A kind of preparation method of nutrition keratin facial mask
Technical field
The present invention relates to cosmetics and biomedical engineering fields, and in particular to a kind of preparation side of nutrition keratin facial mask
Method.
Background technique
With the development of the global economy with the raising of living standards of the people and total quality, more and more people start to make
It applies some make up, especially for the daily nursing of face skin, and with the development of society, people require also to get over to cosmetics
Come it is higher, people more want using have preferably activity and preservative free cosmetics.In existing cosmetics, make in addition to daily
Creams class cosmetics, facial mask are also a kind of daily required product of face skin nursing.The form of facial mask mainly has mud cream
Type, tear-pull, gel-type, four kinds of hygenic towelette type.Hygenic towelette formula is generally exactly the face paper for infiltrating Essence of mmic package,
It is divided by material: non-woven fabrics, silk, cotton, terylene, blended, tencel, biological fiber etc..Hygenic towelette type facial mask is application method
It is most simple, and have the characteristics that nutrition distribution pattern is uniform, so such facial mask is the most wide a kind of facial mask of use scope.
Common facial mask mainly has the function of cleaning, replenishing water and preserving moisture, whitening, the old, Sage Extract of removing wrinkle and resisting aging etc. in the market,
These facial masks inevitably introduce certain amount by many aspects such as raw material, ingredient, packaging materials in process of production
Microorganism, protein inherently rich in, polysaccharide, oligosaccharides, the vitamin etc. in facial mask essence easily cause in addition
The ingredient of microbial reproduction, this is easy to cause bacterium mass propagation in facial mask, from causing the rotten of facial mask.Therefore in facial mask
Different types of preservative will be added in production process to inhibit the breeding of microorganism or kill microorganism.In cosmetics
The use of preservative main function is to prevent microorganism from growing in the product, keeps the property of skin care item stable and use of uncapping
After be unlikely to deteriorate.The more skin care item of moisture more need preservative.
In addition, more and more active constituents are used for facial mask class product with the progress of science and technology, life is specifically included that
Long factor type, activated protein class, active peptides class, vitamins and some Polyphenols have the substance of antioxidant activity.This
A little substances are easy to lose activity in hygenic towelette type facial mask.Therefore it is high and be unlikely to deteriorate to develop a kind of trophic factors joint efficiency
Facial mask is extremely important for the development of mask product.
Keratin has the advantage biodegradable, bioactivity is high and compatibility is good, the keratin extracted from human hair
Also there is low immune rejection.Relative to other bulk materials, keratin source is almost unrestricted, thus in cosmetic field
Research using more and more being paid attention to.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of preparation method of nutrition keratin facial mask, the present invention is utilized
Multinomial technology, including electrostatic spinning technique, low-temperature plasma processing technique, negative pressure dodge quick-fried technology etc., obtain and seek with skin
Support the keratin nanofiber facial mask that the factor is strengthened.
The present invention provides the preparation methods of nutrition keratin facial mask, include the following steps:
S1: regeneration human hair keratin is dissolved completely in the formic acid solution of 98v/v%, stirs evenly, obtains spinning solution;
S2: electrostatic spinning is carried out using the spinning solution that step S1 is obtained, obtains keratin nano fibrous membrane;
S3: it is 7.4 that the keratin nano fibrous membrane, which is washed with phosphate buffer to pH value, through plasma after drying
Processor processing activation;
S4: the keratin nano fibrous membrane that S3 is obtained is immersed in the phosphate buffer added with skin nutrition factors and is carried out
Negative pressure sudden strain of a muscle is quick-fried, then carries out graft reaction;
S5: the keratin nano fibrous membrane centrifugation freeze-drying of graft reaction will be completed, obtains the nutrition keratin facial mask.
Preferably, in step S1, the concentration of the regeneration human hair keratin is 10~30g/L.
Preferably, in step S2, in electrostatic spinning process, the specification of syringe used is 10ml, and needle gauge is tack,
No. 7 needles;Electrospinning conditions are 12~20KV of voltage, 7~10cm of distance, 0.3~1.0ml/h of sample rate, temperature 25~35
℃。
Preferably, in step S3, drying temperature is 37~45 DEG C, and drying time is 2~4h.
Preferably, in step S3, the condition of the plasma processor processing are as follows: gas uses nitrogen or oxygen, processing
Power is 250~300W, and 50~60Pa of pressure, the processing time is 10~15min.
Preferably, in step S4, the composition of the skin nutrition factors is as follows:
Preferably, the phosphate buffer pH value is 7.4.
