CN107773600A - A kind of preparation method of acne compound - Google Patents
A kind of preparation method of acne compound Download PDFInfo
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- CN107773600A CN107773600A CN201610744384.7A CN201610744384A CN107773600A CN 107773600 A CN107773600 A CN 107773600A CN 201610744384 A CN201610744384 A CN 201610744384A CN 107773600 A CN107773600 A CN 107773600A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/74—Rubiaceae (Madder family)
- A61K36/748—Oldenlandia or Hedyotis
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/35—Caprifoliaceae (Honeysuckle family)
- A61K36/355—Lonicera (honeysuckle)
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/48—Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
- A61K36/483—Gleditsia (locust)
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/53—Lamiaceae or Labiatae (Mint family), e.g. thyme, rosemary or lavender
- A61K36/537—Salvia (sage)
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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- Health & Medical Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Epidemiology (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
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- Medicines Containing Material From Animals Or Micro-Organisms (AREA)
- Cosmetics (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a kind of preparation method of acne compound, belong to cosmetic skin field.It is as follows that it mixes Chinese medicinal component：15 40 parts of oldenlandia diffusa, 20 45 parts of caulis lonicerae, 20 40 parts of red sage root, 15 45 parts of fruitlet Chinese honey locust seed, it is extracted by alcohol reflux, filtering and impurity removing, the methods of being concentrated under reduced pressure and purifying prepare anti-acne compound.A kind of preparation method of acne compound provided by the invention, the method solvent can reclaim, do not produce waste water, cost is low, the active component of medicinal material is not damaged, product active ingredient that the method obtains is high, stably, safely, it is possible to reduce the formation of acne print and prevents the generation of acne after acne and acne, the defects of overcoming existing naturally bad, poor heat resistance of product for resolving poxes stability etc. in the market.
Description
Technical field
The present invention relates to cosmetic skin field, specifically a kind of preparation method of acne compound.
Background technology
Acne is a kind of chronic inflammation disease of puberty common pilosebaceous follicle, is a kind of common skin of clinic
Disease, be apt to occur in face, shirtfront and the back of puberty men and women, the principal pathogenetic age between 13-29 year, next to that in 20-29
Between year, acne lesions feature is mainly characterized by papule, warts, tubercle, tumour and a variety of infringements of scar.The patient of acne,
Particularly patient's Confidence of Medium or severe type is reduced, and quality of life reduces, and is presented with the table in terms of depressed and other abalienations
Existing, wherein in acne crowd, the scar that acne is formed accounts for teen-age 20%.
Due to the pollution of environment and the increase of life stress, the incidence of disease of China's whelk is in ascendant trend year by year, and 80%
More than people it is different degrees of encountered whelk problem, so anti-acne has the very big market demand.
Pathogenesis of acne complicated mechanism, mainly with androgen secretion, hair follicle conduit mouth hyperkeratinization, propionibacterium acnes it is big
Amount breeding and inflammation etc. are relevant.Secondly, as the factors such as inherent cause, some foods, medicine, cosmetics can influence, induce and
Aggravate the generation of acne.
At present to the treatment of acne, doctor suggests by based on oral tretinoin medicines and antibiotics, the course for the treatment of compared with
Long, side effect is larger, and curative effect is indefinite, so in the market urgent need safety, stabilization
Effectively, the anti-acne skin care item without any hormone, antibiotic.
The content of the invention
The invention aims to provide a kind of preparation method of acne compound, the method solvent can be reclaimed, do not produced
Raw waste water, cost is low, does not damage the active component of medicinal material, and the product active ingredient that the method obtains is high, stably, safely, can be with
The formation of acne print and the generation of prevention acne, overcome existing natural product for resolving poxes in the market after reduction acne and acne
The defects of stability is bad, poor heat resistance etc..
