CN108659141A - The extracting method of its anesthesia stem polysaccharide and application - Google Patents
The extracting method of its anesthesia stem polysaccharide and application Download PDFInfo
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- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
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- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
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Abstract
The present invention provides the extracting method of day anesthesia stem polysaccharide and applications.The extracting method of anesthesia stem polysaccharide in day of the present invention, includes the following steps：After the pretreatment of its anesthesia stem, add water refluxing extraction, after separation of solid and liquid, filtrate and filter residue is separately recovered；Filter residue carries out repeating extraction under the same conditions, is concentrated after filtrate is merged, then alcohol precipitation at low temperature, dry after separation of solid and liquid, obtains a day anesthesia stem polysaccharide；The day anesthesia stem pre-processes：By day anesthesia stem crushed after being dried, then it is sieved.The method and process step of gastrodia elata polysaccharide extraction of the present invention is easy, and abundant, effective extraction can be realized to polysaccharose substance in day anesthesia stem；Meanwhile by the adjustment and optimization for extraction conditions, also improving the polyoses content in extract crude product.
Description
Technical field
The present invention relates to field of plant extraction, the extracting method in particular to day anesthesia stem polysaccharide and application.
Background technology
Rhizoma Gastrodiae (Gastrodia elata Blume.) first of Guizhou Province " ten big authentic medicinal herbs " and is put into Guizhou Province's weight
One of " the eight big industrial chains " of point cultivation and development, is the rhizome of orchid family herbaceos perennial Rhizoma Gastrodiae, is divided into winter fiber crops, spring fiber crops, winter
Numb is superior in quality, and spring fiber crops take second place, and Rhizoma Gastrodiae is also referred to as " rhizoma gastrodiae, solely shakes sesame at wind grass " etc., is distributed in Yunnan Province of China, Guizhou, four
The ground such as river, Hunan, Hubei are grown under 400-3200 meters of sparse woods of height above sea level, shrubbery edge.Wherein Eastern Yunnan, WESTERN GUIZHOU, four
It is famous authentic medicinal herbs that river south, which is produced,.
Rhizoma Gastrodiae has long medicinal history, is traditional rare Chinese medicine, medicinal to be initially published in《Sheng Nong's herbal classic》：Taste
Pungent-warm.Pharmacological experiments show：Rhizoma Gastrodiae is relieved pain with ceases wind, calm, anticonvulsion, anti-epileptic, antirheumatic, improves study note
Recall, strengthen immunity, the effect of cardiovascular and cerebrovascular and neuroprotection etc., at this stage, is applied to clinical treatment mainly with day
The rhizome portion of fiber crops is divided into medicine energy relieving convulsion and soothing the liver, and treatment intermittent headache, the diseases such as headache
Rhizoma Gastrodiae underground stem tuber main chemical compositions include phenols and its " glycoside, polysaccharide, organic acid and its esters ", amino acid
Deng wherein Gastrodin is the main component and active constituent of Rhizoma Gastrodiae.And gastrodia elata polysaccharide has following effect：Remove free radical, drop blood
Pressure, immunological regulation, replenishing water and preserving moisture and bacteriostasis, gastrodia elata polysaccharide have a variety of physiological activity to cytotoxic side effect,
Contain a large amount of hydrophilic hydroxyl groups in its structure, with good film forming characteristics and shows the characteristic of moisture absorption, moisturizing, often make
" cosmetics magistery ".
However, gastrodia elata polysaccharide mostly is extracted to obtain by Rhizoma Gastrodiae rhizome at present, this is not only restricted its raw material sources, and
And for day anesthesia stem the like waste, also it is not carried out effective recycling of resource.
In view of this, special propose the present invention.
Invention content
The first object of the present invention is to provide the extracting method of a kind of day anesthesia stem polysaccharide, in the extracting method,
Gastrodia elata polysaccharide extraction is carried out by raw material of day anesthesia stem, not only expands the raw material sources range of gastrodia elata polysaccharide, while but also
Its anesthesia stem is fully used.
The second object of the present invention is to provide one kind by the obtained gastrodia elata polysaccharide of extracting method of the present invention.
The third object of the present invention is to provide a kind of application of gastrodia elata polysaccharide of the present invention.
The fourth object of the present invention is to provide a kind of using gastrodia elata polysaccharide of the present invention as the skin care item prepared by raw material.
In order to realize that the above-mentioned purpose of the present invention, spy use following technical scheme：
The extracting method of a kind of day anesthesia stem polysaccharide, includes the following steps：After the pretreatment of its anesthesia stem, water reflux is added to carry
It takes, after separation of solid and liquid, filtrate and filter residue is separately recovered；Filter residue carries out repeating extraction under the same conditions, dense after filtrate is merged
Contracting, then alcohol precipitation at low temperature is dry after separation of solid and liquid, obtains a day anesthesia stem polysaccharide；Preferably, the day anesthesia stem pretreatment
Including：By day anesthesia stem crushed after being dried, then it is sieved.