Preferably, in step S4, it is 0.100~0.024mBar that negative pressure, which dodges quick-fried vacuum degree,.
Preferably, in step S4, the soaking bath ratio of graft reaction is 1:100~1:300, and reaction temperature is 0~4 DEG C, instead
Between seasonable for 12~for 24 hours.
Preferably, in step S5, centrifugal gravity acceleration is 10000g, and time 10min, the temperature of freeze-drying is -30~-20
DEG C, vacuum degree is 0.100~0.024mBar, and freeze-drying time is 3~5d.
Compared with prior art, the invention has the benefit that the present invention, which utilizes, has biodegradable, bioactivity
High, the advantages such as compatibility is good keratin use nanofiber preparation method and are grafted skin nutrition factors, develop a kind of battalion
Support the facial mask that factor joint efficiency is high and is unlikely to deteriorate.Wherein, nutrition keratin facial mask is prepared by multinomial technology, including electrostatic
Spining technology, low-temperature plasma processing technique, negative pressure dodge quick-fried technology etc., the use of these technologies substantially increase skin-nourishing because
The Percentage bound of son and fiber, load capacity is bigger, and is covalently attached and is unlikely to deteriorate, and facial mask obtained being capable of preferably nutrition and reparation
Skin Cell, reach epidermis maintenance, wake up anti-ageing skin, U.S. myotrophy the effect of, the access times of facial mask can also be increased.In addition,
Moisture-free in facial mask provided by the invention can realize the function of facial mask by way of rehydration when in use, of the invention in this way
Facial mask has better stability compared with facial mask in the prior art during preservation.
Detailed description of the invention
Fig. 1: the L929 mouse fibroblast cells proliferation rate under the embodiment of the present invention and comparative example processing.
Specific embodiment
According to following embodiments, the present invention may be better understood.However, as it will be easily appreciated by one skilled in the art that real
It applies content described in example and is merely to illustrate the present invention, without sheet described in detail in claims should will not be limited
Invention.
The technical solution adopted by the invention is as follows:
A kind of preparation method of nutrition keratin facial mask, which comprises the steps of:
S1: a certain amount of regeneration human hair keratin is dissolved completely in 98% (v/v) formic acid solution, stirs evenly, is spun
Silk liquid;
S2: electrostatic spinning is carried out using spinning solution, obtains keratin nano fibrous membrane;
S3: by keratin nano fibrous membrane with commercially available phosphate buffer wash to pH value be 7.4, after drying through grade from
Sub-processors handle activation;
S4: the nano fibrous membrane that step 3 is obtained is immersed in the phosphate buffer added with skin nutrition factors and bears
Pressure sudden strain of a muscle is quick-fried, carries out graft reaction later;
S5: the nano fibrous membrane centrifugation freeze-drying of graft reaction will be completed, obtains nutrition keratin facial mask.
In above-mentioned preparation method of the invention:
It is preferably 10~30g/L that the concentration of human hair keratin is regenerated in step S1, more preferably 20g/L;
In step S2, in electrostatic spinning process, the specification of syringe used is preferably 10ml, and needle gauge is preferably flat
Head, No. 7 needles;Electrospinning conditions are preferably that voltage is 12~20KV, more preferably 15KV, and distance is 7~10cm, more preferably
For 8cm, sample rate is 0.3~1.0ml/h, and more preferably 0.5ml/h, temperature is 25~35 DEG C, more preferably 30 DEG C;
In step S3, the pH value of phosphate buffer is 7.4, and the temperature of drying is 37~45 DEG C, more preferably preferably 37 DEG C,
Drying time is 2~4h, more preferably 4h.The condition of plasma treatment are as follows: gas use nitrogen or oxygen, more preferable oxygen,
Processing power be 250~300W, more preferably 280W, 50~60Pa of pressure, more preferably 55Pa, processing the time be 10~
15min, more preferably 15min.