A kind of preparation method of acne compound of the present invention, comprises the following steps：
(1) the mixing medicinal material of oldenlandia diffusa, caulis lonicerae, red sage root and fruitlet Chinese honey locust seed is weighed, adds mixing medicinal material matter
The ethanol solution of 10-20 times of amount, 3h is extracted at 70-80 DEG C, is then filtered, filters out liquid；
(2) filtrate after step (1) is filtered adds flocculant, stirs to flocculate and continues to stir 20min after occurring, quiet
Filtered after putting 30min；
(3) filtrate after step (2) is filtered concentrates 1-5 hours at 40-70 DEG C, and filtrate adds water to gross mass and is after concentration
0.3-0.8 times of mixing quality of medicinal material；
(4) solvent is added, medicinal herb componentses are redissolved；
(5) filtrate is purified；
(6) sterilize, detection.
At least one of flocculant is in the step (2) lignin and chitosan.
The mass fraction of flocculant is 1-10% (w/w), mixing speed 30-100r/min in the step (2).
Pressure when being concentrated in the step (3) is 0.01-0.05Mpa, and the alcohol vapour being evaporated is after condensation
Recovery, return to step (1) use.
Solvent is at least one of butanediol, propane diols, glycerine, DPG in the step (4).
Purifying is realized by way of ultrafiltration in the step (5), the small active ingredient of purifying molecule amount.
The mass fraction of a component is oldenlandia diffusa in the mixing medicinal material：Caulis lonicerae：Red sage root：Fruitlet Chinese honey locust seed
=15-40 parts：20-45 parts：20-40 parts：15-45 parts.
It is of the invention to be had the following advantages compared with existing product for resolving poxes：
(1) the product for resolving poxes active ingredient that the present invention extracts is high, and good penetrability, impurity is few, is used alone just with notable
Anti-acne and reduce acne print the effect of, reached unlike many product for resolving poxes effects are weaker on the market, it is necessary to compound other product for resolving poxes
To acne-removing.
(2) solvent used in extraction process of the present invention can reclaim, and recycle, do not produce waste water.
(3) product for resolving poxes of the invention is directed to multiple target spots caused by acne, has suppression well to propionibacterium acnes
Make use, and suppress 5 alpha-reductases activity, reduce due to fat secretion excessively caused by acne.
(4) no matter equal under low temperature or hot conditions product for resolving poxes of the invention be in formula application aspect, easily addition
It can add, and stability is good, phenomena such as being not in discoloration and be layered.
Embodiment
Below in conjunction with specific example, present invention is described and explanation, in order to which the public is better understood from this
The technology contents of invention, rather than the limitation to the technology contents, under identical or approximate principle, to the processing step
The improvement of progress, including reaction condition, agents useful for same are improved and replaced, and reach identical purpose, then all in the present patent application institute
Within claimed technical scheme.
The preferred embodiments of the present invention are illustrated below, it will be appreciated that preferred embodiment described herein is only used
In the description and interpretation present invention, it is not intended to limit the present invention.
Embodiment 1
(1) the mixing medicine of 20 parts of 40 parts of oldenlandia diffusa, 20 parts of caulis lonicerae, 20 parts of red sage root and fruitlet Chinese honey locust seed is weighed
Material, the ethanol solution of 10 times of quality of medicinal material of mixing is added, 3h is extracted at 70 DEG C, filtered, filter out liquid.
(2) filtrate after step (1) is filtered adds flocculant, stirs to flocculate and continues to stir 20min after occurring, quiet
Filtered after putting 30min.
(3) filtrate after step (2) is filtered concentrates 2.5 hours at 60 DEG C, and it is 0.4 times that dense filtrate, which adds water to gross mass,
Mix quality of medicinal material.
(4) solvent is added, medicinal herb componentses are redissolved；
(5) filtrate is purified by milipore filter；
(6) sterilize, detection.
The lignin that flocculant is in the step (2).
The mass fraction of flocculant is 5% (w/w), mixing speed 80r/min in the step (2).
