CN106038343B - A kind of extraction process of mulberrin crude product - Google Patents
A kind of extraction process of mulberrin crude product Download PDFInfo
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
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- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
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- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/40—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
- A61K8/41—Amines
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- A—HUMAN NECESSITIES
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- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/55—Phosphorus compounds
- A61K8/553—Phospholipids, e.g. lecithin
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- A61K8/67—Vitamins
- A61K8/678—Tocopherol, i.e. vitamin E
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- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/81—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- A61K8/8141—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
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- A—HUMAN NECESSITIES
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- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
- A61Q17/04—Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning preparations
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- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
- C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
- C07D311/28—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only
- C07D311/30—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only not hydrogenated in the hetero ring, e.g. flavones
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- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
- C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
- C07D311/40—Separation, e.g. from natural material; Purification
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- A—HUMAN NECESSITIES
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- 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
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
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Abstract
The present invention relates to a kind of extraction processes of mulberrin crude product, belong to sun-prevention component extractive technique field.A kind of extraction process of mulberrin crude product, includes the following steps：1. crushing；2. degreasing；3. weighing；4. Microwave Extraction；5. detaching drying；A kind of includes the sun-screening agent of mulberrin, includes 1 15 parts of mulberrin intermediate, 3 parts of lecithin, 1 part of carbomer, 1 part of carbomer neutralizer and water according to mass fraction；The mulberrin intermediate is the mixture of mulberrin, lipid solvent and antioxidant.A kind of more general microwave extraction method of extraction process extraction rate of mulberrin crude product of the present invention faster, extraction efficiency higher；Include mulberrin sun-screening agent is of low cost, sun-proof result is good.
Description
Technical field
The present invention relates to sun-prevention component extractive technique fields, and in particular to a kind of extraction process of mulberrin crude product.
Background technology
Sunburn generally refers to injury of the ultraviolet light to human body, and usually, short wave ultraviolet UVC rays are substantially big
Ozone layer in gas absorbs, and remaining a small amount of arrival ground will not damage human body, ultraviolet B radiation UVB can penetrate skin
Epidermis and cuticula, be cause to burn, the main contributor of indirect pigment deposition and skin cancer, main performance skin of burning
There is erythema, severe patient is likely to occur the symptom of oedema, blister, decortication, fever and nausea, and long wave ultraviolet UVA is to human body
Injury gradually causes the concern of people, it can penetrate skin corium or even subcutaneous tissue, and have cumulative bad, can also aggravate UVB and make
At injury.
Mulberrin (mulberroside) belongs to Polyhydroxystibene (polyhydroxystibene, PHS),
Polyhydroxystibene is present in the bast of plant more, when plant is by germ infection, ultraviolet light irradiation or chemical contamination
When Deng stimulating, being excited position and generating this degeneration-resistant substance, i.e. phytoalexin, it is anti-that mulberrin can substitute parts of traditional chemistry
Agent is shone, while reducing the usage amount of traditional chemical sun-screening agent, improves the product safety in utilization of cosmetics.
The Chinese invention patent that Authorization Notice No. is CN 103006519B discloses a kind of natural plant sun agent and its system
Preparation Method and application use ethyl alcohol to be heated to reflux to extract the mulberrin in paper mulberry bark, and the method for purification recovery rate is low, consumes
Duration；Also have microwave abstracting in the prior art, be made using the effect of electromagnetic field it is certain organic in solid or semisolid substance
Object ingredient is efficiently separated with matrix, and can keep a kind of separation method of the script compound state of analysis object, extraction
Efficiency and extraction rate are heated to reflux extraction compared with ethyl alcohol and greatly improve, and the time of general Microwave Extraction Phellinus skin element is 90 seconds
Left and right, the Phellinus skin element crude product that every gram of paper mulberry bark powder can be extracted into is about at 0.47-0.50 grams；But by microwave extraction method
Extraction for Phellinus skin element also has very big potentiality to further increase extraction efficiency and rate of extraction.
Invention content
The purpose of the present invention is to solve the above-mentioned problems, to provide a kind of extraction process and packet of mulberrin crude product
Sun-screening agent containing mulberrin.