In step S4, phosphate buffer pH is 7.4.The composition of skin nutrition factors is preferred are as follows: and tremella polysaccharides 100~
300g/L, more preferably 200g/L;Sodium alginate 50~100g/L, more preferable 80g/L;1~3g/L of Rosa Damascana, more preferably
2g/L;1~3g/L of lemon, more preferably 2g/L;Vitamin e1~3g/L, more preferably 2g/L;5~10g/ of vitamin C
L, more preferably 8g/L;5~15g/L of propylene glycol, more preferably 10g/L;5~15g/L of glycerol, more preferably 10g/L;Monoglyceride
1~5g/L, more preferably 2g/L;Cetearyl alcohol 1~5g/L of alcohol ether, more preferably 2g/L.Negative pressure dodges quick-fried vacuum degree
0.100~0.024mBar, more preferably 0.024mBar.The soaking bath of graft reaction is more excellent than being preferably 1:100~1:300
It is selected as 1:200, reaction temperature is preferably 0~4 DEG C, and more preferably 4 DEG C, the reaction time is preferably 12~for 24 hours, more preferably
24h。
In step S5, centrifugal gravity acceleration is preferably 10000g, and the time is preferably 10min, the temperature of freeze-drying preferably-
30~-20 DEG C, more preferably -30 DEG C, vacuum degree are preferably 0.100~0.024mBar, more preferably 0.024mBar, when freeze-drying
Between preferably 3~5d, more preferably 4d.
Embodiment 1:
1,2g regeneration human hair keratin is dissolved completely in 100ml 98% (v/v) formic acid solution, stirs evenly, is spun
Silk liquid;
2, electrostatic spinning is carried out using spinning solution, the specification of syringe used is 10ml, and needle gauge is tack, No. 7 needles;
Electrospinning conditions are voltage 15KV, distance 8cm, sample rate 0.5ml/h, and 30 DEG C of temperature obtain keratin nano fibrous membrane;
3, by keratin nano fibrous membrane with commercially available phosphate buffer (pH7.4) wash to pH be 7.4,37 DEG C of baking 4h it
It handles and activates by plasma processor, the condition of plasma treatment are as follows: gas uses oxygen, processing power 280W, pressure
55Pa, processing time are 15min;
4, the nano fibrous membrane for obtaining step 3 is immersed in containing 200g/L tremella polysaccharides, 80g/L sodium alginate, 2g/L
Rosa Damascana, 2g/L lemon, 2g/L vitamin E, 8g/L vitamin C, 10g/L propylene glycol, 10g/L glycerol, 2g/L are mono- sweet
Progress negative pressure is dodged quick-fried in the phosphate buffer of the pH7.4 of ester and 2g/L cetearyl alcohol alcohol ether, and negative pressure dodges quick-fried vacuum degree and is
0.024mBar carries out graft reaction later, and the soaking bath ratio of graft reaction is 1:200, and soaking temperature is 4 DEG C, and soaking time is
24h;
5, will complete graft reaction nanofiber centrifugation, centrifugal gravity acceleration be 10000g, time 10min, later
Freeze-drying, temperature are -30 DEG C, vacuum degree 0.024mBar, and freeze-drying time is 4d to get nutrition keratin facial mask.
Embodiment 2:
1,1g regeneration human hair keratin is dissolved completely in 100ml 98% (v/v) formic acid solution, stirs evenly, is spun
Silk liquid;
2, electrostatic spinning is carried out using spinning solution, the specification of syringe used is 10ml, and needle gauge is tack, No. 7 needles;
Electrospinning conditions are voltage 12KV, distance 7cm, sample rate 0.3ml/h, and 25 DEG C of temperature obtain keratin nano fibrous membrane;
3, keratin nano fibrous membrane is washed with commercially available phosphate buffer (pH7.4) after being 7.4,45 DEG C of baking 2h to pH
Plasma treated device processing activation, the condition of plasma treatment are as follows: gas uses nitrogen, processing power 250W, pressure
50Pa, processing time are 10min;
4, the nanofiber for obtaining step 3 is immersed in containing 100g/L tremella polysaccharides, 50g/L sodium alginate, 1g/L rose
Rare essential oil, 1g/L lemon, 1g/L vitamin E, 5g/L vitamin C, 5g/L propylene glycol, 5g/L glycerol, 1g/L monoglyceride and
Progress negative pressure is dodged quick-fried in the phosphate buffer of the pH7.4 of 1g/L cetearyl alcohol alcohol ether, and negative pressure dodges quick-fried vacuum degree and is
0.100mBar carries out graft reaction later, and the soaking bath ratio of graft reaction is 1:100, and soaking temperature is 0 DEG C, and soaking time is
12h;
5, will complete graft reaction nanofiber centrifugation, centrifugal gravity acceleration be 10000g, time 10min, later
Freeze-drying, temperature are -20 DEG C, vacuum degree 0.100mBar, and freeze-drying time is 3d to get nutrition keratin facial mask.