Preferably, in the extracting method of anesthesia stem polysaccharide in day of the present invention, the quality grams of pretreated Rhizoma Gastrodiae
It is 1 with the ratio between the volume ml of added water：(20~60)；It is furthermore preferred that the quality grams of pretreated Rhizoma Gastrodiae with it is added
The ratio between volume ml of water is 1：(30~50)；It is further preferred that the quality grams of pretreated Rhizoma Gastrodiae and added water
The ratio between volume ml be 1：40.
Preferably, in the extracting method of anesthesia stem polysaccharide in day of the present invention, the temperature of refluxing extraction is 60~80 DEG C；
It is furthermore preferred that the temperature of refluxing extraction is 70~80 DEG C；It is further preferred that the temperature of refluxing extraction is 70 DEG C.
Preferably, in the extracting method of anesthesia stem polysaccharide in day of the present invention, the time of refluxing extraction is 1~3h；More
Preferably, the time of refluxing extraction is 2~3h；It is further preferred that the time of refluxing extraction is 2h.
Meanwhile the present invention also provides the gastrodia elata polysaccharides obtained by extracting method of the present invention.
Likewise, the application present invention provides the day anesthesia stem polysaccharide in preparing skin care item.
Further, the present invention also provides a kind of skin care item, which is characterized in that the raw material of the skin cream includes this hair
The bright gastrodia elata polysaccharide.
Preferably, the raw material of skin care item of the present invention still further comprises：Vaseline, atoleine, Arlacel-60,
Octadecyl alcolol, hexadecanol, glycerine, lanolin, Tween-80, propylene glycol, 2,6-di-tert-butyl p-cresol, Rosa Damascana, and go from
It is one or more in son.
Preferably, in parts by weight, in skin care item of the present invention, each raw material dosage is as follows：Gastrodia elata polysaccharide 0.1~
0.2 part, 1~2 part of vaseline, 4~6 parts of atoleine, 1~2 part of Arlacel-60,2~3 parts of octadecyl alcolol, 1~2 part of hexadecanol is sweet
1~2 part of oil, 1~2 part of lanolin, 1~2 part of Tween-80,1~2 part of propylene glycol, 2,6-di-tert-butyl p-cresol 0.005~
0.0008 part, 30~55 parts of 0.01~0.02 part of Rosa Damascana and water.
Likewise, the present invention also provides the preparation methods of the skin care item, including：By vaseline, atoleine, department
It is dissolved by heating after disk -60, octadecyl alcolol, hexadecanol, glycerine, 2,6-di-tert-butyl p-cresol and lanolin mixing, obtains oil
Phase；Gastrodia elata polysaccharide, Tween-80, propylene glycol and Rosa Damascana are added to the water dissolving heating and obtain water phase；Then, it is stirring
Under the conditions of, during the oil phase is added to the aqueous phase, obtain skin care item.
Compared with prior art, beneficial effects of the present invention are：
(1) the method and process step of gastrodia elata polysaccharide extraction of the present invention is easy, and can be to polysaccharide object in day anesthesia stem
Matter, which is realized, fully, effectively to be extracted；
Meanwhile by the adjustment and optimization for extraction conditions, also improving the polyoses content in extract crude product；
(2) it in the present invention, by the adjustment for skin care item mesostroma class raw material dosage, also effectively improves prepared
The sense organ and physicochemical property of skin care item comply with country and professional standard, meet actual use needs.
Description of the drawings
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technology description to be briefly described.
Fig. 1 is specific embodiment of the invention glucose standard curve figure.
Specific implementation mode
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.It is not specified in embodiment specific
Condition person carries out according to conventional conditions or manufacturer's recommended conditions.Reagents or instruments used without specified manufacturer is
The conventional products that can be obtained by commercially available purchase.
Gastrodia elata polysaccharide is the Rhizoma Gastrodiae active ingredient for being only second to Gastrodin, however, gastrodia elata polysaccharide raw material sources are in Rhizoma Gastrodiae at present
Stem tuber, extraction cost is relatively high, causes the research that gastrodia elata polysaccharide is applied in cosmetic field actually rare, in view of this, this
Invention has provided a kind of method that the waste day anesthesia stem generated in being planted using Rhizoma Gastrodiae carries out gastrodia elata polysaccharide extraction as raw material,
The problems of in the prior art with solution.
Specifically, the present invention by day anesthesia stem carry out gastrodia elata polysaccharide extraction method can refer to it is as follows：
(preferably dry 4h under the conditions of 60 DEG C) is dried in raw material day anesthesia stem dry product first, is then cut into small
After section, crushing, the pre-treatment steps such as sieving (preferably being sieved with the sieve of 60 mesh of aperture) obtain Rhizoma Gastrodiae powder, and conduct
The raw material further extracted；
Then, (the preferably laboratory levels extraction element such as flask, or extraction is added in extraction vessel in Rhizoma Gastrodiae powder
The technical grades extraction elements such as tank, extraction kettle), water (preferably distilled water) is then added；
Wherein, solid-liquid ratio control is 1:20~1:60g/ml, such as can be, but it is not limited to 1:25、1:30、1:35、1:
40、1:45、1:50 or 1:55g/ml etc.；Preferably 1:30~1:50g/ml；More preferably 1:40g/ml；
Then, preferred in such a way that water-bath heat is heated to reflux, carry out the extraction of gastrodia elata polysaccharide；
Wherein, the temperature of heating water bath refluxing extraction is 60~80 DEG C, such as can be, but is not limited to 65,70 or 75
DEG C etc.；Preferably, the temperature of heating water bath refluxing extraction is 70~80 DEG C；It is furthermore preferred that the temperature of heating water bath refluxing extraction
It is 70 DEG C；
Meanwhile the time of heating water bath refluxing extraction is 1~3h, such as can be, but it is not limited to 1.5,2 or 2.5h
Deng；Preferably, the time of heating water bath refluxing extraction is 2~3h；It is furthermore preferred that the time of heating water bath refluxing extraction is 2h.