Technical proposal that the invention solves the above-mentioned problems is as follows：
A kind of extraction process of mulberrin crude product, includes the following steps：
1. crushing：Paper mulberry bark is crushed, to form paper mulberry bark powder spare for sieving；
2. degreasing：The paper mulberry bark powder is subjected to ungrease treatment, is then dried；
3. weighing：Weigh the paper mulberry bark powder after 1 mass parts degreasing, the extractant of 250-350 mass parts, after degreasing
Paper mulberry bark powder is placed in the extractant；
4. Microwave Extraction：Step 3. in extractant in dispersion microballon is added, microwave power arranges 500-800W, will
Step 3. in the extractant containing paper mulberry bark powder using Microwave Extraction 5-15 seconds；
5. detaching drying：Extraction solution after Microwave Extraction is filtered to filter out dispersion microballon, is in by filtrate rotary evaporation
Powdered.
The mechanism of microwave abstracting can be analyzed in terms of following 3：
1. microwave radiation process is frequency electromagnetic waves penetrate spe medium reach material inside microtubule fasolculus and glandular cell's system
Process.Due to absorbing microwave energy, the temperature of cell interior will rise rapidly, to make the pressure of cell interior be more than cell
Wall expands the ability that can bear, as a result cell rupture, in active ingredient freely flow out, and dissolve at a lower temperature
In spe medium.
2. electromagnetic field caused by microwave can accelerate the molecule for being extracted component to be spread from solid interior to solid liquid interface
Rate.For example, when with water as solvent, under the action of microwave field, hydrone is changed into excitation state by high-speed rotation state, this is
A kind of unstable state of high-energy.Hydrone either vaporizes the driving force to reinforce extracted component or discharges and comes from this time
The extra energy of body returns to ground state, and the energy released will be passed to the molecule of other substances, to accelerate its warm-up movement, to
The molecule for shortening extracted component is diffused to the time of solid liquid interface by solid interior, and extraction rate is as a result made to improve several times, and energy
Extraction temperature is reduced, ensures the quality of extract to the maximum extent.
3. the frequency and the frequency dependence of molecule rotation due to microwave connect, microwave energy is one kind by Ion transfer and idol
Extremely son rotates and causes the non-ionising radiation energy of molecular motion that can promote the rotational motion of molecule when it acts on molecule,
If molecule has certain polarity, you can generate instantaneous polarization under the action of microwave field, and made with the speed of 24.5 hundred million times/s
Reversal campaign to generate vibration, tearing and the interparticle friction and collision of key, and is quickly generated a large amount of thermal energy,
Promote cell rupture, cell liquid is made to overflow and diffuse in solvent.In microwave abstracting, base can be made by absorbing the difference of microwave ability
The some regions of body substance or certain components in extraction system are selectively heated, to make to be extracted substance from matrix or body
It detaches, is entered in the relatively poor extractant of smaller dielectric constant, microwave absorption capacity in system.
A diameter of 0.1-0.5mm of the dispersion microballon, when carrying out microwave abstracting, since microwave causes solvent and mulberry tree
Material absorbing inside skin powder simultaneously discharges amount of heat, and this warm-up movement drives paper mulberry bark powder particles and the dispersion microballon expecting
Irregular movement in liquid system, wherein the dispersion microballon is played grinding by the collision with paper mulberry bark powder particles and stirred herein
The effect mixed accelerates extraction process, improves extraction efficiency so that the time of microwave heating substantially reduces, and improves mulberry skin
The extraction efficiency of flavine reduces extraction cost.
As a preferred embodiment of the above technical solution, step 4. in for hold extractant and disperse microballon container be use
Extraction container made of polypropylene material, the inner surface of the extraction container is fine and close, the inner surface of the extraction container and described
Flexible polypropylene fiber layer is provided between the outer surface of extraction container；The extraction container be placed on can shake it is flat
On platform, when extraction, the platform vibrations, auxiliary drives the dispersion microballon to make irregular movement in the extractant.
As a preferred embodiment of the above technical solution, the dispersion microballon used in the Microwave Extraction step is the glass of surface compact
Glass or ceramic microsphere.
Glass and ceramic material can be used for grinding and stirring material under microwave condition, and can not by microwave action
Reusability.
As a preferred embodiment of the above technical solution, the dispersion microballon inner sealing has phase-change wax, the phase alternating temperature of the phase-change wax
Degree is more than 60 DEG C.
