CN110772447B - Method for preparing silymarin skin care product - Google Patents
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- CN110772447B CN110772447B CN201911291865.7A CN201911291865A CN110772447B CN 110772447 B CN110772447 B CN 110772447B CN 201911291865 A CN201911291865 A CN 201911291865A CN 110772447 B CN110772447 B CN 110772447B
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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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/49—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
- A61K8/4973—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with oxygen as the only hetero atom
- A61K8/498—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with oxygen as the only hetero atom having 6-membered rings or their condensed derivatives, e.g. coumarin
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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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/34—Alcohols
- A61K8/345—Alcohols containing more than one hydroxy group
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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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/40—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
- A61K8/41—Amines
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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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/64—Proteins; Peptides; Derivatives or degradation products thereof
- A61K8/65—Collagen; Gelatin; Keratin; Derivatives or degradation products thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
- A61Q17/04—Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning preparations
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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
- A61Q19/08—Anti-ageing preparations
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/82—Preparation or application process involves sonication or ultrasonication
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Abstract
The invention discloses a method for preparing a silymarin skin care product, which comprises the steps of dissolving silymarin and meglumine in absolute ethyl alcohol, heating, and then recovering the absolute ethyl alcohol to obtain a silymarin meglumine raw material; mixing with deionized water, stirring in a stirrer, adding gelatin and glycerol, stirring, adding sodium benzoate, and ultrasonic processing to obtain the desired silymarin skin care product. The invention overcomes the defects that the skin care product is too much in facial skin grease and pores are blocked due to long-term use of the traditional skin care product which is brought by directly adopting silymarin to prepare the related skin care product; and the silymarin meglumine and sodium benzoate are uniformly distributed in other matrixes by an ultrasonic uniformly mixing technology, and the silymarin meglumine cannot be decomposed and damaged.
Description
Technical Field
The invention relates to the field of skin care products, in particular to a preparation method of a silymarin skin care product.
Background
Research data show that silymarin has anti-aging and anti-radiation effects clinically, according to the above effect characteristics of silymarin, many research units at home and abroad actively develop the research of silymarin for cosmetic skin care products, at present, although the technical requirement that cosmetics are not layered in a container is solved through the technology of coating the silymarin with water and oil, the method of coating with water and oil only can solve the separation of macromolecular of silymarin due to the special property of fat-soluble substances, and cannot fundamentally change the characteristic that silymarin is not beneficial to skin absorption, and the current silymarin skin care products have the following problems: (1) silymarin is distributed unevenly and unstably in the cosmetic matrix; (2) has the problems of difficult absorption by skin and easy blockage of skin pores after long-term use.
Disclosure of Invention
The invention aims to: in order to overcome the defects in the prior art, the invention provides a preparation method of a silymarin skin care product, which not only fundamentally solves the problem that the silymarin is insoluble in skin and is absorbed, but also is easy to master and popularize in the whole production process.
The technical scheme is as follows: in order to solve the technical problems, the technical scheme adopted by the invention is as follows: a method for preparing silymarin skin care product comprises the following steps:
(1) firstly, weighing 1 part of silymarin and 0.2-0.5 part of meglumine by weight, dissolving in absolute ethyl alcohol which is 3-5 times of the total weight of the silymarin and the meglumine, heating to slightly boil, and keeping for 40-50 min to obtain a solution A;
(2) recovering absolute ethyl alcohol in the solution A to obtain a silymarin meglumine raw material;
(3) weighing the silymarin meglumine raw material and deionized water according to the weight ratio of 1 (5-12), uniformly mixing, and placing in a stirrer for stirring for 5-10 min to obtain a solution B;
(4) adding gelatin with the weight 2-3 times of that of silymarin meglumine and glycerol with the weight 5-7 times of that of the silymarin meglumine into the solution B, and stirring for 10-15 min;
(5) and adding sodium benzoate with the weight of 0.01-0.003 times of that of the silymarin meglumine into the stirred solution, and putting the solution into an ultrasonic mixer for ultrasonic treatment for 20-40 min to obtain the silymarin skin care product.
Further, the method for recovering the absolute ethyl alcohol in the step (2) is as follows:
A) adding the solution A into a rotary water bath film evaporator, heating at 70-100 ℃ and rotating at the rotating speed of 60-100 r/min; after the solution starts to reflux, opening vacuum with the vacuum degree of more than-0.06 MPa, recovering ethanol, and heating and selecting simultaneously;
B. closing vacuum, heating at 100 deg.C, rotating at a rotating speed until the silymarin meglumine solution becomes pasty, and vacuum filtering to remove all ethanol in the silymarin meglumine solution;
C. taking completely dried crisp silymarin meglumine, and crushing to 60-80 meshes of water to obtain a silymarin meglumine fine powder raw material for later use.
