CN110483655A - A kind of Polysaccharide from Portulaca oleracea extraction process and its application in skin care item - Google Patents
A kind of Polysaccharide from Portulaca oleracea extraction process and its application in skin care item Download PDFInfo
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- CN110483655A CN110483655A CN201910812429.3A CN201910812429A CN110483655A CN 110483655 A CN110483655 A CN 110483655A CN 201910812429 A CN201910812429 A CN 201910812429A CN 110483655 A CN110483655 A CN 110483655A
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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
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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Abstract
The present invention relates to a kind of Polysaccharide from Portulaca oleracea extraction process and its applications in skin care item, comprising the following steps: crushes after D1 freeze-drying;D2 decoloration removes impurity;The extraction of D3 low temperature;D4 deproteinization;D5 purification: gained upper layer polysaccharide solution in D6 being concentrated into close to saturation, alcohol precipitation, static layering, centrifugation, washing are carried out, and then after vacuum or freeze-drying, obtains Polysaccharide from Portulaca oleracea.The extracting method of Polysaccharide from Portulaca oleracea in the present invention, using freeze-drying repeatedly, cell wall is punctured using the ice crystal in purslane in refrigerating process, completely release polysaccharide component, extraction conducive to deionized water in a low temperature of the later period to polysaccharide, recovery rate is improved, and in whole process, without high temperature, toxic solvent, the activity of purslane extract is maintained to greatest extent, together with the skin care substance good with other moistening effects, it is applied to skin-protection product, better effect can be obtained.
Description
Technical field
The present invention relates to Polysaccharide from Portulaca oleracea extraction process technology field, and in particular to a kind of Polysaccharide from Portulaca oleracea extraction process and its
Application in skin care item.
Background technique
Purslane has effects that clearing heat and detoxicating and scattered blood detumescence, and full of nutrition, herb contains methylepinephrine, tonka-bean
Essence, flavones and cardiac glycoside, polysaccharide and vitamin, purslane Thick many candies have the function of that anti-hydroxy radical and oxygen radical are dual
Effect, be in dose-dependence, research find purslane to grease have certain antioxygenic property, greasy skin with promotion on
The physiological function of chrotoplast tends to normally act on, it is possible to reduce because of the production of dead skin and cuticula caused by drying, prevents the winter
Season pruitus, be mainly used for the various stimulations of antiallergy, anti-inflammatory anti-inflammatory and anti-outer bound pair skin, there are also acne-removal function,
Especially there are apparent anti-allergic effects to the skin allergy that the generation of steroids cosmetics is used for a long time.
Summary of the invention
To overcome the deficiency, the purpose of the present invention is to provide a kind of Polysaccharide from Portulaca oleracea extraction process and its in skin care item
In application.