It is preferred by the way of filtering after extraction, it is separated by solid-liquid separation, and gained filtrate and filter residue are received respectively
Collection；
Collected obtained filter residue extracts under the same conditions in Rhizoma Gastrodiae powder as above, then extracts once, and preferably uses
The mode of filtering is separated by solid-liquid separation, and filtrate is collected；
Gained filtrate it will merge twice, it is then preferred to be concentrated combined filtrate by the way of heating evaporation,
Obtain Rhizoma Gastrodiae extract concentrate；
Then, absolute ethyl alcohol is added into gained concentrate, and the concentration of ethyl alcohol is made to reach the left and right 80% (v/v)；So
Afterwards, alcohol precipitation is stood under cryogenic, and the time control of standing is in 12h or so；
Then, be separated by solid-liquid separation (preferred using the filterings such as filter by the way of), obtained solid dry after to get to production
Object gastrodia elata polysaccharide crude product (Rhizoma Gastrodiae Thick many candies).
The measurement of gastrodia elata polysaccharide content can be carried out by phend-sulphuric acid by extracting obtained gastrodia elata polysaccharide crude product, and be adopted
With this assay method, not only step is easy quickly, while high sensitivity, color stability.
By the Rhizoma Gastrodiae Thick many candies prepared by method as above after the purification steps such as de- albumen, it can obtain with higher degree
Gastrodia elata polysaccharide, and purify obtained gastrodia elata polysaccharide can also be further used as functional raw material, and be used for skin cream etc. it is a variety of
In the preparation of skin care item.
Skin care item provided by the present invention are preferably skin cream, in the raw material of currently preferred skin cream, remove conduct
Can also include the Rosa Damascana as flavouring agent, and as base starting material outside the gastrodia elata polysaccharide of functional components：All scholars
Woods, atoleine, Arlacel-60, octadecyl alcolol, hexadecanol, glycerine, DBPC 2,6 ditertiary butyl p cresol, lanolin, Tween-80, the third two
Alcohol and water (preferably distilled water)；
In parts by weight, as above each raw material dosage is as follows：0.1~0.2 part of gastrodia elata polysaccharide, 1~2 part of vaseline, liquid
4~6 parts of body paraffin, 1~2 part of Arlacel-60,2~3 parts of octadecyl alcolol, 1~2 part of hexadecanol, 1~2 part of glycerine, lanolin 1~2
Part, 1~2 part of Tween-80,1~2 part of propylene glycol, 0.005~0.0008 part of 2,6-di-tert-butyl p-cresol, Rosa Damascana 0.01
~0.02 part and 30~55 parts of water；
Preferably, in parts by weight, as above each raw material dosage is as follows：0.1 part of gastrodia elata polysaccharide, 2 parts of vaseline, liquid
4 parts of paraffin, 1 part of Arlacel-60,2 parts of octadecyl alcolol, 1 part of hexadecanol, 2 parts of glycerine, 1 part of lanolin, 2 parts of Tween-80, propylene glycol 1
55 parts of part, 0.005 part of 2,6-di-tert-butyl p-cresol, 0.02 part of Rosa Damascana and water.
The step of preparation process of skin care item as above is also relatively simple, can refer to as follows：
By vaseline, atoleine, Arlacel-60, octadecyl alcolol, hexadecanol, glycerine, 2,6-di-tert-butyl p-cresol, and
After lanolin mixing, is dissolved under 80 DEG C of condition of water bath heating, obtain oil phase；
Gastrodia elata polysaccharide, Tween-80, propylene glycol and Rosa Damascana are added to the water dissolving, then added in 80 DEG C of water-baths
Heating obtains water phase under heat condition；
Finally oil phase is slowly added to along glass bar in water phase and constantly stirred along the same direction to condensation to get
Oil-in-water type (O/W) skin cream.
Embodiment 1
Day anesthesia stem is placed in pallet, dry 4h, is cut into segment and is crushed with pulverizer at 60 DEG C, is filled after crossing 60 mesh sieve
Enter in hermetic bag, it is spare, obtain Rhizoma Gastrodiae powder；
5g Rhizoma Gastrodiae powders are weighed, are poured into the round-bottomed flask of 500mL, 200mL distilled water are then added into flask, in 70 DEG C
Water-bath in after heating and refluxing extraction 2h, filtered while hot, filter residue with identical condition repeated to extract primary, merged twice
Filtrate, filtrate are concentrated into 20mL or so through Rotary Evaporators, and absolute ethyl alcohol to concentration of alcohol is added after being cooled to room temperature and reaches
80% or so, it is filtered after refrigerator places 12h, is drying to obtain Thick many candies 0.395g.
