CN107569411A - A kind of plant source Moschus cosmetics and preparation method thereof - Google Patents
A kind of plant source Moschus cosmetics and preparation method thereof Download PDFInfo
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- CN107569411A CN107569411A CN201710658474.9A CN201710658474A CN107569411A CN 107569411 A CN107569411 A CN 107569411A CN 201710658474 A CN201710658474 A CN 201710658474A CN 107569411 A CN107569411 A CN 107569411A
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Abstract
A kind of plant source Moschus cosmetics, are made up of by weight percentage following components:10 30 parts of ethanol, 35 parts of Lavender, 25 parts of nerol, 28 parts of eucalyptus oil, 12 parts of Archangelica officinalis Hoffmann lactone, 12 parts of cinnamic acid, 12 parts of citronellal, 14 parts of plant source muskone, 30 50 parts of rose pure dew water.For the present invention using the single-stranded aliphatic acid musk ambrette ketone containing carbochain identical with muskone, energy bottom line reduces muskone synthesis cost, the use of vegetable oil is raw material, natural environmental-protective, the new application of edible oil is opened, expands the application of edible oil, industrialization large-scale production and application can be used as.
Description
Technical field
The invention belongs to field of pharmacology, in particular it relates to a kind of natural product extraction application field, more specifically, relating to
And a kind of method using vegetable oil musk ambrette ketone and its application in household chemicals field.
Background technology
Moschus is one kind of Chinese medicine, and its medicinal source be musk deer section animal, such as woods musk deer, horse musk deer or former musk deer, the hero of maturation
Drying secretion in body note capsule.Moschus is pungent, warm, nontoxic, bitter.Enter the heart, spleen, Liver Channel, have and have one's ideas straightened out, ward off dirty, dredging collateral, scattered silt
Function.Cure mainly apoplexy, coma due to blocking of the respiratory system, frightened epilepsy, middle evil unhappiness, trusted subordinate sudden and violent pain, traumatic injury, swollen ulcer drug.Many clinical material tables
It is bright, during patients with coronary heart disease angina pectoris attacks, or in faint suffer a shock when, take the Soviet Union using Moschus as main component and close ball, the state of an illness
It can be eased.Moschus is also the important source material for preparing advanced essence, is allotment advanced articles for use of burning incense, cosmetics and flavouring
Valuable spices.
Muskone is important active ingredient, its content account in natural musk meat 1.58%~1.84%, account for natural musk deer
0.90%~3.08% in fragrant hair shell, have been able to artificial synthesized.Moschus principle active component is muskone, containing muskone,
Normuscone, 3-methylcyclopentadecanol, Moschus pyrans, muscopyridine, hydroxyl muscopyridine-A, hydroxyl muscopyridine-B, 3- methyl ring 13
Ketone, ring tetradecane ketone etc..
But musk deer is animals under first-class state protection, the male musk deer that China only deposits only has 50,000 remainders, in Critical Condition, China
The annual requirement of Moschus can use fragrant 10g to calculate more than 15 tons, by every male musk deer, also be only capable of obtaining 0.5 ton even if all catching and killing,
Medication demand can not all meet, let alone fragrance applications, and imbalance between supply and demand is huge.At present, can be with by artificial synthesized method
Go out product using petroleum by-product butadiene, long-chain biatomic acid, ethyl acetoacetate etc. and musk deer is synthesized by the methods of bromination, oxidation
Ketone musk, succeed, but because muskone is a kind of macrolides compound, its synthesis material is less susceptible to obtain, profit
Ring enlargement reaction condition harshness is carried out with short chain fatty acids, yield is relatively low, also highly difficult using single-stranded big ring open loop chain rupture, so
It is more direct come musk ambrette ketone using the chemical composition similar with muskone structure.
The material of naturally occurring 15 carbochains is using nervonic acid as representative, in Malania Oleifera Oil, mustard oil and Queensland nut
It is found in oil, obtains the diluted acid of carbon 15 using the diluted acid of plant oil extract carbon 15, then through peroxone oxidation, be finally catalyzed
The lower progress cyclization of agent effect obtains muskone.