The technical solution adopted by the present invention to solve the technical problems is: a kind of Polysaccharide from Portulaca oleracea extraction process, including with
Lower step:
It is crushed after D1 freeze-drying: clean disease-free fresh purslane, or dry purslane being selected to be immersed in water
In at least 2 hours or more rehydrations, the purslane after fresh purslane or rehydration is put into refrigerator and is freezed, molding to be frozen
Afterwards, it is put into freeze dryer, is freeze-dried, then rehydration after freeze-drying is freeze-dried at least 3 times, again by finally dried horse
Bitterroot is ground into purslane powder, and powder particle size is in 60-100 mesh;
D2 decoloration removes impurity: by purslane powder more in step D1, with 70%wt-100%wt ethyl alcohol in a water bath into
Row refluxing extraction 2-4 times, bath temperature are 20-30 DEG C, reflux extracting time 1-2h, and purslane residue is stayed in filtering, remove institute
The small molecular weight impurities such as the monosaccharide, glycoside, polyphenol, fat, the pigment that contain;
The extraction of D3 low temperature: the purslane residue in step D2 is added in deionized water and carries out low temperature extraction 24-48h, material
Liquor ratio is 10-30g/mL, and temperature is 20-30 DEG C, and centrifugation obtains Polysaccharide from Portulaca oleracea leaching liquor and insoluble purslane residue;
D4 deproteinization: by Polysaccharide from Portulaca oleracea leaching liquor obtained in step D3 through micro-filtration, reduced pressure, micro-filtration micro-filtration mistake
Journey is that Polysaccharide from Portulaca oleracea leaching liquor is successively passed through to the filter-cloth filtering of 200 mesh, 400 mesh, then passes through 0.1 to 1 μm of microstrainer
It is filtered, is then concentrated under reduced pressure into the 3/10 of original volume, sevage reagent is added in concentrate, and (chloroform: n-butanol volume ratio is
5:1), additional amount is the 1/4-3/4 of concentrate, is sufficiently stirred, static layering, removes isolating protein, repetitive operation at least 3 times, receives
Collect upper layer polysaccharide solution;
D5 purification: gained upper layer polysaccharide solution in D6 is concentrated into close to saturation, the concentration of upper layer polysaccharide solution is added
2-5 times of ethyl alcohol of volume afterwards, carries out alcohol precipitation, and the concentration of ethyl alcohol is 95%-100%wt, static layering, 8000r/min centrifugation
10min, with 100%wt ethanol washing at least 2 times, then vacuum or freeze-drying after, obtain Polysaccharide from Portulaca oleracea.
Specifically, in the step D3, in low temperature leaching process, ultrasonic-leaching 10min is at least divided into 2 completions.
A kind of Polysaccharide from Portulaca oleracea extracts the application in skin care item, using the Polysaccharide from Portulaca oleracea of above method preparation in skin care
The application of kind.
The invention has the following advantages: in the present invention Polysaccharide from Portulaca oleracea extracting method, it is dry to use freezing repeatedly
Dry method punctures cell wall using the ice crystal in purslane in refrigerating process, and in reconstitution process, and par-tial polysaccharide is precipitated, freezing
In drying process, only water sublimate, polysaccharide component are stayed in dry purslane residue, completely release polysaccharide component, after being conducive to
Extraction of the deionized water to polysaccharide in a low temperature of phase, improves recovery rate, and in whole process, without high temperature, toxic solvent, most
The activity for maintaining purslane extract of limits together with the skin care substance good with other moistening effects, is applied to skin care and produces
Product can obtain better effect.
Specific embodiment
The present invention is described in further detail now.
Embodiment 1
A kind of Polysaccharide from Portulaca oleracea extraction process, comprising the following steps:
It is crushed after D1 freeze-drying: clean disease-free fresh purslane, or dry purslane being selected to be immersed in water
In at least 2 hours or more rehydrations, the purslane after fresh purslane or rehydration is put into refrigerator and is freezed, molding to be frozen
Afterwards, it is put into freeze dryer, is freeze-dried, then rehydration after freeze-drying is freeze-dried at least 3 times, again by finally dried horse
Bitterroot is ground into purslane powder, and powder particle size is in 60-100 mesh;
D2 decoloration removes impurity: purslane powder 100g more in step D1 is returned in a water bath with 70%wt ethyl alcohol
Stream extracts 3 times, and bath temperature is 20-30 DEG C, reflux extracting time 1h, and purslane residue is stayed in filtering, removes contained list
The small molecular weight impurities such as sugar, glycoside, polyphenol, fat, pigment;
