in the extract, namely taxol. Paclitaxel is the antitumor active component separated from the bark of taxus brevifolia at the earliest, is one of the best medicaments for treating metastatic ovarian cancer and breast cancer, has obvious curative effect on lung cancer and esophageal cancer, and has obvious inhibiting effect on nephritis and parvovirus inflammation. The root, stem and leaf of Taxus chinensis can be used as medicine, has effects of relieving swelling, resolving hard mass, dredging channels and promoting urination, and can be used for treating lump and accumulation, edema, dysuria, rheumatalgia, etc. According to the abundant medicinal characteristics of the taxus chinensis, the active ingredients in the branches and leaves of the taxus chinensis are completely reserved, and the slow release particles of the taxus chinensis are rich in various micromolecule volatile ingredients, phenolic compounds and the like, have strong fragrance, calm and calm the nerves, and can play roles in improving microcirculation, purifying air and the like. The volatile micromolecules of the taxus chinensis can be combined with odor receptor cells positioned on the epithelium of the nasal mucosa after entering a respiratory system of a human body, and the odor receptor cells can generate strong signals after being activated by the taxus chinensis micromolecules, are quickly transmitted to olfactory bulbar microcells of the brain, and then are transmitted to other brain areas to be combined into a specific mode to act on the human body. According to the principle, the information of various micromolecular odor receptors volatilized by the taxus chinensis is combined into a mode corresponding to the specific odor stimulation, and the brain consciously senses the stimulation of the specific micromolecular odor, so that the nervous system is regulated, and corresponding physiological response is induced.
Comparison document 2: the invention discloses a health-care perfume product taking purified oil of taxus chinensis and taxus chinensis extract as raw materials, which is named as 'CN 201310035244.9', and discloses a health-care perfume product taking purified oil of taxus chinensis and taxus chinensis extract as raw materials. The perfume comprises the extract of the taxus chinensis, but the specific extraction of the effective components in the taxus chinensis is not mentioned. The volatile fragrant substance has the characteristics of small molecular weight and volatility, and the perfume microencapsulation can convert liquid perfume into solid powder, improve the stability of the fragrant substance and effectively control the release of the fragrant component.
Comparison document 3: the invention discloses a method for extracting a fat-soluble active component of taxus chinensis, which is a patent with the application number of 'CN 201210125062.6' and the name of 'preparation method of taxus chinensis active extract and antifungal application thereof', and the preparation method comprises the steps of 50-95% ethanol extraction, low-polarity solvent extraction, centrifugation and macroporous resin, so that the taxus chinensis active extract with the total flavonoid content of 30-90% is obtained. The invention adopts the conventional method for preparing medicines, health products and daily chemical products to prepare the active ingredients of the taxus chinensis into various preparations, such as tablets, sprays, hand sanitizer, bath lotion, foot bath agent, hair washing cream, massage cream and the like. The active ingredients of the taxus chinensis prepared by the method have obvious bacteriostatic effect. The preparation method of the active ingredients of the taxus chinensis is simple, low in production cost, high in content of active ingredients in the product, stable in quality and easy to control. The preparation method comprises the steps of extracting with 50-95% ethanol, extracting with a low-polarity solvent, and centrifuging to obtain the active extract of the taxus chinensis, but the content of total flavonoids is yet to be improved, the obtained extract is not volatile oil, and is not suitable for being used as perfume, and no relevant report is provided on how to develop the solid perfume of the taxus chinensis.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides the taxus chinensis solid perfume which fully utilizes taxus chinensis resources, has simple process and lower cost, draws the essence of concentrated taxus chinensis, has the unique faint scent of a Youyou forest of taxus chinensis, has good slow release effect and lasting fragrance and is convenient to carry.