The accurate Thick many candies for weighing 0.025g, being dissolved in water and being transferred to 50mL volumetric flasks adds water to scale, shakes up up to sample
Product solution, it is spare.
Determination of polysaccharide in Thick many candies：
(1) standard curve
Take 5 10mL tool plug test tubes, be separately added into 0.01mg/mL, 0.02mg/mL, 0.03mg/mL, 0.04mg/mL,
Each 1.0mL of 0.05mg/mL glucose standards solutions, precision pipette, and then respectively distilled water are added to supply 2.0mL, then be separately added into
6% phenol solution that 1.0mL has been prepared, 5.0mL concentrated sulfuric acid solutions are slowly added to after shaking up along test tube wall, and test tube is put into ice
10 minutes in water, it is cooled to room temperature through flowing water after 80 DEG C of heating water baths 15 minutes.Using reagent blank as reference, that is, 2mL is taken to steam
Distilled water is same as above step operation.
Under the conditions of selected wavelength X=490nm, by determined by ultraviolet spectrophotometry absorbance, sat using absorbance as vertical
Mark and concentration draw standard curve as abscissa, the results showed that concentration of glucose in measurement range 0.01-0.05mg/mL and
Absorbance has good linear relationship, obtains equation of linear regression y=9.66C+0.0394, R2=0.998.Specific experiment data
Referring to table 1, canonical plotting is referring to Fig. 1.
1 experimental data of table
(2) determination of polysaccharide
Precision pipettes 1.0mL sample solutions and is added in 10mL tool plug test tubes, and distilled water is added to supply 2.0mL, then presses step
(1) assay method of standard curve is operated, and measures absorbance, and returning journey according to gained in step (1) calculates polysaccharide concentration,
Polyoses content in 1 Rhizoma Gastrodiae Thick many candies of embodiment is obtained by formula polyoses content (%)=C × D × f/W × 100%.
In formula：The polysaccharide concentration (mg/mL) that C is acquired by regression equation；D dilutes volume (mL)；F conversion factors；W polysaccharide samples
Quality (mg)
(3) determination of conversion factor f
Precision weighs 0.020g Rhizoma Gastrodiae Thick many candies, is dissolved in beaker with distilled water, is then transferred in 250mL volumetric flasks simultaneously
Scale constant volume is added water to, shakes up and obtains stock solution, takes 1.0mL stock solutions, then presses the assay method of step (1) standard curve
It is operated, measures absorbance, the content of polysaccharide, measurement result A=0.457 are calculated from calibration curve equation.
Concentration is calculated by calibration curve equation, then calculates conversion factor f=1.85, calculation formula f=m/ (C × V).
In formula：The polysaccharide quality (mg) that m is weighed；C sugar concentration (mg/mL)；V constant volumes (mL).
It according to method as above, is calculated, in 1 product Thick many candies of embodiment, the content of gastrodia elata polysaccharide is 22.33%.
Embodiment 2
With reference to the method for embodiment 1, Rhizoma Gastrodiae powder is obtained；
5g Rhizoma Gastrodiae powders are weighed, are poured into the round-bottomed flask of 500mL, 200mL distilled water are then added into flask, in 60 DEG C
Water-bath in after heating and refluxing extraction 2h, filtered while hot, filter residue with identical condition repeated to extract primary, merged twice
Filtrate, filtrate are concentrated into 20mL or so through Rotary Evaporators, and absolute ethyl alcohol to concentration of alcohol is added after being cooled to room temperature and reaches
80% or so, it is filtered after refrigerator places 12h, is dried to obtain the Thick many candies 0.135g of embodiment 2.
Then, with reference to the method in embodiment 1, in the product Thick many candies for measuring embodiment 2, the content of gastrodia elata polysaccharide is
11.97%.
Embodiment 3
With reference to the method for embodiment 1, Rhizoma Gastrodiae powder is obtained；
5g Rhizoma Gastrodiae powders are weighed, are poured into the round-bottomed flask of 500mL, 200mL distilled water are then added into flask, in 65 DEG C
Water-bath in after heating and refluxing extraction 2h, filtered while hot, filter residue with identical condition repeated to extract primary, merged twice
Filtrate, filtrate are concentrated into 20mL or so through Rotary Evaporators, and absolute ethyl alcohol to concentration of alcohol is added after being cooled to room temperature and reaches
80% or so, it is filtered after refrigerator places 12h, is dried to obtain the Thick many candies 0.226g of embodiment 3.
Then, with reference to the method in embodiment 1, in the product Thick many candies for measuring embodiment 3, the content of gastrodia elata polysaccharide is
12.67%.
Embodiment 4
With reference to the method for embodiment 1, Rhizoma Gastrodiae powder is obtained；
5g Rhizoma Gastrodiae powders are weighed, are poured into the round-bottomed flask of 500mL, 200mL distilled water are then added into flask, in 75 DEG C
Water-bath in after heating and refluxing extraction 2h, filtered while hot, filter residue with identical condition repeated to extract primary, merged twice
Filtrate, filtrate are concentrated into 20mL or so through Rotary Evaporators, and absolute ethyl alcohol to concentration of alcohol is added after being cooled to room temperature and reaches
80% or so, it is filtered after refrigerator places 12h, is dried to obtain the Thick many candies 0.328g of embodiment 4.