The extraction of D3 low temperature ultrasonic: the purslane residue in step D2 being added in deionized water and carries out low temperature extraction for 24 hours, temperature
Degree is 20-30 DEG C, and 4000r/min is centrifuged 10min, obtains Polysaccharide from Portulaca oleracea leaching liquor and insoluble purslane residue;
D4 deproteinization: by Polysaccharide from Portulaca oleracea leaching liquor obtained in step D3 through micro-filtration, reduced pressure, micro-filtration micro-filtration mistake
Journey is that Polysaccharide from Portulaca oleracea leaching liquor is successively passed through to the filter-cloth filtering of 200 mesh, 400 mesh, then passes through 0.1 to 1 μm of microstrainer
It is filtered, is then concentrated under reduced pressure into the 3/10 of original volume, sevage reagent is added in concentrate, and (chloroform: n-butanol volume ratio is
5:1), additional amount is the 1/4 of concentrate, is sufficiently stirred, static layering, removes isolating protein, repetitive operation at least 3 times, in collection
Layer polysaccharide solution;
D5 purification: gained upper layer polysaccharide solution in D6 is concentrated into close to saturation, the concentration of upper layer polysaccharide solution is added
5 times of ethyl alcohol of volume afterwards, carry out alcohol precipitation, and the concentration of ethyl alcohol is 95%wt, static layering, 8000r/min centrifugation 10min, use
100%wt ethanol washing at least 2 times, then vacuum or freeze-drying after, obtain Polysaccharide from Portulaca oleracea 14.5g, account for dry horse
The 14.5% of bitterroot weight, after sulfuric acid-phynol method measures, measuring polyoses content is 97.1%.
A kind of application of Polysaccharide from Portulaca oleracea in skin care item, Polysaccharide from Portulaca oleracea have antioxygenic property, greasy skin and rush
Physiological function into epithelial cell tends to normally act on, it is possible to reduce because of the production of dead skin and cuticula caused by drying, prevents
Only skin pruritus in winter is mainly used for the various stimulations of antiallergy, anti-inflammatory anti-inflammatory and anti-outer bound pair skin, with moisture-keeping function
It is used after preferable skin care item, such as extract solution from aloe, tremella extract material mixing, there is more preferably effect.
Embodiment 2
A kind of Polysaccharide from Portulaca oleracea extraction process, comprising the following steps:
It is crushed after D1 freeze-drying: clean disease-free fresh purslane, or dry purslane being selected to be immersed in water
In at least 2 hours or more rehydrations, the purslane after fresh purslane or rehydration is put into refrigerator and is freezed, molding to be frozen
Afterwards, it is put into freeze dryer, is freeze-dried, then rehydration after freeze-drying is freeze-dried at least 3 times, again by finally dried horse
Bitterroot is ground into purslane powder, and powder particle size is in 60-100 mesh;
D2 decoloration removes impurity: purslane powder 100g more in step D1 is returned in a water bath with 80%wt ethyl alcohol
Stream extracts 2 times, and bath temperature is 20-30 DEG C, reflux extracting time 1.5h, and purslane residue is stayed in filtering, removes contained list
The small molecular weight impurities such as sugar, glycoside, polyphenol, fat, pigment;
The extraction of D3 low temperature ultrasonic: the purslane residue in step D2 is added in deionized water and carries out low temperature extraction 30h, temperature
Degree is 20-30 DEG C, and 4000r/min is centrifuged 10min, obtains Polysaccharide from Portulaca oleracea leaching liquor and insoluble purslane residue;
D4 deproteinization: by Polysaccharide from Portulaca oleracea leaching liquor obtained in step D3 through micro-filtration, reduced pressure, micro-filtration micro-filtration mistake
Journey is that Polysaccharide from Portulaca oleracea leaching liquor is successively passed through to the filter-cloth filtering of 200 mesh, 400 mesh, then passes through 0.1 to 1 μm of microstrainer
It is filtered, is then concentrated under reduced pressure into the 3/10 of original volume, sevage reagent is added in concentrate, and (chloroform: n-butanol volume ratio is
5:1), additional amount is the 1/2 of concentrate, is sufficiently stirred, static layering, removes isolating protein, repetitive operation at least 3 times, in collection
Layer polysaccharide solution;
D5 purification: gained upper layer polysaccharide solution in D6 is concentrated into close to saturation, the concentration of upper layer polysaccharide solution is added
4 times of ethyl alcohol of volume afterwards, carry out alcohol precipitation, and the concentration of ethyl alcohol is 98%wt, static layering, 8000r/min centrifugation 10min, use
100%wt ethanol washing at least 2 times, then vacuum or freeze-drying after, obtain Polysaccharide from Portulaca oleracea 13.1g, account for dry horse
The 13.1% of bitterroot weight, after sulfuric acid-phynol method measures, measuring polyoses content is 96.8%.