The invention is realized by the following steps:
one of the purposes of the invention is to provide a preparation method of taxus chinensis solid perfume, which comprises the following steps:
step 1, pretreatment of raw materials: selecting fresh branches and leaves of taxus chinensis, cleaning, drying and crushing;
step 2, leaching of volatile oil: leaching pulverized branches and leaves of Taxus chinensis in petroleum ether, filtering to obtain leaching solution, and removing residue to obtain leaching solution containing volatile oil;
step 3, post-treatment of the leaching liquor: evaporating petroleum ether in the leaching liquor to obtain extract; dissolving the extract in ethanol, cooling, filtering to remove residue to obtain ethanol extractive solution, concentrating under reduced pressure, removing ethanol, and removing residue to obtain pure oil of Taxus chinensis;
step 4, preparing the microcapsule solid perfume: mixing beta-cyclodextrin, maltodextrin and water, stirring to obtain saturated solution, and primarily emulsifying to obtain water phase; and (3) adding absolute ethyl alcohol into the pure oil of the taxus chinensis obtained in the step (3) to dissolve the pure oil of the taxus chinensis to prepare an oil phase, slowly adding the oil phase into the water phase, embedding, cooling to room temperature, refrigerating, filtering and drying to obtain the solid perfume microcapsule of the taxus chinensis.
The invention also aims to provide the taxus chinensis solid perfume obtained by the preparation method of the taxus chinensis solid perfume.
The efficacy and activity of each main raw material medicine are as follows:
and (3) taxus mairei: the composition contains a large amount of alkanes, alkenes, esters and alcohol compounds, except part of alkanes which are relatively stable in property and have no toxic effect, most of the alkanes are volatile substances which are beneficial to human bodies and have faint scent, and the active ingredients enter blood circulation after being inhaled into respiratory tracts and absorbed by local skin, so that the composition can effectively relieve a nervous system, a respiratory system and a circulatory system and exert biological effects of the compositions, such as: 9-hexadecenoic acid and 9-hexadecene ester, lignans, flavonoids and phenolic compounds, etc., all have the functions of improving microcirculation, tranquilizing and allaying excitement; taxol contained in Taxus chinensis var mairei has a unique anticancer mechanism and high anticancer activity, can prevent the propagation of cancer cells and inhibit the migration of tumor cells, and is known as the most important anticancer active substance in the field of natural medicines at present; the small molecule volatile components contained in the taxus mairei, such as lignans, flavonoids and phenolic compounds, can improve microcirculation, absorb carcinogenic substances, such as formaldehyde, benzene, carbon dioxide, sulfur dioxide, carbon monoxide and other harmful substances, release a large amount of negative oxygen ions, purify air and improve air quality; the south yew has the advantages that citronellal which volatilizes odor molecules outwards can repel mosquitoes, and the higher the temperature is, the more the odor molecules volatilize, the better the mosquito repelling effect is; in addition, the taxus mairei can also secrete different alkaloids, and the alkaloids can be sterilized and disinfected and can prevent cold and cardiovascular and cerebrovascular diseases when being emitted into the air.
Compared with the prior art, the invention has the following advantages and effects:
1. the invention fully utilizes the taxus resources, has simple process and lower cost, and the obtained taxus solid perfume draws the essence of concentrated taxus, has the unique faint scent of the yoyo forest of the taxus, has good slow release effect, lasting fragrance and convenient carrying, adopts the composite wall material of beta-cyclodextrin and maltodextrin, avoids the defect that the volatile oil of the taxus cannot be effectively embedded by singly using one wall material, not only can improve the embedding rate of the taxus microcapsules, but also can achieve the effect of improving the compactness of the taxus microcapsule membrane, the fragrance is kept for more than 10 weeks under the high-temperature condition of summer, the fragrance is kept for more than 12 weeks in spring, autumn and winter, and the demand of people is fully met;
2. the solid perfume of the taxus chinensis provided by the invention can effectively inhibit escherichia coli, staphylococcus aureus and salmonella on the surfaces of air and objects, so as to achieve the effects of purifying air and sterilizing, and the MICs of the purified oil of the taxus chinensis extracted by the invention on the escherichia coli, the staphylococcus aureus and the salmonella are respectively 0.32mg/mL, 0.08mg/mL and 0.64 mg/mL;
