CN1183271A - Collagen E milk and preparing method thereof - Google Patents
Collagen E milk and preparing method thereof Download PDFInfo
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- CN1183271A CN1183271A CN 96120783 CN96120783A CN1183271A CN 1183271 A CN1183271 A CN 1183271A CN 96120783 CN96120783 CN 96120783 CN 96120783 A CN96120783 A CN 96120783A CN 1183271 A CN1183271 A CN 1183271A
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- collagen
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Abstract
A collagen E milk is prepared through loading sodium laurylsulfate, triethanolamine, glycerine, ethyl hydroxybenzoate and distilled water in a container, heating until they are fully dissolved, maintaining temp at 70 deg. C, heating white beeswax and hexadecanol until fusion, slowly adding to the container, continuous grinding in same direction, cooling, addition of collagen and VE and grinding.
Description
The invention provides skin care item, specifically be meant a kind of collagen E milk and preparation method thereof.
Collagen protein is the new type of cosmetic cosmetics that current international aesthetic field is popular and praise highly, skin is had significantly moisten, brighten, anti-ageing and wrinkle removing effect.Collagen protein is a kind of extracellular matrix, is the stock that corium reproduces and grows in the human body skin structure.Because repairing and moist effect that it is peculiar to skin have the favorable tissue compatibility again concurrently, are widely used in world today's shaping and beauty circle.1931, be used for the filling shaping and beauty first in the U.S., be mainly used in facial cicatrix, atrophy, the nasolabial fold wrinkle, glabella, mouthful between, the wrinkle around the eye socket etc., only in the period of 1981-1985 five, in 150,000 person-times, obtain remarkable effect, and obtain the licence that FDA Food and Drug Administration issues.The domestic face crinkle-removing that carries out of being used for is in recent years corrected good in more than 90% in 123 examples.Draw again later on and be applied to medical circle deeply, be mixed with cream and gelatum agent is used for acne outward, erythra, the cicatrix that burn, purport rises after the wound and because the soft tissue atrophy due to the infection, stimulation, illumination etc. with it.According to prominent domestic burn expert report: the gel for treating of in 337 routine shallow II degree-deep ii degree burn patients, using collagen protein, average every example has been used 3-4 time, and slough is dissolved rapidly, the wound surface cleaning, inflammation alleviates, and healing time shifts to an earlier date 3.4-4.5 days respectively than other method therapist.Another report, the patient uses the former albumen cream of magnetic behind the burn of 150 examples, confirms that also it has remarkable curative effect.Collagen protein has good biological action; The overall process that heals after its participation skin and the tissue injury promotes epithelial adhesion differentiation, accelerates epithelial growth speed, accelerates tissue repair; Collagen protein also has the barrier action of organizing in addition, increases the hydration levels of skin and collenchyme, keeps the skin wet, and increases the fine and close and soft of skin, so that skin of face exquisiteness, brilliant white.Clean.Natural Vitamin E comes from the plumule of Semen Tritici aestivi and beans in addition, is one of necessary vitamin of human body, and the adult needs to be 25-100mg in amount every day.It influences reproductive function, lipid metabolism, cell senescence and the circulatory function of human body.The animal genitals is impaired during shortage, arteriosclerosis and erythrocyte embrittlement.But even more important effect is the old and feeble effect of its anti-tissue of a large amount of reports in recent years.There are two according to certified its antidotal basic point: the one, can prevent or suppress the peroxidating of human body cell film adipose membrane, reduce the content of senescence-factor lipofuscin in the cell, and reduce the accumulation of pigment in the human body cell; The 2nd, vitamin E can also suppress another factor of human senility, promptly reduces the interior free yl reaction, cushions the damage that the radical pair body causes, and can improve the circulation and the oxygen supply state of local blood capillary.Domestic, outer expert uses vitamin E antagonism human senility, has obtained good effect, and the relevant expert also uses vitamin E cream external curing 30 examples by the senile keratotic plaque due to the aging, and effective percentage reaches 94%.In addition, because collagen protein has the faint antigenicity and the favorable tissue compatibility, vitamin E is again the vitamin of needed by human body, thereby can not cause tissue reaction or inflammation, does not have to cause anaphylaxis, no cytotoxicity.
The object of the present invention is to provide a kind of skin care item and preparation method thereof, specifically be meant a kind of collagen E milk and preparation method thereof.