A kind of application of Polysaccharide from Portulaca oleracea in skin care item, Polysaccharide from Portulaca oleracea have antioxygenic property, greasy skin and rush
Physiological function into epithelial cell tends to normally act on, it is possible to reduce because of the production of dead skin and cuticula caused by drying, prevents
Only skin pruritus in winter is mainly used for the various stimulations of antiallergy, anti-inflammatory anti-inflammatory and anti-outer bound pair skin, with moisture-keeping function
It is used after preferable skin care item, such as extract solution from aloe, tremella extract material mixing, there is more preferably effect.
Embodiment 3
A kind of Polysaccharide from Portulaca oleracea extraction process, comprising the following steps:
It is crushed after D1 freeze-drying: clean disease-free fresh purslane, or dry purslane being selected to be immersed in water
In at least 2 hours or more rehydrations, the purslane after fresh purslane or rehydration is put into refrigerator and is freezed, molding to be frozen
Afterwards, it is put into freeze dryer, is freeze-dried, then rehydration after freeze-drying is freeze-dried at least 3 times, again by finally dried horse
Bitterroot is ground into purslane powder, and powder particle size is in 60-100 mesh;
D2 decoloration removes impurity: purslane powder 100g more in step D1 is returned in a water bath with 90%wt ethyl alcohol
Stream extracts 4 times, and bath temperature is 20-30 DEG C, reflux extracting time 2h, and purslane residue is stayed in filtering, removes contained list
The small molecular weight impurities such as sugar, glycoside, polyphenol, fat, pigment;
The extraction of D3 low temperature ultrasonic: the purslane residue in step D2 is added in deionized water and carries out low temperature extraction 36h, temperature
Degree is 20-30 DEG C, and 4000r/min is centrifuged 10min, obtains Polysaccharide from Portulaca oleracea leaching liquor and insoluble purslane residue;
D4 deproteinization: by Polysaccharide from Portulaca oleracea leaching liquor obtained in step D3 through micro-filtration, reduced pressure, micro-filtration micro-filtration mistake
Journey is that Polysaccharide from Portulaca oleracea leaching liquor is successively passed through to the filter-cloth filtering of 200 mesh, 400 mesh, then passes through 0.1 to 1 μm of microstrainer
It is filtered, is then concentrated under reduced pressure into the 3/10 of original volume, sevage reagent is added in concentrate, and (chloroform: n-butanol volume ratio is
5:1), additional amount is the 3/4 of concentrate, is sufficiently stirred, static layering, removes isolating protein, repetitive operation at least 3 times, in collection
Layer polysaccharide solution;
D5 purification: gained upper layer polysaccharide solution in D6 is concentrated into close to saturation, the concentration of upper layer polysaccharide solution is added
3 times of ethyl alcohol of volume afterwards, carry out alcohol precipitation, and the concentration of ethyl alcohol is 100%wt, static layering, 8000r/min centrifugation 10min, use
100%wt ethanol washing at least 2 times, then vacuum or freeze-drying after, obtain Polysaccharide from Portulaca oleracea 14.8g, account for dry horse
The 14.8% of bitterroot weight, after sulfuric acid-phynol method measures, measuring polyoses content is 97.7%.