3. the solvent aroma-extracting petroleum ether selected by the solvent extraction method has good selectivity and lower viscosity on the effective components, the good selectivity enables the effective components of the taxus chinensis to have relatively large solubility, the lower viscosity enables the taxus chinensis to have larger diffusion degree, the aroma-extracting petroleum ether is easy to recover, and the dissolving amount of unnecessary components such as pectin, pigment and the like is small, so that the volatile oil can be concentrated and purified; meanwhile, the selected solvent for extracting the fragrant petroleum ether is low in price and toxicity;
4. in the process of extracting the taxus chinensis var mairei, the extraction rate of the pure oil of the taxus chinensis is up to 5 percent, the invention creatively provides the optimal extraction time, the proper solid-to-liquid ratio of the taxus chinensis branches and leaves to the aroma-extracting petroleum ether, the extraction temperature:
(1) the length of leaching time is also an important factor. The leaching time is too short, the volatile oil cannot be leached completely, the leaching effect is poor, and even the volatile oil cannot be leached out; the optimal leaching times obtained by repeatedly searching are twice, the first time is 2-4h, the second time is 1-3h, and the leaching liquor is combined and concentrated after filtering to obtain a product;
(2) in the extraction process of the volatile oil, the solid-to-liquid ratio of the taxus chinensis branches and leaves to the fragrance-extracting petroleum ether is too small, and the extraction is incomplete, so that the extraction rate of the volatile oil is influenced; the solid-liquid ratio is too large, the extraction rate is improved, but the waste of energy and solvent is easily caused, and some other unnecessary components can be leached out, so that the purity of the product fragrance is influenced. In the invention, 1kg of taxus chinensis branches and leaves are added with 10-20kg of fragrance-enhanced petroleum ether as a solvent for extraction each time, so that the best effect of extracting volatile oil from taxus chinensis can be achieved;
(3) along with the increase of the leaching temperature, the solubility of the volatile oil is increased, the diffusion rate is also increased, and the extraction rate is obviously improved; along with the increase of the temperature, the solubility of a plurality of ether-soluble substances in the taxus chinensis is increased, the extraction rate is improved, but the filtration is difficult during the concentration. Therefore, considering all together, the extraction temperature in the present invention is 30-55 ℃.
Detailed Description
Example 1
The solid taxus chinensis perfume and the preparation method thereof comprise the following steps:
step 1, pretreatment of raw materials: selecting fresh branches and leaves of taxus chinensis, cleaning, drying in an oven, controlling the temperature below 60 ℃, and then crushing with the granularity of 30-40 meshes;
step 2, leaching of volatile oil: 1kg of crushed taxus chinensis branches and leaves are put into 35 ℃ fragrance-enhanced petroleum ether for continuous leaching twice, 15kg of fragrance-enhanced petroleum ether is added each time, and the leaching time is 4 hours for the first time and 2 hours for the second time. Filtering, mixing the extractive solutions, and removing residue to obtain extractive solution containing volatile oil;
step 3, post-treatment of the leaching liquor: putting the leaching liquor into a distiller to distill off petroleum ether in the leaching liquor to obtain extract; dissolving the extract with 5 times of 75% ethanol, cooling at-20 deg.C for 12 hr, filtering to remove residue to obtain ethanol extractive solution, placing into a vacuum distiller, concentrating under reduced pressure, removing ethanol, and removing residue to obtain pure oil of Taxus chinensis;
step 4, preparing the microcapsule solid perfume: mixing and stirring 10g of beta-cyclodextrin, 1g of maltodextrin and 100mL of water at 60 ℃ to prepare a saturated solution, preliminarily emulsifying to prepare a water phase, cooling to 35 ℃, dissolving 1mL of absolute oil of the taxus chinensis and 1mL of absolute ethanol to prepare an oil phase, slowly adding the oil phase into the water phase, magnetically stirring and embedding for 1h, cooling to room temperature, refrigerating at 0-5 ℃, filtering, and drying to obtain the taxus chinensis microcapsule solid perfume.