The composition of collagen E milk provided by the present invention comprises: collagen protein, vitamin E, cera alba, hexadecanol, sodium lauryl sulphate, triethanolamine, glycerol, ethyl hydroxybenzoate, distilled water;
The composition proportioning of wherein said collagen E milk is:
Form proportioning (ratio of weight and number)
Collagen protein Collagou 0.05-0.25 part;
Vitamin E Vitamin E 1-3 part;
Cera alba White Wax 1-3 part;
Hexadecanol Cetyl Alcohol 7-13 part;
Sodium lauryl sulphate Sodium Lanyl Sulfate 0.5-2 part;
Triethanolamine Triethanolamine 0.5-2 part;
Glycerol Glycerin 7-13 part;
Ethyl hydroxybenzoate Ethylparaben 0.05-0.25 part;
Distilled water Water Destikkate surplus;
Make 100 parts altogether.
The composition proportioning of wherein said collagen E milk is:
Form proportioning (ratio of weight and number)
0.15 part of collagen protein Collagon;
2 parts of vitamin E Vitamin E;
2 parts of cera alba White Wax;
10 parts of hexadecanol Cetyl Alcohol;
1 part of sodium lauryl sulphate Sodium Lanyl Sulfate;
1 part of triethanolamine Triethanolamine;
10 parts of glycerol Glycerin;
0.1 part of ethyl hydroxybenzoate Ethylparaben;
Distilled water Water Destikkate surplus;
Make 100 parts altogether.
The preparation method of collagen E milk provided by the present invention comprises: take by weighing sodium lauryl sulphate, triethanolamine, glycerol, ethyl hydroxybenzoate and distilled water by said ratio and put in the adaptation container, be heated to whole dissolvings and be incubated about about 70 ℃; After other gets cera alba, hexadecanol heating and melting, keep slowly joining in the water tank with the proximate temperature of last liquid, constantly grind according to same direction, closely add collagen protein when cold, vitamin E grinds even.
Collagen E milk quality standard provided by the present invention
Character: white emulsifiable paste has slight fragrance.
Differentiate
(vitamin E)
Get the about 1g of this product, add dehydrated alcohol 10ml dissolving after, under wavelength 231nm, show absorption maximum.Check
The uniformity: should be even, exquisiteness is applied to and answers nonirritant on the skin, and should have suitable toughness, is easy to be coated with on skin or the mucosa.
Acidity: PH5.0～8.0
Content uniformity: get 3～5 of test samples, weight decided in the precision title, obtains the loading amount and average loading amount of each container contents, and average loading amount is no less than 95% of sign loading amount, and each container loading amount is no less than 90% of sign loading amount.
Microbial standard:
Total number of bacteria: every gram should be less than 10
Excrement colibacillus group: must not detect
Bacillus pyocyaneus: must not detect
Staphylococcus aureus: must not detect
The hygienic chemistry standard:
Hydrargyrum is got the 1g sample determination should be lower than 0.01ppm
Arsenic is got the 1g sample determination should be lower than 0.5ppm
Lead is got the 1g sample determination should be lower than 4ppm
Assay:
1 instrument and reagent
7530 type ultraviolet spectrophotometers, Shanghai analytical tool factory; The vitamin E standard substance, Chinese biological goods calibrating institute; The vitamin E raw material, Shenyang pharmaceutical factory; Dehydrated alcohol GR level.
The preparation of 2 test solutions
2.1VE the preparation of standard solution, precision take by weighing VE standard substance 2498mg and put in the brown volumetric flask of 100ml, with anhydrous alcohol solution and be diluted to scale, shake up standby.
2.2 the preparation of matrix solution is at first made cream base in the prescription ratio, smart again its substrate 0.3803g that claims puts in the 100ml volumetric flask, with anhydrous alcohol solution and be diluted to scale, jolting 15min leaves standstill with sudden force, filters with dry filter paper, discard filtrate just, the subsequent filtrate filter is to clarification.
2.3 the smart collagen E Emulsion 0.3873g that makes with above-mentioned substrate that claims of the preparation of emulsion solution puts in the brown volumetric flask of 100ml, by operating of " using dehydrated alcohol ... clarify " under 2.2 clear liquor.
3 measure
3.1 measure the selection of wavelength above-mentioned solution is made blank with anhydrous alcohol solution, carry out spectral scan at 235～300nm place respectively.Slit 1nm, scanning speed 120nm/min must absorb collection of illustrative plates.