As the advanced scheme of the dispersion microballon, it is closed with phase-change wax inside the dispersion microballon so that dispersion is micro-
Pearl remains at same temperature during agitation grinding, with consistently forming a temperature between feed liquid and paper mulberry bark powder particles
Gradient is spent, mulberrin is promoted to ooze out and dissolve outward under the action of concentration difference；It implies that and increases in paper mulberry bark powder particles
The power that mulberrin oozes out outward increases what temperature difference was brought other than concentration difference, the release of microwave energy, agitation grinding
Diffusion kinetics further improve the extraction efficiency and extraction rate of mulberrin.
As a preferred embodiment of the above technical solution, the extractant used in step that weighs is the ethanol water of 50%-90%
Solution.
As a preferred embodiment of the above technical solution, in the defatting step, degreasing method is that paper mulberry bark powder is immersed in caustic soda
In aqueous solution, soaking time is 5-12 hours, is taken out after immersion；Or, being taken out after paper mulberry bark powder is boiled 30 minutes in water.
As a preferred embodiment of the above technical solution, the sieve of 40-200 mesh is used in the pulverising step to the sieving of paper mulberry bark powder
Son.
A kind of includes the sun-screening agent of mulberrin, includes 1-15 parts of mulberrin intermediate, lecithin 3 according to mass parts
Part, 1 part of carbomer, 1 part of carbomer neutralizer and water；The mulberrin intermediate is mulberrin, lipid solvent and resists
The mixture of oxidant.
As a preferred embodiment of the above technical solution, the mulberrin intermediate is mulberrin, isononyl isononanoate and dimension
The mixture of raw element E, wherein the mass fraction ratio of mulberrin, isononyl isononanoate and vitamin E are 2:4:3.
As a preferred embodiment of the above technical solution, the carbomer neutralizer is triethanolamine.
As a preferred embodiment of the above technical solution, the water is the deionized water by reverse osmosis membrane filtration.
The sun-screening agent is the more single sun-screening agent of function, has the effect of that of low cost, sun-proof result is good.Wherein ovum
Phosphatide has the function of Palmitoleic Acid so that sun-screening agent can be preferably bonded on the skin, the card wave neutralized through triethanolamine
Nurse viscosity increases so that sun-screening agent is easier to shape.
In conclusion the invention has the advantages that：
A kind of more general microwave extraction method of extraction process extraction rate of mulberrin crude product of the present invention is more
Soon, extraction efficiency higher；Include mulberrin sun-screening agent is of low cost, sun-proof result is good.
Specific implementation mode
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Embodiment in the present invention, ordinary skill
All other embodiment that personnel are obtained under the premise of not doing creative work, shall fall within the protection scope of the present invention.
With embodiment, the present invention is described in detail below, and embodiment 1-3 is the extraction process of mulberrin crude product,
Its technological parameter and extraction effect are shown in Table 1：
The technological parameter and extraction effect of the extraction process of 1 mulberrin crude product of table
It is as follows：
Embodiment 1：A kind of extraction process of mulberrin crude product, includes the following steps：
1. crushing：Paper mulberry bark is crushed, to form paper mulberry bark powder spare for sieving；
2. degreasing：The paper mulberry bark powder is immersed in caustic-soda aqueous solution, soaking time is 5 hours, and then drying is weighed；
3. weighing：Weigh the paper mulberry bark powder after 1 mass parts degreasing, the extractant of 250 mass parts, by the mulberry tree after degreasing
Skin powder is placed in 90% ethanol water；
4. Microwave Extraction：Step 3. in extractant in the dispersion microballon of glass system is added, microwave power arranges
500W, by step 3. in the extractant containing paper mulberry bark powder using Microwave Extraction 5 seconds；
5. detaching drying：Extraction solution after Microwave Extraction is filtered to filter out dispersion microballon, is in by filtrate rotary evaporation
Powdered.
Such method can extract the crude product of 0.49 gram of mulberrin of mulberrin product in every gram of paper mulberry bark powder, carry
It is 5 seconds to take the time.