Example 2
The solid taxus chinensis perfume and the preparation method thereof comprise the following steps:
step 1, pretreatment of raw materials: selecting fresh branches and leaves of taxus chinensis, cleaning, drying in an oven, controlling the temperature below 60 ℃, and then crushing with the granularity of 30-40 meshes;
and 2, leaching the volatile oil. 1kg of crushed taxus chinensis branches and leaves are put into 45 ℃ fragrance-enhanced petroleum ether for continuous leaching twice, 20kg of fragrance-enhanced petroleum ether is added each time, and the leaching time is 3 hours for the first time and 1 hour for the second time. Filtering, mixing the extractive solutions, and removing residue to obtain extractive solution containing volatile oil;
and 3, post-treating the leaching liquor. Putting the leaching liquor into a distiller to distill off petroleum ether in the leaching liquor to obtain extract; dissolving the extract in 3 times of 90% ethanol by weight, cooling at-20 deg.C for 24 hr, filtering to remove residue to obtain ethanol extractive solution, placing into a vacuum distiller, concentrating under reduced pressure, and removing ethanol to obtain pure oil of Taxus chinensis;
and 4, preparing the microcapsule solid perfume. Mixing and stirring 10g of beta-cyclodextrin, 1g of maltodextrin and 100mL of water at 60 ℃ to prepare a saturated solution, preliminarily emulsifying to prepare a water phase, cooling to 35 ℃, dissolving 1.5mL of absolute oil of the taxus chinensis and 1.5mL of absolute ethyl alcohol to prepare an oil phase, slowly adding the oil phase into the water phase, magnetically stirring and embedding for 1h, cooling to room temperature, refrigerating at 0-5 ℃, filtering, and drying to obtain the solid perfume microcapsule of the taxus chinensis.
Example 3
The solid taxus chinensis perfume and the preparation method thereof comprise the following steps:
step 1, pretreatment of raw materials: selecting fresh branches and leaves of taxus chinensis, cleaning, drying in an oven, controlling the temperature below 60 ℃, and then crushing with the granularity of 30-40 meshes;
step 2, leaching of volatile oil: 1kg of crushed branches and leaves of the taxus chinensis is put into the 45 ℃ fragrance-enhanced petroleum ether for continuous leaching twice, 20kg of fragrance-enhanced petroleum ether is added each time, and the leaching time is 2.5 hours for the first time and 1.5 hours for the second time. Filtering, mixing the extractive solutions, and removing residue to obtain extractive solution containing volatile oil;
step 3, post-treatment of the leaching liquor: putting the leaching liquor into a distiller to distill off petroleum ether in the leaching liquor to obtain extract; dissolving the extract in 5 times of 80% ethanol by weight, cooling at-20 deg.C for 24 hr, filtering to remove residue to obtain ethanol extractive solution, placing into a vacuum distiller, concentrating under reduced pressure, removing ethanol, and removing residue to obtain pure oil of Taxus chinensis;
step 4, preparing the microcapsule solid perfume: mixing and stirring 10g of beta-cyclodextrin, 1g of maltodextrin and 100mL of water at 60 ℃ to prepare a saturated solution, preliminarily emulsifying to prepare a water phase, cooling to 35 ℃, dissolving 2mL of absolute oil of the taxus chinensis and 2mL of absolute ethanol to prepare an oil phase, slowly adding the oil phase into the water phase, magnetically stirring and embedding for 1h, cooling to room temperature, refrigerating at 0-5 ℃, filtering, and drying to obtain the taxus chinensis microcapsule solid perfume.
Experimental example 1 antibacterial function test of purified oil of Taxus chinensis
(1) Selection of strains
The strains selected in the in vitro bacteriostasis test are respectively as follows: escherichia coli, staphylococcus aureus, and salmonella.
(2) Preparation of oil-purifying bacteriostatic agent of taxus chinensis
Precisely measuring 256mg of Taxus chinensis absolute oil in a 5mL brown volumetric flask, and adding dimethyl sulfoxide to a constant volume for later use. And finally, the mass concentration of the taxus chinensis absolute oil bacteriostatic agent is 51.2 mg/mL.