Press three-wavelength selection principle, on interference curve one emulsion bases absorption curve, earlier selected A1, A2 point, its pairing wavelength 292.2n and 284.0nm are as measuring wavelength X 1 and λ 2, connect A1, A2 and prolong friendship VE standard substance absorption curve in A3 point (seeing accompanying drawing), the pairing wavelength X 3 of A3 point is defined as 250.9nm after measured, measure the cream of variable concentrations substrate respectively at λ 1, λ 2, λ 3 wavelength places, the result does not have influence (seeing Table 1) to the Δ A value of vitamin E, illustrates that the wavelength selection is correct.
The emulsion bases of table 1 variable concentrations influences VE substrate concentration A292.2 A284.8 A250.9 Δ A (g) (μ g/2.5ml) 2.498 36.880 0.150 0.485 0.274 0.31042.498 51.632 0.155 0.502 0.347 0.30892.498 66.384 0.172 0.529 0.408 0.3101 to VE Δ A measured value
3.2 the preparation of standard curve, precision is drawn VE standard solution 0.8ml, 1.2ml, 1.6ml, 2.0ml, is put in the brown measuring bottle of 50ml respectively, be diluted to scale with dehydrated alcohol, shake up, do blank with dehydrated alcohol, survey trap in three selected skin strong points respectively, calculate Δ A value, try to achieve regression equation C=329.0466A-0.6896 correlation coefficient r=0.9998 through recurrence.VE concentration is good in 39.97～119.90 μ g/ml scope internal linear relation.
3.3 the not commensurability VE standard solution of the accurate absorption of recovery test is put respectively in the brown measuring bottle of 50ml, distinguish the dehydrated alcohol extraction liquid of a certain amount of collagen E milk of finishing again, rare with dehydrated alcohol to scale, shake up with anhydrous second and make blank, survey the trap value respectively at the three-wavelength place, calculate recovery rate (seeing Table 2).
The recovery test of table 2 collagen E milk (n=3)
The numbering input amount amount of recording response rate meansigma methods RSD
(μg/ml) (μg/ml) (％) (％) (％)
1 59.952 60.531 100.97
2 69.944 69.676 99.62
3 79.936 79.841 99.43 100.04 0.72
4 89.928 90.534 100.67
5 99.920 99.416 99.50
It is an amount of that 3.4 sample determination, essence are got various product, put in the brown measuring bottle of 100ml, by operate under the emulsion solution preparation each sample liquid, survey trap at selected three-wavelength place, measurement result sees Table 3.
The assay of vitamin E (N=3) in table 3 sample
Lot number labelled amount actual measured amount is equivalent to labelled amount
(μg/ml) (μg/ml) (％)
960215 80.198 82.991 103.48
960308 102.651 101.656 99.03
960316 75.627 77.435 102.53
960325 100.136 100.869 100.73
The safety evaluatio data of collagen E milk provided by the present invention:
1, collagen protein frost acute dermal toxicity testing data
Purpose: estimate the toxic reaction that collagen E milk transdermal flux and shortterm effect are produced.
Test material: collagen E milk
Animal rat.Beijing animal housing of medicine inspecting institute provides
Test method
Select body weight 200 ± 20g rat for use,, under light, the condition that all is consistent of ingesting, in cage for animal, observed 5 days in room temperature, after be divided into 7 groups at random, 10 every group, male and female half and half, establishing 1～6 group is that the examination that is subjected to of various dose is organized, 7 groups is matched group (excipient).The group spacing is 1: 0.7.Get 1～6 group spinal column diamond wool loss of hairs fallen (3 * 5cm), will be tried thing and evenly be coated on the back, and cover with oilpaper and two-layer gauze and to use immobilization with adhesive tape, drug of topical application 24h.The 7th treated animal coating excipient, method is the same.After gauze is taken off, with the warm water flush away residual tried thing, continue to observe seven days.
The result
Bradykinesia all appears in rat before death, activity is slowed down, righting reflex loss, and stupor is breathed symptoms such as decreased heart rate; Main organs such as the dead rat postmortem and the perusal heart, lung, liver, kidney, blood vessel and tissue there is no unusually.Adopt the BLOSS method to calculate LD
50, the results are shown in Table 1
Table 1 acute toxicity as a result tested material dosage is counted the LD50 of death rate probit and confidence limit to application amount number of animals dead animal, (mg/kg), (*), (only), (only), (%), (y), (mg/kg), (95%) 5,840 3.766 10 10 100 7.4004672 3.670 10 9 90 6.2823796 3.579 10 5 50 5.000 3685 ± 370.62920 3.465 10 2 20 4.1582336 3.368 10 00 2.8001788 3.252 10 00 2.000
2. collagen protein skin irritation test
Purpose: the reversibility inflammation and the irritation that produce behind the evaluating skin contact collagen E milk.