Embodiment 3:
1,3g regeneration human hair keratin is dissolved completely in 100ml 98% (v/v) formic acid solution, stirs evenly, is spun
Silk liquid;
2, electrostatic spinning is carried out using spinning solution, the specification of syringe used is 10ml, and needle gauge is tack, No. 7 needles;
Electrospinning conditions are voltage 20KV, distance 10cm, sample rate 1.0ml/h, and 35 DEG C of temperature obtain keratin nanofiber
Film;
3, keratin nano fibrous membrane is washed with commercially available phosphate buffer (pH7.4) after being 7.4,37 DEG C of baking 4h to pH
Plasma treated device processing activation, the condition of plasma treatment are as follows: gas uses oxygen, processing power 300W, pressure
60Pa, processing time are 15min;
4, the nanofiber for obtaining step 3 is immersed in containing 300g/L tremella polysaccharides, 100g/L sodium alginate, 3g/L
Rosa Damascana, 3g/L lemon, 3g/L vitamin E, 10g/L vitamin C, 15g/L propylene glycol, 15g/L glycerol, 5g/L are mono- sweet
Progress negative pressure is dodged quick-fried in the phosphate buffer of the pH7.4 of ester and 5g/L cetearyl alcohol alcohol ether, and negative pressure dodges quick-fried vacuum degree and is
0.024mBar carries out graft reaction later, and the soaking bath ratio of graft reaction is 1:300, and soaking temperature is 4 DEG C, and soaking time is
24h;
5, will complete graft reaction nanofiber centrifugation, centrifugal gravity acceleration be 10000g, time 10min, later
Freeze-drying, temperature are -30 DEG C, vacuum degree 0.024mBar, and freeze-drying time is 5d to get nutrition keratin facial mask.
Comparative example 1:
1,2g regeneration human hair keratin is dissolved completely in 100ml 98% (v/v) formic acid solution, stirs evenly, is spun
Silk liquid;
2, electrostatic spinning is carried out using spinning solution, the specification of syringe used is 10ml, and needle gauge is tack, No. 7 needles;
Electrospinning conditions are voltage 15KV, distance 8cm, sample rate 0.5ml/h, and 30 DEG C of temperature obtain keratin nano fibrous membrane;
3, by keratin nano fibrous membrane with commercially available phosphate buffer (pH7.4) wash to pH be 7.4,37 DEG C of baking 4h it
It handles and activates by plasma processor, the condition of plasma treatment are as follows: gas uses oxygen, processing power 280W, pressure
55Pa, processing time are 15min;
4, the nano fibrous membrane for obtaining step 3, which is immersed in the phosphate buffer of pH7.4, carries out quick-fried, the negative pressure of negative pressure sudden strain of a muscle
Dodging quick-fried vacuum degree is 0.024mBar, carries out graft reaction later, the soaking bath ratio of graft reaction is 1:200, and soaking temperature is
4 DEG C, soaking time is for 24 hours;
5, will complete graft reaction nanofiber centrifugation, centrifugal gravity acceleration be 10000g, time 10min, later
Freeze-drying, temperature are -30 DEG C, vacuum degree 0.024mBar, and freeze-drying time is a kind of nanofiber of the 4d to get plasma treatment
Facial mask.
Comparative example 2:
1,2g regeneration human hair keratin is dissolved completely in 100ml 98% (v/v) formic acid solution, stirs evenly, is spun
Silk liquid;
2, electrostatic spinning is carried out using spinning solution, the specification of syringe used is 10ml, and needle gauge is tack, No. 7 needles;
Electrospinning conditions are voltage 15KV, distance 8cm, sample rate 0.5ml/h, and 30 DEG C of temperature obtain keratin nano fibrous membrane;
3, by keratin nano fibrous membrane with commercially available phosphate buffer (pH7.4) wash to pH be 7.4,37 DEG C of baking 4h it
It handles and activates by plasma processor, the condition of plasma treatment are as follows: gas uses oxygen, processing power 280W, pressure
55Pa, processing time are 15min;
4, the nano fibrous membrane for obtaining step 3 is immersed in containing 200g/L tremella polysaccharides, 80g/L sodium alginate, 2g/L
Rosa Damascana, 2g/L lemon, 2g/L vitamin E, 8g/L vitamin C, 10g/L propylene glycol, 10g/L glycerol, 2g/L are mono- sweet
Graft reaction is carried out in the phosphate buffer of the pH7.4 of ester and 2g/L cetearyl alcohol alcohol ether, the soaking bath ratio of graft reaction is 1:
200, soaking temperature is 4 DEG C, and soaking time is for 24 hours;
5, will complete graft reaction nanofiber centrifugation, centrifugal gravity acceleration be 10000g, time 10min, later
Freeze-drying, temperature are -30 DEG C, vacuum degree 0.024mBar, and freeze-drying time is 4d to get a kind of plasma surface grafting skin battalion
Support the nanofiber facial mask of the factor.