Then, with reference to the method in embodiment 1, in the product Thick many candies for measuring embodiment 4, the content of gastrodia elata polysaccharide is
21.09%.
Embodiment 5
With reference to the method for embodiment 1, Rhizoma Gastrodiae powder is obtained；
5g Rhizoma Gastrodiae powders are weighed, are poured into the round-bottomed flask of 500mL, 200mL distilled water are then added into flask, in 65 DEG C
Water-bath in after heating and refluxing extraction 2h, filtered while hot, filter residue with identical condition repeated to extract primary, merged twice
Filtrate, filtrate are concentrated into 20mL or so through Rotary Evaporators, and absolute ethyl alcohol to concentration of alcohol is added after being cooled to room temperature and reaches
80% or so, it is filtered after refrigerator places 12h, is dried to obtain the Thick many candies 0.309g of embodiment 5.
Then, with reference to the method in embodiment 1, in the product Thick many candies for measuring embodiment 5, the content of gastrodia elata polysaccharide is
21.07%.
Embodiment 6
With reference to the method for embodiment 1, Rhizoma Gastrodiae powder is obtained；
5g Rhizoma Gastrodiae powders are weighed, are poured into the round-bottomed flask of 500mL, 200mL distilled water are then added into flask, in 70 DEG C
Water-bath in after heating and refluxing extraction 1h, filtered while hot, filter residue with identical condition repeated to extract primary, merged twice
Filtrate, filtrate are concentrated into 20mL or so through Rotary Evaporators, and absolute ethyl alcohol to concentration of alcohol is added after being cooled to room temperature and reaches
80% or so, it is filtered after refrigerator places 12h, is dried to obtain the Thick many candies 0.218g of embodiment 6.
Then, with reference to the method in embodiment 1, in the product Thick many candies for measuring embodiment 6, the content of gastrodia elata polysaccharide is
12.13%.
Embodiment 7
With reference to the method for embodiment 1, Rhizoma Gastrodiae powder is obtained；
5g Rhizoma Gastrodiae powders are weighed, are poured into the round-bottomed flask of 500mL, 200mL distilled water are then added into flask, in 70 DEG C
Water-bath in after heating and refluxing extraction 1.5h, filtered while hot, filter residue with identical condition repeated to extract primary, merge two
Secondary filtrate, filtrate are concentrated into 20mL or so through Rotary Evaporators, and absolute ethyl alcohol to concentration of alcohol is added after being cooled to room temperature and reaches
80% or so, it is filtered after refrigerator places 12h, is dried to obtain the Thick many candies 0.276g of embodiment 7.
Then, with reference to the method in embodiment 1, in the product Thick many candies for measuring embodiment 7, the content of gastrodia elata polysaccharide is
17.3%.
Embodiment 8
With reference to the method for embodiment 1, Rhizoma Gastrodiae powder is obtained；
5g Rhizoma Gastrodiae powders are weighed, are poured into the round-bottomed flask of 500mL, 200mL distilled water are then added into flask, in 70 DEG C
Water-bath in after heating and refluxing extraction 2.5h, filtered while hot, filter residue with identical condition repeated to extract primary, merge two
Secondary filtrate, filtrate are concentrated into 20mL or so through Rotary Evaporators, and absolute ethyl alcohol to concentration of alcohol is added after being cooled to room temperature and reaches
80% or so, it is filtered after refrigerator places 12h, is dried to obtain the Thick many candies 0.354g of embodiment 8.
Then, with reference to the method in embodiment 1, in the product Thick many candies for measuring embodiment 8, the content of gastrodia elata polysaccharide is
22.16%.
Embodiment 9
With reference to the method for embodiment 1, Rhizoma Gastrodiae powder is obtained；
5g Rhizoma Gastrodiae powders are weighed, are poured into the round-bottomed flask of 500mL, 200mL distilled water are then added into flask, in 70 DEG C
Water-bath in after heating and refluxing extraction 3h, filtered while hot, filter residue with identical condition repeated to extract primary, merged twice
Filtrate, filtrate are concentrated into 20mL or so through Rotary Evaporators, and absolute ethyl alcohol to concentration of alcohol is added after being cooled to room temperature and reaches
80% or so, it is filtered after refrigerator places 12h, is dried to obtain the Thick many candies 0.316g of embodiment 9.
Then, with reference to the method in embodiment 1, in the product Thick many candies for measuring embodiment 9, the content of gastrodia elata polysaccharide is
21.13%.
Embodiment 10
With reference to the method for embodiment 1, Rhizoma Gastrodiae powder is obtained；
5g Rhizoma Gastrodiae powders are weighed, are poured into the round-bottomed flask of 500mL, 100mL distilled water are then added into flask, in 70 DEG C
Water-bath in after heating and refluxing extraction 2h, filtered while hot, filter residue with identical condition repeated to extract primary, merged twice
Filtrate, filtrate are concentrated into 20mL or so through Rotary Evaporators, and absolute ethyl alcohol to concentration of alcohol is added after being cooled to room temperature and reaches
80% or so, it is filtered after refrigerator places 12h, is dried to obtain the Thick many candies 0.122g of embodiment 6.