A kind of application of Polysaccharide from Portulaca oleracea in skin care item, Polysaccharide from Portulaca oleracea have antioxygenic property, greasy skin and rush
Physiological function into epithelial cell tends to normally act on, it is possible to reduce because of the production of dead skin and cuticula caused by drying, prevents
Only skin pruritus in winter is mainly used for the various stimulations of antiallergy, anti-inflammatory anti-inflammatory and anti-outer bound pair skin, with moisture-keeping function
It is used after preferable skin care item, such as extract solution from aloe, tremella extract material mixing, there is more preferably effect.
Embodiment 4
A kind of Polysaccharide from Portulaca oleracea extraction process, comprising the following steps:
It is crushed after D1 freeze-drying: clean disease-free fresh purslane, or dry purslane being selected to be immersed in water
In at least 2 hours or more rehydrations, the purslane after fresh purslane or rehydration is put into refrigerator and is freezed, molding to be frozen
Afterwards, it is put into freeze dryer, is freeze-dried, then rehydration after freeze-drying is freeze-dried at least 3 times, again by finally dried horse
Bitterroot is ground into purslane powder, and powder particle size is in 60-100 mesh;
D2 decoloration removes impurity: purslane powder 100g more in step D1 is returned in a water bath with 100%wt ethyl alcohol
Stream extracts 4 times, and bath temperature is 20-30 DEG C, reflux extracting time 1.5h, and purslane residue is stayed in filtering, removes contained list
The small molecular weight impurities such as sugar, glycoside, polyphenol, fat, pigment;
The extraction of D3 low temperature ultrasonic: the purslane residue in step D2 is added in deionized water and carries out low temperature extraction 48h, temperature
Degree is 20-30 DEG C, and 4000r/min is centrifuged 10min, obtains Polysaccharide from Portulaca oleracea leaching liquor and insoluble purslane residue;
D4 deproteinization: by Polysaccharide from Portulaca oleracea leaching liquor obtained in step D3 through micro-filtration, reduced pressure, micro-filtration micro-filtration mistake
Journey is that Polysaccharide from Portulaca oleracea leaching liquor is successively passed through to the filter-cloth filtering of 200 mesh, 400 mesh, then passes through 0.1 to 1 μm of microstrainer
It is filtered, is then concentrated under reduced pressure into the 3/10 of original volume, sevage reagent is added in concentrate, and (chloroform: n-butanol volume ratio is
5:1), additional amount is the 3/4 of concentrate, is sufficiently stirred, static layering, removes isolating protein, repetitive operation at least 3 times, in collection
Layer polysaccharide solution;
D5 purification: gained upper layer polysaccharide solution in D6 is concentrated into close to saturation, the concentration of upper layer polysaccharide solution is added
2 times of ethyl alcohol of volume afterwards, carry out alcohol precipitation, and the concentration of ethyl alcohol is 100%wt, static layering, 8000r/min centrifugation 10min, use
100%wt ethanol washing at least 2 times, then vacuum or freeze-drying after, obtain Polysaccharide from Portulaca oleracea 13.9g, account for dry horse
The 13.9% of bitterroot weight, after sulfuric acid-phynol method measures, measuring polyoses content is 98.1%.
A kind of application of Polysaccharide from Portulaca oleracea in skin care item, Polysaccharide from Portulaca oleracea have antioxygenic property, greasy skin and rush
Physiological function into epithelial cell tends to normally act on, it is possible to reduce because of the production of dead skin and cuticula caused by drying, prevents
Only skin pruritus in winter is mainly used for the various stimulations of antiallergy, anti-inflammatory anti-inflammatory and anti-outer bound pair skin, with moisture-keeping function
It is used after preferable skin care item, such as extract solution from aloe, tremella extract material mixing, there is more preferably effect.
The present invention is not limited to the embodiment, anyone should learn that the structure made under the inspiration of the present invention becomes
Change, the technical schemes that are same or similar to the present invention are fallen within the scope of protection of the present invention.
Technology not described in detail in the present invention, shape, construction portion are well-known technique.