National inventing patent disclosed in 2016 " efficiently a kind of gently prepare muskone method ", use natural musk for
Raw material prepares muskone, obtains high purity muscone using the method for alcohol reflux and spray drying, but raw material is still country
Animal is protected, can not be mass produced;Invention disclosed patent " (the 4R) -4- methyl-15s-ketone of alkenyl 6- 16 in 2008
Derivative, synthetic method and its purposes in musk ambrette ketone ", use the small fragment lactone obtained with steroid sapogenin degradation
Prepared for raw material, this kind of compound can be used for pure muskone (the R)-Muscone of synthesizing optical.The invention provides
A kind of method using steroid saponin musk ambrette ketone.
At present, the method for the single-stranded aliphatic acid musk ambrette ketone with carbochain identical with muskone is there are no in the prior art
Patent report.
The content of the invention
The vegetable oil rich in the diluted acid of carbon 15, further extraction separation, synthesis are utilized it is an object of the invention to provide a kind of
Muscone and method, and developed, using Phytochemistry means from Malania Oleifera Oil, mustard oil and macadimia nut oil
In prepare the diluted acid of carbon 15 first, further according to the consumption demand of different consumption, add other natural essential oils and active component, prepare
Natural cosmetics, natural perfume atmosphere series of products.The present invention is using the single-stranded aliphatic acid synthesis musk deer containing carbochain identical with muskone
Ketone musk, energy bottom line reduce muskone synthesis cost, the use of vegetable oil are raw material, natural environmental-protective, open the new of edible oil
Purposes, the application of edible oil is expanded, industrialization large-scale production and application can be used as.
For achieving the above object, the present invention is realized by following technical scheme:
Natural cosmetics containing plant source muskone, combined by weight percentage by following components:Ethanol
10-30 parts;Lavender 3-5 parts;Nerol 2-5 parts;Eucalyptus oil 2-8 parts;Archangelica officinalis Hoffmann lactone 1-2 parts;Cinnamic acid 1-2 parts;
Citronellal 1-2 parts;Plant source muskone 1-4 parts;Rose pure dew water 30-50 parts.
Wherein plant source muskone is prepared as follows:
The preparation of the diluted acid of carbon 15:
Using vegetable oil, the vegetable oil includes Malania Oleifera Oil, mustard oil, macadimia nut oil one kind therein, adds anhydrous
Ethanol is stirred, and the ratio of ethanol and vegetable oil is 3-5:1(V:V), it is stirring evenly and then adding into the 1-5mol/L of isometric ratio
NaOH fully stir evenly, carry out saponification, 50-60 DEG C of saponification temperature, heating water bath 4-6h, after question response is complete, filter, filter
The hydrochloric acid that liquid adds 1-5mol/L is neutralized, and when pH value is to 3-4, stops adding hydrochloric acid, stands 4-6h, the solidification of scraping upper strata
It is saponified, neutrality is washed to distillation, obtains fatty acid mixed, the fatty acid mixed is dissolved using absolute ethyl alcohol, places 4-5 DEG C
Refrigerator overnight, after band separates out crystallization completely, crystallization is filtered, obtains the diluted acid sterling of tetracosa carbon 15.
The preparation of plant source muskone:
Tetracosa carbon -15- diluted acids are subjected to ozonization under ice bath, KBH is then slowly added dropwise4Solution reduction, instead
After should terminating, it is acidified with dilute HCl, adjustment pH is 2-3, filtering, washs to neutrality, is dried in vacuo to obtain hydroxyl glyceride, reusing
Methanol and the 1-5mol/L concentrated sulfuric acid press 3-5:1(V:V) mixed solution of volume ratio is dissolved, under 80-90 DEG C of water-bath
Flowed back 2-3h, flows back 2-3 times, and filtering, filtrate is extracted with ether, and ether layer is washed with water to neutrality, pH6-7, Ran Houjin
Row is concentrated under reduced pressure, and thickening temperature is 50-60 DEG C, is concentrated into ether and volatilizes completely, obtains vegetable oil muskone.
The component of the present invention can add other natural essential oils and active component, prepare natural cosmetics, natural perfume atmosphere system
Row product.
The plant source Moschus one compositions contained in the present invention can be used for topical skin care composition.These compositions can be with
Make emulsifying agent (such as oil-in-water, Water-In-Oil, silicon Water-In-Oil, water bag silicone oil, W/O/W, Water-In-Oil bag oil, Water-In-Oil bag
Silicone oil etc.), creme, shin moisturizer, liquid (such as aqua or water-alcohol solution), anhydrous substrate (such as lipstick or pulvis etc.), Gel
Curry, ointment, milk, ointment, spray, solid formulation, eye cream etc..