Then, with reference to the method in embodiment 1, in the product Thick many candies for measuring embodiment 10, the content of gastrodia elata polysaccharide is
10.06%.
Embodiment 11
With reference to the method for embodiment 1, Rhizoma Gastrodiae powder is obtained；
5g Rhizoma Gastrodiae powders are weighed, are poured into the round-bottomed flask of 500mL, 150mL distilled water are then added into flask, in 70 DEG C
Water-bath in after heating and refluxing extraction 2h, filtered while hot, filter residue with identical condition repeated to extract primary, merged twice
Filtrate, filtrate are concentrated into 20mL or so through Rotary Evaporators, and absolute ethyl alcohol to concentration of alcohol is added after being cooled to room temperature and reaches
80% or so, it is filtered after refrigerator places 12h, is dried to obtain the Thick many candies 0.288g of embodiment 6.
Then, with reference to the method in embodiment 1, in the product Thick many candies for measuring embodiment 11, the content of gastrodia elata polysaccharide is
13.28%.
Embodiment 12
With reference to the method for embodiment 1, Rhizoma Gastrodiae powder is obtained；
5g Rhizoma Gastrodiae powders are weighed, are poured into the round-bottomed flask of 500mL, 250mL distilled water are then added into flask, in 70 DEG C
Water-bath in after heating and refluxing extraction 2h, filtered while hot, filter residue with identical condition repeated to extract primary, merged twice
Filtrate, filtrate are concentrated into 20mL or so through Rotary Evaporators, and absolute ethyl alcohol to concentration of alcohol is added after being cooled to room temperature and reaches
80% or so, it is filtered after refrigerator places 12h, is dried to obtain the Thick many candies 0.337g of embodiment 12.
Then, with reference to the method in embodiment 1, in the product Thick many candies for measuring embodiment 12, the content of gastrodia elata polysaccharide is
21.59%.
Embodiment 10
With reference to the method for embodiment 1, Rhizoma Gastrodiae powder is obtained；
5g Rhizoma Gastrodiae powders are weighed, are poured into the round-bottomed flask of 500mL, 300mL distilled water are then added into flask, in 70 DEG C
Water-bath in after heating and refluxing extraction 2h, filtered while hot, filter residue with identical condition repeated to extract primary, merged twice
Filtrate, filtrate are concentrated into 20mL or so through Rotary Evaporators, and absolute ethyl alcohol to concentration of alcohol is added after being cooled to room temperature and reaches
80% or so, it is filtered after refrigerator places 12h, is dried to obtain the Thick many candies 0.312g of embodiment 13.
Then, with reference to the method in embodiment 1, in the product Thick many candies for measuring embodiment 13, the content of gastrodia elata polysaccharide is
20.7%.
Embodiment 11
According to：Octadecyl alcolol 2g, DBPC 2,6 ditertiary butyl p cresol 0.005g, hexadecanol 1g, vaseline 2g, Arlacel-60 1g,
Lanolin 1g, atoleine 4g, glycerine 2g；And Tween-80 2g, propylene glycol 1g, the gastrodia elata polysaccharide (day prepared by embodiment 1
Numb Thick many candies purify to obtain) 0.1g, Rosa Damascana 0.02g, distilled water 55g, weigh each raw material respectively；
By octadecyl alcolol, DBPC 2,6 ditertiary butyl p cresol, hexadecanol, vaseline, Arlacel-60, lanolin, atoleine, sweet
Oil mixing, which is placed in 80 DEG C of thermostat water bath, to be dissolved by heating, as oil phase；
Then, Tween-80, propylene glycol, gastrodia elata polysaccharide and Rosa Damascana are added in distilled water；
Finally, oil phase is slowly added to along glass bar in water phase and is constantly stirred along the same direction to condensing, i.e.,
Obtain oil-in-water type (O/W) skin cream.
Experimental example 1
Matrix is for the sense organ, heat-resisting of skin care item, and cold-resistant equal physicochemical properties have certain influence, it is then desired to
Adjustment is optimized for matrix formulations dosage.
Experiment 1
It weighs respectively：Vaseline 1g, atoleine 4g, Arlacel-60 1g, octadecyl alcolol 2g, hexadecanol 1g, glycerine 1g, wool
Fat 1g, Tween-80 1g, propylene glycol 1g, 2,6-di-tert-butyl p-cresol 0.005g and distilled water 30g；
Then, vaseline, atoleine, Arlacel-60, octadecyl alcolol, hexadecanol, glycerine, lanolin, 2,6- are taken according to formula
Di-tert-butyl p-cresol is stirred evenly in 80 DEG C of heating water baths to melting as skin cream matrix oil phase after being added in beaker according to quantity,
Heat preservation 10 minutes；Propylene glycol, Tween-80, distilled water separately are taken, as matrix water phase, is added in beaker adds in 80 DEG C of water-baths according to quantity
Heat keeps the temperature ten minutes to dissolving；Oil phase is slowly added into along glass bar in water phase, and constantly stirring is straight in a counterclockwise direction
To condensation to get to experiment 1 skin cream matrix lotion.