Comparative example 3:
1,2g regeneration human hair keratin is dissolved completely in 100ml 98% (v/v) formic acid solution, stirs evenly, is spun
Silk liquid;
2, electrostatic spinning is carried out using spinning solution, the specification of syringe used is 10ml, and needle gauge is tack, No. 7 needles;
Electrospinning conditions are voltage 15KV, distance 8cm, sample rate 0.5ml/h, and 30 DEG C of temperature obtain keratin nano fibrous membrane;
3, washing keratin nano fibrous membrane to pH with commercially available phosphate buffer (pH7.4) is 7.4,37 DEG C of baking 4h;
4, the nano fibrous membrane for obtaining step 3 is immersed in containing 200g/L tremella polysaccharides, 80g/L sodium alginate, 2g/L
Rosa Damascana, 2g/L lemon, 2g/L vitamin E, 8g/L vitamin C, 10g/L propylene glycol, 10g/L glycerol, 2g/L are mono- sweet
Progress negative pressure is dodged quick-fried in the phosphate buffer of the pH7.4 of ester and 2g/L cetearyl alcohol alcohol ether, and negative pressure dodges quick-fried vacuum degree and is
0.024mBar carries out graft reaction later, and the soaking bath ratio of graft reaction is 1:200, and soaking temperature is 4 DEG C, and soaking time is
24h;
5, will complete graft reaction nanofiber centrifugation, centrifugal gravity acceleration be 10000g, time 10min, later
Freeze-drying, temperature are -30 DEG C, vacuum degree 0.024mBar, and freeze-drying time is 4d to get a kind of surface grafting skin nutrition factors
Nanofiber facial mask.
Fibroblast proliferation experiment:
Keratin nanofiber facial mask in embodiment and comparative example is laid on 96 hole board bottoms, then by mouse L929 at fiber
Cell is with 1 × 105The density plantation of/ml is placed in 5%CO in 96 orifice plates, every 100 μ l of hole, every group of 5 multiple holes2, 37 DEG C of constant temperature trainings
It supports to cultivate in case and absorbs culture solution afterwards for 24 hours, the MTT (5mg/ml) that 20 μ L are made into PBS is added in every hole, is placed in 5%CO2、37
3h in DEG C constant incubator shakes 10min after 150 μ l DMSO are added, and is placed in microplate reader 570nm and reads absorbance OD value, finds out
Each group OD average value, judges cell proliferative conditions.
From figure 1 it appears that the keratin nanofiber facial mask of each embodiment, can effectively facilitate fibroblast
Proliferation, effect promote the effect of cell Proliferation better than comparative example.The result shows that keratin nanofiber prepared by the present invention face
Film can effective activation Skin Cell, boost metabolism.
The application method of facial mask of the present invention: product pours into 20-30ml pure water or nothing in use, only need to open packaging
Bacterium water, place 3-5min, facial mask will rapid rehydration, then by facial mask apply carry out normal skin nursing on the skin,
4 DEG C of storages are put into after used, may be reused 3-5 times.
Total number of bacterial colonies when table 1 is reused
|
Access times |
Measurement result (CFU/g) |
|
Access times |
Measurement result (CFU/g) |
Embodiment 1 |
1 |
<10 |
Comparative example 1 |
1 |
<10 |
|
3 |
<10 |
|
3 |
8000 |
|
5 |
<10 |
|
5 |
>10000 |
Embodiment 2 |
1 |
<10 |
Comparative example 2 |
1 |
<10 |
|
3 |
<10 |
|
3 |
5000 |
|
5 |
40 |
|
5 |
>10000 |
Embodiment 3 |
1 |
<10 |
Comparative example 3 |
1 |
<10 |
|
3 |
<10 |
|
3 |
2000 |
|
5 |
60 |
|
5 |
>10000 |
As shown in Table 1, in the case where repeating 3-5 use, nutrition keratin facial mask bacterium base prepared by the present invention
Originally it stops growing, illustrates that its trophic factors is not utilized the matter that concurrently changes, and the facial mask bacterium raised growth of comparative example, explanation
Its trophic factors is absorbed and utilized and is occurred rotten by bacterium.
The above is only a preferred embodiment of the present invention, it is noted that come for those of ordinary skill in the art
It says, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications should also regard
For protection scope of the present invention.