Pressure when being concentrated in the step (3) is 0.02Mpa, and the alcohol vapour being evaporated reclaims after condensation,
Return to step (1) uses.
Solvent is butanediol in the step (4).
Purifying is realized by way of ultrafiltration in the step (5), the small active ingredient of purifying molecule amount.
Embodiment 2
(1) the mixing medicine of 20 parts of 20 parts of oldenlandia diffusa, 40 parts of caulis lonicerae, 20 parts of red sage root and fruitlet Chinese honey locust seed is weighed
Material, 15 times of ethanol solutions are added, 3h is extracted at 76 DEG C, filtered, filter out liquid.
(2) filtrate after step (1) is filtered adds flocculant, stirs to flocculate and continues to stir 20min after occurring, quiet
Filtered after putting 30min.
(3) for the filtrate after step (2) is filtered in 60 DEG C of concentrations, dense filtrate adds water to the mixing medicine that gross mass is 0.5 times
Material amount.
(4) solvent is added, medicinal herb componentses are redissolved.
(5) filtrate is purified by milipore filter；
(6) sterilize, detection.
Flocculant is chitosan in the step (2).
The mass fraction of flocculant is 6% (w/w), mixing speed 90r/min in the step (2).
Pressure when being concentrated in the step (3) is 0.04Mpa, and the alcohol vapour being evaporated reclaims after condensation,
Return to step (1) uses.
Solvent is propane diols in the step (4).
Purifying is realized by way of ultrafiltration in the step (5), the small active ingredient of purifying molecule amount.
Embodiment 3
(1) the mixing medicine of 20 parts of 20 parts of oldenlandia diffusa, 20 parts of caulis lonicerae, 40 parts of red sage root and fruitlet Chinese honey locust seed is weighed
Material, 15 times of ethanol solutions are added, 3h is extracted at 80 DEG C, filtered, filter out liquid.
(2) filtrate after step (1) is filtered adds flocculant, stirs to flocculate and continues to stir 20min after occurring, quiet
Filtered after putting 30min.
(3) for the filtrate after step (2) is filtered in 60 DEG C of concentrations, dense filtrate adds water to the mixing medicine that gross mass is 0.4 times
Material amount.
(4) solvent is added, medicinal herb componentses are redissolved.
(5) filtrate is purified by milipore filter；
(6) sterilize, detection.
The lignin that flocculant is in the step (2).
The mass fraction of flocculant is 5% (w/w), mixing speed 80r/min in the step (2).
Pressure when being concentrated in the step (3) is 0.04Mpa, and the alcohol vapour being evaporated reclaims after condensation,
Return to step (1) uses.
Solvent is DPG in the step (4).
Purifying is realized by way of ultrafiltration in the step (5), the small active ingredient of purifying molecule amount.
Effect example
(1) minimum inhibitory concentration of the observation to propionibacterium acnes
1) embodiment anti-acne compound is diluted to propane diols 5% to 0.5% solubility, 0.5% is differed between concentration
Concentration.
2) test strain and culture medium：Propionibacterium acnes (ATCC6919).Propionibacterium acnes culture medium, regulation pH are
6.6~7.0.Agar 15g/L, 115 DEG C of 20min autoclavings are added wherein in solid medium.
3) measure of minimum inhibitory concentration (MIC value)：The μ of decoction 100 of the μ L of bacterium solution 100 and various concentrations is added in micropore
L, at the same set be not added with bacterium negative control and be not added with decoction normal growth control, every kind of medicine do 3 it is parallel, average.Put
37 DEG C of anaerobism are incubated, and result is observed after 48h.Using muddiness is visually determined whether, data are read using direct method.As a result judge
On condition that growth control is good, blank control asepsis growth is clear, other holes with drug concentration gradient raise and the growth of bacterium by
To suppression.