(3) Preparation of the bacterial suspension
Activating test strains, inoculating to corresponding culture medium, passaging twice, determining bacterial amount by turbidimetry, and making into 1 × 106cFu/mL of bacterial suspension.
(4) Preparation of the culture Medium
MH broth was prepared.
(5) Detection of Minimum Inhibitory Concentration (MIC)
The MIC of the purified oil of taxus chinensis prepared in the three examples was measured by the two-fold dilution method. 48 sterile test tubes are taken and averagely divided into 4 groups and numbered. Taking 12 sterile test tubes (13 × 100mm) of the first group, arranging in a row, adding 1mL MH broth into each tube except 1.6mL MH broth into the 1 st tube, adding 0.4mL of the taxus chinensis absolute bacteriostatic agent (51.2mg/mL) obtained in example 1 into the 1 st tube, mixing uniformly, sucking 1mL into the 2 nd tube, sucking 1mL into the 3 rd tube after mixing uniformly, diluting to the 11 th tube in a multiple proportion continuously, sucking 1mL from the 11 th tube, discardingTube 12 is a growth control without drug. In this case, the drug concentrations in each tube were 10.24, 5.12, 2.56, 1.28, 0.64, 0.32, 0.16, 0.08, 0.04, 0.02, and 0.01mg/mL in this order. Then, 1mL of each prepared bacterial suspension was added to each tube to give a final bacterial liquid concentration of about 5X 105cFu/mL. The drug concentrations of the 1 st tube to the 11 th tube are 5.12, 2.56, 1.28, 0.64, 0.32, 0.16, 0.08, 0.04, 0.02, 0.01 and 0.005mg/mL respectively. Culturing for 24h in a 37 ℃ incubator, and recording the minimum bacteriostatic concentration of the liquid culture medium without turbidity after the culture is finished, namely the minimum bacteriostatic concentration. The second, third and fourth groups were added with the oil-purifying bacteriostatic agent of Taxus chinensis obtained in examples 2, 3 and 4, respectively, and the rest were performed as above.
(4) Test results
The lowest inhibitory concentration of the sample. The results are shown in the following table:
TABLE 2 minimum inhibitory concentrations (mg/mL) for three examples against three bacteria
As can be seen from Table 2, the MICs of the Taxus chinensis absolute oil on Escherichia coli, Staphylococcus aureus and Salmonella were 0.32mg/mL, 0.08mg/mL and 0.64mg/mL, respectively. The antibacterial effect of the taxus chinensis absolute on staphylococcus aureus is the best.
Experimental example 2 fragrance retention time test
100g of each of the products of examples 1 to 3 was placed in an open cup at a normal temperature of 26 to 36 ℃ for 10 weeks in summer, and subjected to a nasal odor test every full week. The test results confirmed that examples 1 to 3 all maintained a strong fragrance for 10 weeks or more. After 10 weeks, the aroma was reduced.
100g of each of the products of examples 1 and 2 was placed in an open cup at a room temperature of 26 ℃ or lower in spring and autumn and winter for 12 weeks, and a nasal odor test was performed every full week. The test results confirmed that the fragrance retention time of examples 1 to 3 was 12 weeks or more.
The invention adopts the composite wall material of beta-cyclodextrin and maltodextrin, avoids the defect that the volatile oil of the taxus chinensis cannot be effectively embedded by using one wall material alone, not only can improve the embedding rate of the taxus chinensis microcapsules, but also can achieve the effect of improving the compactness of the taxus chinensis microcapsule membrane, the aroma is kept for more than 10 weeks under the high-temperature condition in summer, and the aroma is kept for more than 12 weeks in spring, autumn and winter, thereby fully meeting the requirements of people.