Claims (8)
1. a kind of Polysaccharide from Portulaca oleracea extraction process, it is characterised in that: the following steps are included:
It is crushed after D1 freeze-drying: clean disease-free fresh purslane, or dry purslane being selected to impregnate in water extremely
Then few 2 hours or more rehydrations, freeze-drying, rehydration after freeze-drying are freeze-dried at least 3 times, again by finally dried horse
Bitterroot is ground into purslane powder;
D2 decoloration removes impurity: purslane powder more in step D1 filters after carrying out refluxing extraction in a water bath with 7 ethyl alcohol,
Stay purslane residue;
The extraction of D3 low temperature: the purslane residue in step D2 being added in deionized water and carries out low temperature extraction, and centrifugation obtains dent
Amaranth polysaccharide leaching liquor and insoluble purslane residue;
D4 deproteinization: by Polysaccharide from Portulaca oleracea leaching liquor obtained in step D3 through micro-filtration, reduced pressure, concentrate is added
Sevage reagent, additional amount are the 1/4-3/4 of concentrate, are sufficiently stirred, static layering, go isolating protein, repetitive operation at least 3
It is secondary, collect upper layer polysaccharide solution;
D5 purification: gained upper layer polysaccharide solution in D6 is concentrated into close to saturation, body after the concentration of upper layer polysaccharide solution is added
2-5 times of long-pending ethyl alcohol, carry out alcohol precipitation, static layering, centrifugation, washing, then vacuum or freeze-drying after, it is more to obtain purslane
Sugar.
2. a kind of Polysaccharide from Portulaca oleracea extraction process according to claim 1, it is characterised in that: in the step D1, dent
Amaranth powder particle size is in 60-100 mesh.
3. a kind of Polysaccharide from Portulaca oleracea extraction process according to claim 1, it is characterised in that: the parameter of alcohol reflux are as follows:
It is carried out in a water bath refluxing extraction 2-4 times with 70%wt-100%wt ethyl alcohol, bath temperature is 20-30 DEG C, reflux extracting time
For 1-2h.
4. a kind of Polysaccharide from Portulaca oleracea extraction process according to claim 1, it is characterised in that: in the step D3, low temperature
In leaching process, ultrasonic-leaching 10min is at least divided into 2 completions.
5. a kind of Polysaccharide from Portulaca oleracea extraction process according to claim 1, it is characterised in that: low temperature soaks in the step D3
24-48h, solid-liquid ratio 10-30g/mL are mentioned, temperature is 20-30 DEG C.
6. a kind of Polysaccharide from Portulaca oleracea extraction process according to claim 1, it is characterised in that: micro-filtration mistake in the step D4
Journey is that Polysaccharide from Portulaca oleracea leaching liquor is successively passed through to the filter-cloth filtering of 200 mesh, 400 mesh, then passes through 0.1 to 1 μm of microstrainer
It is filtered, is then concentrated under reduced pressure into the 3/10 of original volume.
7. a kind of Polysaccharide from Portulaca oleracea extraction process according to claim 1, it is characterised in that: alcohol precipitation is adopted in the step D5
The concentration of ethyl alcohol is 95%-100%wt, parameter of noncentricity are as follows: 8000r/min is centrifuged 10min, with 100%wt ethanol washing
At least 2 times.
8. a kind of Polysaccharide from Portulaca oleracea extracts the application in skin care item, it is characterised in that: utilize any one of claim 1-7 work
Application of the Polysaccharide from Portulaca oleracea made from skill in skin care kind.
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CN111602728A (en) * | 2020-06-17 | 2020-09-01 | 中国海洋大学 | Preparation process of tea cake rich in tea polysaccharide |
CN111803400A (en) * | 2020-08-18 | 2020-10-23 | 黑龙江中医药大学 | Traditional Chinese medicine polysaccharide moisturizing and freckle removing mask and preparation method thereof |
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