Embodiment 2：A kind of extraction process of mulberrin crude product, includes the following steps：
1. crushing：Paper mulberry bark is crushed, to form paper mulberry bark powder spare for sieving；
2. degreasing：The paper mulberry bark powder is boiled 30 minutes in boiling water, then drying is weighed；
3. weighing：Weigh the paper mulberry bark powder after 1 mass parts degreasing, the extractant of 350 mass parts, by the mulberry tree after degreasing
Skin powder is placed in 50% ethanol water；
4. Microwave Extraction：Step 3. in extractant in be added dispersion microballon made of ceramics, in the dispersion microballon
Be 70 DEG C of phase-change wax containing phase transition temperature, microwave power arranges 800W, by step 3. in the extractant containing paper mulberry bark powder
It is to be held using being extracted made of polypropylene material for holding extractant and disperseing the container of microballon using Microwave Extraction 15 seconds
The inner surface of device, the extraction container is fine and close, is set between the inner surface of the extraction container and the outer surface of the extraction container
It is equipped with flexible polypropylene fiber layer, the extraction container is placed on the platform that can be shaken, when extraction, the platform shake
Dynamic, auxiliary drives the dispersion microballon to make irregular movement in the extractant；
5. detaching drying：Extraction solution after Microwave Extraction is filtered to filter out dispersion microballon, is in by filtrate rotary evaporation
Powdered.
Such method can extract the crude product of 0.52 gram of mulberrin of mulberrin product in every gram of paper mulberry bark powder, carry
It is 15 seconds to take the time.
Embodiment 3：A kind of extraction process of mulberrin crude product, includes the following steps：
1. crushing：Paper mulberry bark is crushed, to form paper mulberry bark powder spare for sieving；
2. degreasing：The paper mulberry bark powder is immersed in caustic-soda aqueous solution, soaking time is 12 hours, and then drying claims
Weight；
3. weighing：Weigh the paper mulberry bark powder after 1 mass parts degreasing, the extractant of 300 mass parts, by the mulberry tree after degreasing
Skin powder is placed in 70% ethanol water；
4. Microwave Extraction：Step 3. in extractant in be added dispersion microballon made of ceramics, in the dispersion microballon
Be 80 DEG C of phase-change wax containing phase transition temperature, microwave power arranges 800W, by step 3. in the extractant containing paper mulberry bark powder
It is to be held using being extracted made of polypropylene material for holding extractant and disperseing the container of microballon using Microwave Extraction 10 seconds
The inner surface of device, the extraction container is fine and close, is set between the inner surface of the extraction container and the outer surface of the extraction container
It is equipped with flexible polypropylene fiber layer, the extraction container is placed on the platform that can be shaken, when extraction, the platform shake
Dynamic, auxiliary drives the dispersion microballon to make irregular movement in the extractant；
5. detaching drying：Extraction solution after Microwave Extraction is filtered to filter out dispersion microballon, is in by filtrate rotary evaporation
Powdered.
Such method can extract the crude product of 0.55 gram of mulberrin of mulberrin product in every gram of paper mulberry bark powder, carry
It is 10 seconds to take the time.
Embodiment 4：A kind of includes the sun-screening agent of mulberrin, includes 1 part of mulberrin intermediate, ovum according to mass parts
Phosphatidase 3 part, 1 part of carbomer, 1 part of triethanolamine and deionized water；The mulberrin intermediate is mulberrin, lipid is molten
The mixture of agent and antioxidant；The mulberrin intermediate is the mixing of mulberrin, isononyl isononanoate and vitamin E
The mass fraction ratio of object, wherein mulberrin, isononyl isononanoate and vitamin E is 2:4:3.
Embodiment 5：A kind of includes the sun-screening agent of mulberrin, includes 5 parts of mulberrin intermediate, ovum according to mass parts
Phosphatidase 3 part, 1 part of carbomer, 1 part of triethanolamine and deionized water；The mulberrin intermediate is mulberrin, lipid is molten
The mixture of agent and antioxidant；The mulberrin intermediate is the mixing of mulberrin, isononyl isononanoate and vitamin E
The mass fraction ratio of object, wherein mulberrin, isononyl isononanoate and vitamin E is 2:4:3.