Topical skin care compositions in the present invention include plant source muskone extract, and locally applying the extract can be to dry
Property skin, sensitive skin or skin itching or reduce the uneven outward appearance of the colour of skin and have preferable effect.
Embodiment:
Further illustrate the essentiality content of the present invention with embodiments of the invention below, but this is not limited with this
Invention.
Embodiment 1:
First prepare plant source muskone:
The preparation of the diluted acid of carbon 15:
Using vegetable oil, the vegetable oil includes Malania Oleifera Oil, mustard oil, a kind of macadimia nut oil 10.0kg therein, adds
Enter absolute ethyl alcohol to be stirred, the ratio of ethanol and vegetable oil is 3-5:1(V:V), it is stirring evenly and then adding into the 1- of isometric ratio
5mol/L NaOH is fully stirred evenly, progress saponification, 50-60 DEG C of saponification temperature, heating water bath 4-6h, after question response is complete,
Filtering, the hydrochloric acid that filtrate adds 1-5mol/L is neutralized, and when pH value is to 3-4, is stopped adding hydrochloric acid, is stood 4-6h, scraping
Upper strata solidification is saponified, is washed to neutrality with distillation, obtains fatty acid mixed, dissolves the fatty acid mixed using absolute ethyl alcohol,
4-5 DEG C of refrigerator overnight is placed, after band separates out crystallization completely, crystallization is filtered, obtains the diluted acid sterling of tetracosa carbon 15
2.5kg。
The preparation of plant source muskone:
Tetracosa carbon -15- diluted acids are subjected to ozonization under ice bath, KBH is then slowly added dropwise4Solution reduction, instead
After should terminating, it is acidified with dilute HCl, adjustment pH is 2-3, filtering, washs to neutrality, is dried in vacuo to obtain hydroxyl glyceride, reusing
Methanol and the 1-5mol/L concentrated sulfuric acid press 3-5:1(V:V) mixed solution of volume ratio is dissolved, under 80-90 DEG C of water-bath
Flowed back 2-3h, flows back 2-3 times, and filtering, filtrate is extracted with ether, and ether layer is washed with water to neutrality, pH6-7, Ran Houjin
Row is concentrated under reduced pressure, and thickening temperature is 50-60 DEG C, is concentrated into ether and volatilizes completely, obtains vegetable oil muskone 950g.
Then following components are taken by weight percentage:Ethanol 10-30 parts;Lavender 3-5 parts;Nerol 2-5 parts;Eucalyptus
Leaf oil 2-8 parts;Archangelica officinalis Hoffmann lactone 1-2 parts;Cinnamic acid 1-2 parts;Citronellal 1-2 parts;Plant source muskone 1-4 parts;Rose is pure
Dew 30-50 parts.Ethanol is pre-processed, 0.1-1mol/L NaOH is added and be heated to reflux 1-2h, ethanol and NaOH's
Ratio is 10-20:1(V:V/L:L), ethanol after purification is put into 0.1% eucalyptus oil, is used after placing 1 month in the cool.
Lavender, nerol, eucalyptus oil, Archangelica officinalis Hoffmann lactone, cinnamic acid, citronellal are dissolved in ethanol after purification in proportion
In, plant source muskone is eventually adding, is supplemented to rose wate enough.Sealed storage.It is made containing plant source muskone
Natural cosmetics
Embodiment 2:
Skin whitener formula (W%) containing plant source muskone:
The cosmetics of the above-mentioned formula of the present invention are made in the method for routinely making cosmetics.
Embodiment 3:
Emulsion formulations (W%) containing plant source muskone:
The cosmetics of the above-mentioned formula of the present invention are made in the method for routinely making cosmetics.
Embodiment 4:
Formula:
A oil phases w (mass percent)
Beeswax 2%, stearic acid 5%, octadecyl alcolol 3%, lanolin 2%, sorbester p17 3%, POLYSORBATE 80 3%, paraffin oil
3%.
B aqueous phases w (mass percent)
Glycerine 5%, plant source muskone 5%, triethanolamine 0.3%, distilled water 75%.
C essence is appropriate, propylben 0.2%
Method:
Oil phase is placed in thermostat water bath be heated with stirring to 90 DEG C be completely melt into it is homogeneous after, be slowly added to aqueous phase, after
Continuous stirring 30min;Slow cooling continues to stir to essence, propylben is added at 45 DEG C;Treat that temperature is down to 35 DEG C or so
When, stop stirring, stand, cooling, obtain newborn creamy product.