4) experimental result
The minimum inhibitory concentration (MIC value) of different embodiments
| Embodiment | Minimum inhibitory concentration (MIC value) |
| Embodiment 1 | 1.5% |
| Embodiment 2 | 2.0% |
| Embodiment 3 | 2.0% |
(2) the suppression effect of observation to 5α-reductase
1) embodiment anti-acne compound is diluted to propane diols 5% solubility.
2) when 5α-reductase catalysis testosterone (T) is converted into protona (DHT) reduced Coenzyme II (NADPH) is relied on to make
For hydrogen donor, NADPH has intense fluorescence in itself, after NADPH and reductase and substrate reactions, NADPH generation NADP+, and fluorescence
It is quenched therewith, therefore the activity of 5α-reductase can be investigated by fluorescence detector measure NADPH fluorescence intensity.
The orifice plate of black 96 is taken, adds the μ l of testosterone 5 (20 μm of ol/L), the μ l of enzyme extract 5, the μ l (1.3mM) of Finasteride 5 or time
The μ l of compound 20 (50 μM of final concentration) are selected, buffer solution (sucrose 0.73mol/L, calcium chloride 1.91mmol/L) is to 195 μ l, at 37 DEG C
Lower reaction 30min, the μ l (20mmol/L) of NADPH 5 are added, 1h is reacted at 37 DEG C, absorb light 340nm, transmitting light 495nm is surveyed
Determine fluorescence intensity.If the reaction tube for being not added with enzyme extract is blank control, if only enzyme-added extract but being not added with Finasteride and change
The reaction tube of compound is compareed for 100% enzymatic activity, and the percent inhibition of medicine is calculated by following equation：
Inhibiting rate=(blank tube average fluorescent strength-chemical combination property management average fluorescent strength)/(blank tube mean fluorecence is strong
Spend -100% enzymatic activity control fluorescence intensity) × 100
3) experimental result
Suppression effect to 5α-reductase of different embodiments
| Embodiment | Inhibiting rate |
| Embodiment 1 | 42.5% |
| Embodiment 2 | 46.5% |
| Embodiment 3 | 40.8% |
Finally illustrate, the above embodiments are merely illustrative of the technical solutions of the present invention and it is unrestricted, although with reference to compared with
The present invention is described in detail good embodiment, it will be understood by those of skill in the art that can be to the technical side of the present invention
Case is modified or equivalent substitution, and without departing from the objective and scope of technical solution of the present invention, it all should cover in the present invention
Right.
Claims (7)
1. a kind of preparation method of acne compound, it is characterised in that comprise the following steps：
(1) the mixing medicinal material of oldenlandia diffusa, caulis lonicerae, red sage root and fruitlet Chinese honey locust seed is weighed, adds mixing quality of medicinal material 10-
20 times of ethanol solution, 3h is extracted at 70-80 DEG C, is then filtered, filters out liquid；
(2) filtrate after step (1) is filtered adds flocculant, stirs to flocculate and continues to stir 20min after occurring, stands
Filtered after 30min；
(3) filtrate after step (2) is filtered concentrates 1-5 hours at 40-70 DEG C, and it is 0.3- that filtrate, which adds water to gross mass, after concentration
0.8 times of mixing quality of medicinal material；
(4) solvent is added, medicinal herb componentses are redissolved；
(5) filtrate is purified；
(6) sterilize, detection.
2. the preparation method of a kind of acne compound according to claim 1, it is characterised in that flocculated in the step (2)
At least one of lignin and chitosan that agent is.
3. the preparation method of a kind of acne compound according to claim 1, it is characterised in that flocculated in the step (2)
The mass fraction of agent is 1-10% (w/w), mixing speed 30-100r/min.
4. the preparation method of a kind of acne compound according to claim 1, it is characterised in that concentrated in the step (3)
When pressure be 0.01-0.05Mpa, the alcohol vapour being evaporated reclaims after condensation, return to step (1) use.