Test material: collagen E milk
Animal table purplish blue rabbit Beijing animal housing of medicine inspecting institute provides.
Test method
Select 12 of the livid purple blue rabbit of body weight 2.5 ± 0.25kg for use, do not have pregnant health, male and female are not limit.Spinal column diamond wool loss of hairs is fallen, about each 4cm * 6cm, behind the rest 24h, be divided into two groups at random, 6 every group.
First group of 1～4 rabbit left side skin of back respectively is coated with the thing that tried of about 0.1g, cover with oilpaper, and with gauze, immobilization with adhesive tape; Right side skin of back coating excipient compares; Remain 2 and make blank.Drug of topical application 24h under the condition of room temperature, light unanimity.Finish the back with the warm water flush away residual tried thing, and in washing back 1h, 24h and 48h observation both sides dermoreaction.
Second group 1～4 rabbit prescription method is the same, and once a day, 14d remains 2 and makes blank continuously, and flush away is tried the thing observing response before administration every day.Drill through the skin of smearing the position after experiment finishes and carry out histopathologic examination.
The result
Acute skin irritation test group (first group) rabbit ridge both sides skin does not all have erythema, edema, and with normal rabbits skin no significant difference, integration is 0, nonirritant, skin irritation intensity score value 0.2.
The wireless speckle of skin irritation test group rabbit ridge left side skin repeatedly, reluctantly visible edema, and normal rabbit skin moisturizing, color is white, the blood capillary visibility is good.Stimulation index is 14 * 1=14.Skin chronic stimulation test total points is 1+8+1=10.Pathologic finding squamous cell form is normal, and keratinization is moderate, does not see necrosis and hyperemia.
3. the skin allergic reaction of collagen E milk test
Purpose: estimate the immune dermoreaction that transmits of cream body generation that repeats to contact collagen protein.
Test material: collagen E milk
Animal Britain pure lines kind of albino guinea-pig Beijing animal housing of medicine inspecting institute provides.
Test method
Select 20 of body weight 250～350g Cavia porcelluss for use, do not have pregnant health, male and female are not limit, and nape left of spine hair are taken off area 3 * 3cm, rest 24h.To be tried thing 0.2g and be coated on 2 * 2cm filter paper, be applied to every Cavia porcellus unhairing district, and, be continued 6h with two-layer gauze, one deck oilpaper, immobilization with adhesive tape.And in kind repeated once in the 7th day and the 14th day.After last sensitization 20 days, get the unhairing district that is tried every Cavia porcellus spinal column right side that thing (tried thing add equivalent substrate grind well) patch loses hair or feathers before 24h after the 0.2g dilution, area 2 * 2cm.With two-layer gauze, one deck oilpaper and non-stimulated immobilization with adhesive tape 6h, take down patch and tried thing, observe dermoreaction behind 24h and the 48h.Under similarity condition, other gets 10 of Cavia porcelluss, by pasting speckle in contrast with quadrat method.
The result
All perpendicular hair, dyspnea, anaphylaxis and death such as sneeze all do not take place in Cavia porcellus.The part is not show speckle and edema as yet.Nonirritant and cause enemy character.
4. human body excites patch test
Purpose: the overall process of simulation human body sensitization, the potential sensitization originality of prediction collagen protein frost.
Test material and experimenter: collagen E milk
30 of experimenter's Beijing Medical University practical teaching students, at 20～25 years old age, the men and women does not limit.
Test method
After inducing with 5% sodium lauryl sulphate liquid, will like that examination thing 0.2g is coated on four layers of gauze of 2 * 2cm size, and apply ointment or plaster and bend on the side skin, cover with cellophane at each experimenter's left forearm, fixing 48h, after remove the patch thing, rest 24h.Repeat above-mentioned steps 4 times.
In inducing back 14 days for the last time, select experimenter's right forearm to bend two of side skins, spacing 3cm, one compares, apply ointment or plaster for one and contain the 1 * 1cm gauze that is tried thing 0.2g, sealing fixedly behind the 48h, removed the patch thing and is observed dermoreaction immediately, and in 24,48 and 72h after the several development and the disappearance situation of observing dermoreaction.
The result
30 routine experimenters' skin is all reactionless, does not all have sensitivity response after exciting after the administration 48h and removing patch thing 24,48 and 72h, confirms that this product is that weak sensitization can be former.