The invention is not to be considered as limited to the particular embodiments shown, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (4)
1. The preparation method of the taxus chinensis solid perfume is characterized by comprising the following steps:
step 1, pretreatment of raw materials: selecting fresh branches and leaves of taxus chinensis, cleaning, drying and crushing;
step 2, leaching of volatile oil: leaching pulverized branches and leaves of Taxus chinensis in petroleum ether, filtering to obtain leaching solution, and removing residue to obtain leaching solution containing volatile oil;
step 3, post-treatment of the leaching liquor: evaporating petroleum ether in the leaching liquor to obtain extract; dissolving the extract in ethanol, cooling, filtering to remove residue to obtain ethanol extractive solution, concentrating under reduced pressure, removing ethanol, and removing residue to obtain pure oil of Taxus chinensis;
step 4, preparing the microcapsule solid perfume: mixing beta-cyclodextrin, maltodextrin and water, stirring to obtain saturated solution, and primarily emulsifying to obtain water phase; dissolving the taxus chinensis absolute oil obtained in the step 3 with absolute ethyl alcohol to prepare an oil phase, slowly adding the oil phase into the water phase, embedding, cooling to room temperature, refrigerating, filtering, and drying to obtain taxus chinensis microcapsule solid perfume;
during the extraction of the volatile oil in the step 2, the crushed Chinese yew branches and leaves are continuously extracted twice in the aroma-extracting petroleum ether, the leaching liquor is combined after filtration, and the weight ratio of the crushed Chinese yew branches and leaves to the aroma-extracting petroleum ether is 1: 10-20, putting the crushed branches and leaves of the taxus chinensis into aroma-extracting petroleum ether at the temperature of 30-55 ℃ for continuous two times of leaching, wherein the leaching time is 2-4 hours for the first time and 1-3 hours for the second time;
and during the post-treatment of the leaching liquor in the step 3: putting the leaching liquor into a distiller to distill off petroleum ether in the leaching liquor to obtain extract;
in the step 3, adding 60-90% ethanol in an amount which is 3-6 times the weight of the extract to dissolve the extract, cooling the extract at-20 ℃ for 12-24 hours, filtering out residues to obtain an ethanol extract, then placing the ethanol extract into a reduced pressure distiller, concentrating the ethanol extract under reduced pressure under the vacuum degree, removing the ethanol, and removing the residues to obtain the taxus chinensis absolute;
in the step 4, the weight ratio of the beta-cyclodextrin to the maltodextrin is 10:1, the beta-cyclodextrin, the maltodextrin and water are mixed and stirred at 60 ℃ to prepare a saturated solution, the saturated solution is preliminarily emulsified to prepare a water phase, the water phase is cooled to 35 ℃, the absolute oil of the taxus chinensis and absolute ethyl alcohol are dissolved to prepare an oil phase, then the oil phase is slowly added into the water phase, the mixture is magnetically stirred and embedded for 1 hour, the mixture is cooled to room temperature, and the mixture is refrigerated at 0-5 ℃, filtered and dried to obtain the taxus chinensis microcapsule solid perfume.
2. The method for preparing yew solid perfume of claim 1, wherein the raw material is pretreated in step 1 by selecting fresh yew branches and leaves, cleaning, drying in an oven, controlling the temperature below 60 ℃, and then pulverizing to 30-40 mesh.
3. The method for preparing the solid perfume of taxus chinensis as claimed in claim 1, wherein the microcapsule solid perfume in step 4 is prepared by taking 3-5 parts of absolute oil of taxus chinensis, adding 0.2-0.5 part of monoglyceride and a proper amount of 30-50% ethanol aqueous solution, and carrying out rapid homogeneous emulsification to prepare an emulsion.
4. A solid perfume of Taxus chinensis obtained by the method of any one of claims 1 to 3.
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| CN1301321C (en) * | 2004-07-02 | 2007-02-21 | 西北工业大学 | Method for extracting natural perfume from persimmon leaf or bark |
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| CN103211844B (en) * | 2013-03-26 | 2015-04-15 | 安徽和华生物医药科技有限公司 | Extraction method of taxus active extract |
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| CN103877600B (en) * | 2014-03-27 | 2017-04-05 | 沈祖鸿 | Spray containing Ramulus et folium taxi cuspidatae Extract and its manufacture method and manufacture formula |
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| CN106701319A (en) * | 2016-12-20 | 2017-05-24 | 福建喜果红豆杉科技发展有限公司 | Method for extracting taxus chinensis essential oil |
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