Embodiment 6：A kind of includes the sun-screening agent of mulberrin, according to mass parts include 15 parts of mulberrin intermediate,
3 parts of lecithin, 1 part of carbomer, 1 part of triethanolamine and deionized water；The mulberrin intermediate is mulberrin, lipid
The mixture of solvent and antioxidant；The mulberrin intermediate is the mixed of mulberrin, isononyl isononanoate and vitamin E
Object is closed, the wherein mass fraction ratio of mulberrin, isononyl isononanoate and vitamin E is 2:4:3.
Table 2 is that the sun-proof result of the sun-screening agent made by embodiment 4- embodiments 6 compares table, by table as it can be seen that implementing
Sun-screening agent sun-proof result in example 5 is best, and embodiment 6 is taken second place, and embodiment 4 is relatively minimum：
The sun-proof result of sun-screening agent made by 2 embodiment 4- embodiments 6 of table compares
MED is to cause ultraviolet dosage minimum needed for erythema on the skin in table, abbreviation minimal erythema dose (
Minimum Ery themaDose)。
Claims (3)
1. a kind of extraction process of mulberrin crude product, which is characterized in that include the following steps：
1. crushing：Paper mulberry bark is crushed, to form paper mulberry bark powder spare for sieving；
2. degreasing：The paper mulberry bark powder is subjected to ungrease treatment, is then dried；
3. weighing：Weigh the paper mulberry bark powder after 1 mass parts degreasing, the extractant of 250-350 mass parts, by the mulberry tree after degreasing
Skin powder is placed in the extractant, and the extractant is the ethanol water of 50%-90%；
4. Microwave Extraction：Step 3. in extractant in be added dispersion microballon, microwave power arranges 500-800W, by step
Extractant containing paper mulberry bark powder in 3. using Microwave Extraction 5-15 seconds, the dispersion microballon used for the glass of surface compact or
Ceramic microsphere, the dispersion microballon inner sealing have phase-change wax, the phase transition temperature of the phase-change wax to be more than 60 DEG C；
5. detaching drying：Extraction solution after Microwave Extraction is filtered to filter out dispersion microballon, is in powder by filtrate rotary evaporation
Shape.
2. a kind of extraction process of mulberrin crude product according to claim 1, which is characterized in that the defatting step
In, degreasing method is that paper mulberry bark powder is immersed in caustic-soda aqueous solution, and soaking time is 5-12 hours, is taken out after immersion；Or, will
Paper mulberry bark powder takes out after boiling 30 minutes in water.
3. a kind of extraction process of mulberrin crude product according to claim 1, which is characterized in that the pulverising step
In to paper mulberry bark powder sieving using 40-200 mesh sieve.
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| CN107714547A (en) * | 2017-11-02 | 2018-02-23 | 宁波凯斯宝玛卫厨有限公司 | A kind of sun screen |
| CN110169472B (en) * | 2019-05-15 | 2021-05-18 | 安徽省万清堂生物科技有限公司 | Method for extracting natural antioxidant for functional health tea |
| CN110051659A (en) * | 2019-06-14 | 2019-07-26 | 贵州理工学院 | Mulberrin is preparing the application in osteosporosis resistant medicament |
| CN111228140B (en) * | 2020-03-23 | 2022-06-21 | 汕头市奇伟实业有限公司 | A pressed powder composition with nanometer rice starch as matrix powder |
| CN115282141A (en) * | 2022-07-06 | 2022-11-04 | 赵俊杰 | Mulberry bark flavin nano crystal and its application |
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| CN103006519A (en) * | 2013-01-11 | 2013-04-03 | 广州市白云区新东方日用化工品厂 | Natural plant sun-screening agent as well as preparation method and application of natural plant sun-screening agent |
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| KR100253842B1 (en) * | 1997-09-12 | 2000-07-01 | 유상옥 | Mulberrin containing skin whitening compositions |
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| CN103006519A (en) * | 2013-01-11 | 2013-04-03 | 广州市白云区新东方日用化工品厂 | Natural plant sun-screening agent as well as preparation method and application of natural plant sun-screening agent |
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| 微波法提取陈皮中的挥发油;鲁建江等;《中国药师》;20011231;第4卷(第5期);第393页 * |
| 微波萃取法提取桑叶和桑白皮的黄酮类成分;陈菁菁等;《中药材》;20061031;第29卷(第10期);第1090-1092页 * |
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