Embodiment 1
Take by weighing sodium lauryl sulphate 100 grams, triethanolamine 100 grams, glycerol 1000 grams, ethyl hydroxybenzoate 10 grams and distilled water and put in the adaptation container, be heated to whole dissolvings and be incubated about about 70 ℃; After other gets cera alba 200 grams, hexadecanol 1000 gram heating and melting, keep slowly joining in the water tank with the proximate temperature of above-mentioned liquid, constantly grind according to same direction, nearly collagen protein 15 grams that add when cold, vitamin E2 00 gram, grind evenly, wherein the water addition is for guaranteeing that the final product amount is 10000 grams.
Claims (4)
1, a kind of collagen E milk, wherein composition comprises: collagen protein, vitamin E, cera alba, hexadecanol, sodium lauryl sulphate, triethanolamine, glycerol, ethyl hydroxybenzoate, distilled water.
2, the described collagen E milk of claim 1, the composition proportioning of wherein said collagen E milk is:
Form proportioning (ratio of weight and number)
Collagen protein Collagon 0.05-0.25 part;
Vitamin E Vitamin E 1-3 part;
Cera alba White Wax 1-3 part;
Hexadecanol Cetyl Alcohol 7-13 part;
Sodium lauryl sulphate Sodium Lanyl Sulfate 0.5-2 part;
Triethanolamine Triethanolamine 0.5-2 part;
Glycerol Glycerin 7-13 part;
Ethyl hydroxybenzoate Ethylparaben 0.05-0.25 part;
Distilled water Water Destikkate surplus;
Make 100 parts altogether.
3, the described collagen E milk of claim 1, the composition proportioning of wherein said collagen E milk is:
Form proportioning (ratio of weight and number)
0.15 part of collagen protein Collagon;
2 parts of vitamin E Vitamin E;
2 parts of cera alba White Wax;
10 parts of hexadecanol Cetyl Alcohol;
1 part of sodium lauryl sulphate Sodium Lanyl Sulfate;
1 part of triethanolamine Triethanolamine;
10 parts of glycerol Glycerin;
0.1 part of ethyl hydroxybenzoate Ethylparaben;
Distilled water Water Destikkate surplus;
Make 100 parts altogether.
4, a kind of method for preparing the described collagen E milk of claim 1, comprising: take by weighing sodium lauryl sulphate, triethanolamine, glycerol, ethyl hydroxybenzoate and distilled water by said ratio and put in the adaptation container, cushioning is to all dissolving and being incubated about about 70 ℃; After other gets cera alba, hexadecanol heating and melting, keep slowly joining in the water tank with the proximate temperature of last liquid, constantly grind according to same direction, closely add collagen protein when cold, vitamin E grinds even.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 96120783 CN1183271A (en) | 1996-11-27 | 1996-11-27 | Collagen E milk and preparing method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 96120783 CN1183271A (en) | 1996-11-27 | 1996-11-27 | Collagen E milk and preparing method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1183271A true CN1183271A (en) | 1998-06-03 |
Family
ID=5126582
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 96120783 Pending CN1183271A (en) | 1996-11-27 | 1996-11-27 | Collagen E milk and preparing method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1183271A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100352423C (en) * | 2005-11-15 | 2007-12-05 | 湖南师范大学 | Skin-care product contg. tortoise skin collagen composition, and its prepn. method |
| CN102988216A (en) * | 2012-11-30 | 2013-03-27 | 兰晶 | Moisturizing and anti-allergic emulsion |
| CN103536469A (en) * | 2013-10-15 | 2014-01-29 | 倪生标 | Skin-moistening lotion |
| CN109846756A (en) * | 2019-02-01 | 2019-06-07 | 重庆工业职业技术学院 | A kind of moisturizing emulsion of the extract containing beeswax and preparation method thereof |
-
1996
- 1996-11-27 CN CN 96120783 patent/CN1183271A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100352423C (en) * | 2005-11-15 | 2007-12-05 | 湖南师范大学 | Skin-care product contg. tortoise skin collagen composition, and its prepn. method |
| CN102988216A (en) * | 2012-11-30 | 2013-03-27 | 兰晶 | Moisturizing and anti-allergic emulsion |
| CN103536469A (en) * | 2013-10-15 | 2014-01-29 | 倪生标 | Skin-moistening lotion |
| CN109846756A (en) * | 2019-02-01 | 2019-06-07 | 重庆工业职业技术学院 | A kind of moisturizing emulsion of the extract containing beeswax and preparation method thereof |
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