A kind of 5. preparation method of acne compound according to claim 1, it is characterised in that solvent in the step (4)
It is at least one of butanediol, propane diols, glycerine, DPG.
6. the preparation method of a kind of acne compound according to claim 1, it is characterised in that purified in the step (5)
It is to be realized by way of ultrafiltration, the small active ingredient of purifying molecule amount.
A kind of 7. preparation method of acne compound according to claim 1, it is characterised in that each group in the mixing medicinal material
The mass fraction divided is oldenlandia diffusa：Caulis lonicerae：Red sage root：Fruitlet Chinese honey locust seed=15-40 parts：20-45 parts：20-40 parts：
15-45 parts.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610744384.7A CN107773600A (en) | 2016-08-26 | 2016-08-26 | A kind of preparation method of acne compound |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610744384.7A CN107773600A (en) | 2016-08-26 | 2016-08-26 | A kind of preparation method of acne compound |
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| Publication Number | Publication Date |
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| CN107773600A true CN107773600A (en) | 2018-03-09 |
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| CN201610744384.7A Pending CN107773600A (en) | 2016-08-26 | 2016-08-26 | A kind of preparation method of acne compound |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108969429A (en) * | 2018-10-16 | 2018-12-11 | 广州科玛生物科技股份有限公司 | A kind of anti-acne essence |
| CN109157450A (en) * | 2018-10-16 | 2019-01-08 | 广州科玛生物科技股份有限公司 | A kind of anti-acne essence cream |
| CN109157451A (en) * | 2018-10-16 | 2019-01-08 | 广州科玛生物科技股份有限公司 | A kind of anti-acne mildy wash |
| CN109260075A (en) * | 2018-10-16 | 2019-01-25 | 广州科玛生物科技股份有限公司 | A kind of anti-acne opsonic water |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103393801A (en) * | 2013-07-31 | 2013-11-20 | 广州市娇兰化妆品有限公司 | Traditional Chinese medicine composite extract with effect of removing acnes, and preparation method and application thereof |
| CN105168478A (en) * | 2015-08-28 | 2015-12-23 | 无限极（中国）有限公司 | Skin care product and preparation method thereof |
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2016
- 2016-08-26 CN CN201610744384.7A patent/CN107773600A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103393801A (en) * | 2013-07-31 | 2013-11-20 | 广州市娇兰化妆品有限公司 | Traditional Chinese medicine composite extract with effect of removing acnes, and preparation method and application thereof |
| CN105168478A (en) * | 2015-08-28 | 2015-12-23 | 无限极（中国）有限公司 | Skin care product and preparation method thereof |
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| 李全林: "《现代生物工程》", 31 December 2008, 东南大学出版社 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108969429A (en) * | 2018-10-16 | 2018-12-11 | 广州科玛生物科技股份有限公司 | A kind of anti-acne essence |
| CN109157450A (en) * | 2018-10-16 | 2019-01-08 | 广州科玛生物科技股份有限公司 | A kind of anti-acne essence cream |
| CN109157451A (en) * | 2018-10-16 | 2019-01-08 | 广州科玛生物科技股份有限公司 | A kind of anti-acne mildy wash |
| CN109260075A (en) * | 2018-10-16 | 2019-01-25 | 广州科玛生物科技股份有限公司 | A kind of anti-acne opsonic water |
| CN109157450B (en) * | 2018-10-16 | 2021-06-15 | 广州科玛生物科技股份有限公司 | Acne-removing essence |
| CN108969429B (en) * | 2018-10-16 | 2021-06-15 | 广州科玛生物科技股份有限公司 | Acne removing essence |
| CN109260075B (en) * | 2018-10-16 | 2021-06-15 | 广州科玛生物科技股份有限公司 | Acne-removing conditioning water |
| CN109157451B (en) * | 2018-10-16 | 2021-06-15 | 广州科玛生物科技股份有限公司 | Acne-removing facial cleanser |
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Application publication date: 20180309 |