Experiment 2
It weighs respectively：Vaseline 1g, atoleine 4g, Arlacel-60 1g, octadecyl alcolol 2g, hexadecanol 1g, glycerine 1g, wool
Fat 2g, Tween-80 2g, propylene glycol 2g, 2,6-di-tert-butyl p-cresol 0.008g and distilled water 55g；
Then, with reference to the method for experiment 1, the skin cream matrix lotion of experiment 2 is obtained.
Experiment 3
It weighs respectively：Vaseline 1g, atoleine 4g, Arlacel-60 2g, octadecyl alcolol 3g, hexadecanol 2g, glycerine 1g, wool
Fat 1g, Tween-80 1g, propylene glycol 2g, 2,6-di-tert-butyl p-cresol 0.008g and distilled water 55g；
Then, with reference to the method for experiment 1, the skin cream matrix lotion of experiment 3 is obtained.
Experiment 4
It weighs respectively：Vaseline 1g, atoleine 6g, Arlacel-60 1g, octadecyl alcolol 3g, hexadecanol 2g, glycerine 1g, wool
Fat 2g, Tween-80 2g, propylene glycol 1g, 2,6-di-tert-butyl p-cresol 0.005g and distilled water 55g；
Then, with reference to the method for experiment 1, the skin cream matrix lotion of experiment 4 is obtained.
Experiment 5
Vaseline 1g, it atoleine 6g, Arlacel-60 2g, octadecyl alcolol 2g, hexadecanol 2g, glycerine 2g, lanolin 1g, spits
Temperature -80 2g, propylene glycol 1g, 2,6-di-tert-butyl p-cresol 0.008g and distilled water 30g；
Then, with reference to the method for experiment 1, the skin cream matrix lotion of experiment 5 is obtained.
Experiment 6
Vaseline 1g, it atoleine 6g, Arlacel-60 2g, octadecyl alcolol 3g, hexadecanol 1g, glycerine 2g, lanolin 2g, spits
Temperature -80 1g, propylene glycol 2g, 2,6-di-tert-butyl p-cresol 0.005g and distilled water 30g；
Then, with reference to the method for experiment 1, the skin cream matrix lotion of experiment 6 is obtained.
Experiment 7
Vaseline 2g, it atoleine 4g, Arlacel-60 2g, octadecyl alcolol 3g, hexadecanol 1g, glycerine 1g, lanolin 2g, spits
Temperature -80 2g, propylene glycol 1g, 2,6-di-tert-butyl p-cresol 0.008g and distilled water 30g；
Then, with reference to the method for experiment 1, the skin cream matrix lotion of experiment 7 is obtained.
Experiment 8
Vaseline 2g, it atoleine 4g, Arlacel-60 2g, octadecyl alcolol 2g, hexadecanol 2g, glycerine 2g, lanolin 2g, spits
Temperature -80 1g, propylene glycol 1g, 2,6-di-tert-butyl p-cresol 0.005g and distilled water 55g；
Then, with reference to the method for experiment 1, the skin cream matrix lotion of experiment 8 is obtained.
Experiment 9
Vaseline 2g, it atoleine 4g, Arlacel-60 1g, octadecyl alcolol 3g, hexadecanol 2g, glycerine 2g, lanolin 1g, spits
Temperature -80 2g, propylene glycol 2g, 2,6-di-tert-butyl p-cresol 0.005g and distilled water 30g；
Then, with reference to the method for experiment 1, the skin cream matrix lotion of experiment 9 is obtained.
Experiment 10
Vaseline 2g, it atoleine 6g, Arlacel-60 2g, octadecyl alcolol 2g, hexadecanol 1g, glycerine 1g, lanolin 1g, spits
Temperature -80 2g, propylene glycol 2g, 2,6-di-tert-butyl p-cresol 0.005g and distilled water 55g；
Then, with reference to the method for experiment 1, the skin cream matrix lotion of experiment 10 is obtained.
Experiment 11
Vaseline 2g, it atoleine 6g, Arlacel-60 1g, octadecyl alcolol 3g, hexadecanol 1g, glycerine 2g, lanolin 1g, spits
Temperature -80 1g, propylene glycol 1g, 2,6-di-tert-butyl p-cresol 0.008g and distilled water 55g；
Then, with reference to the method for experiment 1, the skin cream matrix lotion of experiment 11 is obtained.
Experiment 12
Vaseline 2g, it atoleine 6g, Arlacel-60 1g, octadecyl alcolol 2g, hexadecanol 2g, glycerine 1g, lanolin 2g, spits
Temperature -80 1g, propylene glycol 2g, 2,6-di-tert-butyl p-cresol 0.008g and distilled water 30g；
Then, with reference to the method for experiment 1, the skin cream matrix lotion of experiment 12 is obtained.
Evaluation and test：
Sense organ is carried out to the skin cream matrix lotion for testing 1-12 respectively and physicochemical property is evaluated and tested；
Wherein, sensory evaluation is evaluated according to People's Republic of China's light industry standard " QB/T 1857-2013 ",
Mainly evaluated in terms of color and luster, viscosity, lotion sophistication, uniformity, stretchability, smell etc. 6.