Foregoing explanation should be understood to only illustrate the present invention.Various selections and amendment can be by one skilled in the art
Designed without departing substantially from the present invention.Thus, it is intended that including all this selections fallen within the scope of the following claims and
Amendment and change.
Claims (2)
- A kind of 1. plant source Moschus cosmetics, it is characterised in that described plant source Moschus cosmetics be by following components by weight Percentage composition:Ethanol 10-30 parts, Lavender 3-5 parts, nerol 2-5 parts, eucalyptus oil 2-8 parts, Archangelica officinalis Hoffmann lactone 1- 2 parts, cinnamic acid 1-2 parts, citronellal 1-2 parts, plant source muskone 1-4 parts, rose pure dew water 30-50 parts.
- A kind of 2. plant source Moschus cosmetics according to claims 1, it is characterised in that wherein described plant source musk deer The preparation of ketone musk is carried out in the steps below:The preparation of the diluted acid of carbon 15:With vegetable oil Malania Oleifera Oil, mustard oil or macadimia nut oil, add absolute ethyl alcohol and stirred Mix, the ratio of ethanol and vegetable oil is 3-5:1V:V, the NaOH for being stirring evenly and then adding into the 1-5mol/L of isometric ratio are fully stirred It is even, saponification is carried out, 50-60 DEG C of saponification temperature, heating water bath 4-6h, after question response is complete, filtering, filtrate adds 1- 5mol/L hydrochloric acid is neutralized, and when pH value is to 3-4, stops adding hydrochloric acid, stands 4-6h, and the solidification of scraping upper strata is saponified, Neutrality is washed to distillation, obtains fatty acid mixed, the fatty acid mixed is dissolved using absolute ethyl alcohol, placed in 4-5 DEG C of refrigerator Overnight, after band separates out crystallization completely, crystallization is filtered, obtains the diluted acid sterling of tetracosa carbon 15;The preparation of plant source muskone:Tetracosa carbon -15- diluted acids obtained by above-mentioned steps are subjected to ozonization under ice bath, Then KBH is slowly added dropwise4Solution reduction, reaction terminate after, with dilute HCl be acidified, adjustment pH be 2-3, filtering, washing to neutrality, Hydroxyl glyceride is dried in vacuo to obtain, reuses methanol and the 1-5mol/L concentrated sulfuric acid by 3-5:1V:The mixed solution of V volume ratios enters Row dissolving, in the 2-3h that flowed back under 80-90 DEG C of water-bath, flow back 2-3 times, filtering, filtrate is extracted with ether, ether layer water Washing pH6-7, is then concentrated under reduced pressure, thickening temperature is 50-60 DEG C, is concentrated into ether and volatilizes completely, is planted to neutrality Thing oil muskone.
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1349988A (en) * | 2001-09-03 | 2002-05-22 | 广西大学 | Exaltolide preparing process from garlic oil |
CN105326704A (en) * | 2015-11-23 | 2016-02-17 | 梁秀萍 | Lavender essential oil floral water and preparation method thereof |
CN106397384A (en) * | 2016-08-30 | 2017-02-15 | 昆明酷特利生物科技有限公司 | Method for synthesis of macrocyclic musk lactone |
CN106397160A (en) * | 2016-08-30 | 2017-02-15 | 昆明酷特利生物科技有限公司 | Synthetic method for macrocyclic musk ketone |
-
2017
- 2017-08-04 CN CN201710658474.9A patent/CN107569411A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1349988A (en) * | 2001-09-03 | 2002-05-22 | 广西大学 | Exaltolide preparing process from garlic oil |
CN105326704A (en) * | 2015-11-23 | 2016-02-17 | 梁秀萍 | Lavender essential oil floral water and preparation method thereof |
CN106397384A (en) * | 2016-08-30 | 2017-02-15 | 昆明酷特利生物科技有限公司 | Method for synthesis of macrocyclic musk lactone |
CN106397160A (en) * | 2016-08-30 | 2017-02-15 | 昆明酷特利生物科技有限公司 | Synthetic method for macrocyclic musk ketone |
Non-Patent Citations (2)
Title |
---|
王文林等: "澳洲坚果脂肪酸成分分析", 《热带农业工程》 * |
赖芳等: "固体酸催化15_羟基十五烷酸酯合成环十五内酯", 《南京理工大学学报》 * |
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Application publication date: 20180112 |