According to professional standard QB/T 1857-2013 oil-in-water types, physics and chemistry evaluation is carried out with cold-resistant, heat resistant test.
Heat resistant test：Under conditions of (40 ± 1) DEG C, it is packed into skin cream 10g placements in test tube and restores afterwards for 24 hours to room
Temperature, observation lotion and have no significant difference whether there is or not water-oil separating phenomenon before experiment.
Low temperature resistant test：Under conditions of (- 8 ± 2) DEG C, it is packed into skin cream 10g placements in test tube and restores afterwards for 24 hours to room
There is no significant difference before temperature, observation lotion character and experiment.
To sum up, with organoleptic indicator (Y1) full marks 5 divide, physical and chemical index (Y2) full marks 5 divide for inspection target, respectively with weight system
Number 5:5 carry out comprehensive score Y=Y1+Y2, total score is 10 points.
Evaluation result is as shown in table 2 below：
Table 2 tests 1-12 skin cream matrix lotion evaluation results
By as above testing evaluation result it is found that 9 matrix various aspects of performance of experiment are optimal, thus are more suitable as shield of the present invention
Skin product matrix formulations
Although illustrate and describing the present invention with specific embodiment, it will be appreciated that without departing substantially from the present invention's
Many other change and modification can be made in the case of spirit and scope.It is, therefore, intended that in the following claims
Including belonging to all such changes and modifications in the scope of the invention.
Claims (10)
1. the extracting method of a kind of day anesthesia stem polysaccharide, which is characterized in that include the following steps：
After the pretreatment of its anesthesia stem, add water refluxing extraction, after separation of solid and liquid, filtrate and filter residue is separately recovered；
Filter residue carries out repeating extraction under the same conditions, is concentrated after filtrate is merged, then alcohol precipitation at low temperature, after separation of solid and liquid
It is dry, obtain a day anesthesia stem polysaccharide；
Preferably, the day anesthesia stem, which pre-processes, includes：By day anesthesia stem crushed after being dried, then it is sieved.
2. the extracting method of according to claim 1 day anesthesia stem polysaccharide, which is characterized in that the matter of pretreated Rhizoma Gastrodiae
It is 1 to measure the ratio between grams and the volume ml of added water：(20~60)；
Preferably, the ratio between the quality grams of pretreated Rhizoma Gastrodiae and the volume ml of added water are 1：(30~50)；
It is furthermore preferred that the ratio between the quality grams of pretreated Rhizoma Gastrodiae and the volume ml of added water are 1：40.
3. the extracting method of according to claim 1 day anesthesia stem polysaccharide, which is characterized in that the temperature of refluxing extraction is 60
~80 DEG C；
Preferably, the temperature of refluxing extraction is 70~80 DEG C；
It is furthermore preferred that the temperature of refluxing extraction is 70 DEG C.
4. the extracting method of according to claim 1 day anesthesia stem polysaccharide, which is characterized in that the time of refluxing extraction is 1
~3h；
Preferably, the time of refluxing extraction is 2~3h；
It is furthermore preferred that the time of refluxing extraction is 2h.
5. the gastrodia elata polysaccharide obtained by the extracting method described in any one of claim 1-4.
6. application of the day anesthesia stem polysaccharide in preparing skin care item described in claim 5.
7. a kind of skin care item, which is characterized in that the raw material of the skin cream includes the gastrodia elata polysaccharide described in claim 5.
8. skin care item according to claim 7, which is characterized in that the raw material of the skin care item still further comprises：
Vaseline, atoleine, Arlacel-60, octadecyl alcolol, hexadecanol, glycerine, lanolin, Tween-80, propylene glycol, bis- uncles of 2,6-
It is one or more in butyl paracresol, Rosa Damascana and deionization.
9. skin care item according to claim 8, which is characterized in that in parts by weight, in the skin care item, each raw material
Dosage is as follows：
0.1~0.2 part of gastrodia elata polysaccharide, 1~2 part of vaseline, 4~6 parts of atoleine, 1~2 part of Arlacel-60, octadecyl alcolol 2~3
Part, 1~2 part of hexadecanol, 1~2 part of glycerine, 1~2 part of lanolin, 1~2 part of Tween-80,1~2 part of propylene glycol, 2,6- bis- uncles
30~55 parts of 0.005~0.0008 part of butyl paracresol, 0.01~0.02 part of Rosa Damascana and water.
10. the preparation method of the skin care item described in claim 8 or 9, which is characterized in that including：
By vaseline, atoleine, Arlacel-60, octadecyl alcolol, hexadecanol, glycerine, 2,6-di-tert-butyl p-cresol and wool
It is dissolved by heating after fat mixing, obtains oil phase；
Gastrodia elata polysaccharide, Tween-80, propylene glycol and Rosa Damascana are added to the water dissolving heating and obtain water phase；
Then, under agitation, during the oil phase is added to the aqueous phase, skin care item are obtained.
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| CN113754706A (en) * | 2021-09-10 | 2021-12-07 | 广东青云山药业有限公司 | Gastrodia elata extract and preparation method thereof |
| CN114306517A (en) * | 2021-12-31 | 2022-04-12 | 西南林业大学 | Comprehensive utilization method of overground part of gastrodia elata |
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