Furthermore, the stirring speed in the step (3) is 50-70 r/min.
Furthermore, the stirring speed in the step (4) is 150-200 r/min.
Furthermore, the ultrasonic treatment frequency in the step (5) is 35-45 Hz.
Furthermore, the ultrasonic treatment temperature in the step (5) is 25-35 ℃.
Has the advantages that: the invention has the following advantages: 1) the technical problem of the preparation and application of the skin care product caused by the water insolubility of the silymarin is solved, the silymarin is easily absorbed by the skin, and the phenomenon of blocking skin pores is avoided after long-term use; 2) in the prepared silymarin skin care product, silymarin is uniformly distributed in a skin care product matrix, and is stable and not layered; 3) by ultrasonic solubilization technology, the technical problem that silymarin meglumine is unstable in glyceryl is solved; meanwhile, the damage of the effective components of the silymarin caused by the action of ultrasonic waves is avoided.
Detailed Description
The present invention will be described in further detail with reference to the following examples:
the sources of drug drugs used in the examples are as follows:
silymarin: jiangsu Zhongxing pharmaceutical Co., Ltd
Meglumine: suzhou Jing pharmaceutical chemical Co., Ltd
Anhydrous ethanol: taicanxintai alcohol Co Ltd
Sodium benzoate: environmental protection science and technology Limited of Kamike Shandong
Gelatin: suqian Nanxiang chemical manufacturing Co., Ltd
Glycerol: henan Yuan Gao chemical products Co Ltd
Example 1:
a method for preparing silymarin skin care product comprises the following steps:
silymarin: 100g
Meglumine: 20g of
Anhydrous ethanol: 300g
Deionized water: 600g
Gelatin: 240g
Glycerol: 600g
Sodium benzoate: 1.2 g;
the preparation method comprises the following steps:
(1) weighing 100g of silymarin and 20g of meglumine, dissolving in 300g of absolute ethanol, and slightly boiling for 40 min;
(2) recovering absolute ethyl alcohol in the silymarin meglumine absolute ethyl alcohol solution:
A) adding silymarin meglumine solution into a rotary water bath film evaporator, heating at 70 deg.C while rotating at a speed of 60r/min, opening vacuum degree of-0.06 MPa after the solution begins to reflux, recovering ethanol, and heating and selecting simultaneously;
B) heating at 100 deg.C, rotating at a rotating speed until the silymarin meglumine solution becomes paste, and vacuum filtering to remove all ethanol in the silymarin meglumine solution;
C) taking completely dried crisp silymarin meglumine, and crushing to 60-mesh water to obtain a silymarin meglumine fine powder raw material for later use to obtain 115g of the silymarin meglumine raw material;
(3) 115g of silymarin meglumine raw material and 575g of deionized water are added into a stirrer at the same time, and stirred for 5min at the speed of 50r/min, so as to obtain 690g of silymarin meglumine deionized water solution.
(4) Adding 240g gelatin and 600g glycerol into 690g silymarin meglumine deionized water solution, stirring to obtain emulsion, and controlling rotation speed at 150r/min for 10 min;
(5) 1530g of the milky liquid is added with 1.2g of sodium benzoate and put into an ultrasonic mixer; regulating frequency to 35Hz, temperature to 25 deg.C, and ultrasonic controlling for 20min to obtain 1531g of herba Silybi Mariani skin care product.
Example 2:
a method for preparing silymarin skin care product comprises the following steps:
silymarin: 100g
Meglumine: 30g of
Anhydrous ethanol: 520g
Deionized water: 1250g
Gelatin: 400g
Glycerol: 1000g
Sodium benzoate: 1g of a compound;
the preparation process comprises the following steps:
(1) weighing 100g of silymarin and 30g of meglumine, dissolving in 520g of absolute ethanol, and slightly boiling for 45 min;
(2) recovering absolute ethyl alcohol in the silymarin meglumine absolute ethyl alcohol solution:
A) adding silymarin meglumine solution into a rotary water bath film evaporator, heating at 80 deg.C while rotating at a rotation speed of 70r/min, opening vacuum after the solution begins to reflux, recovering ethanol under a vacuum degree of-0.07 MPa, and heating and selecting simultaneously;
B) heating at 100 deg.C, rotating at a rotating speed until the silymarin meglumine solution becomes paste, and vacuum filtering to remove all ethanol in the silymarin meglumine solution;
C) taking completely dried crisp silymarin meglumine, and crushing to 70-mesh water to obtain a silymarin meglumine fine powder raw material for later use to obtain 125g of silymarin meglumine raw material;
(3) 125g of silymarin meglumine raw material and 1250g of deionized water are added into a stirrer at the same time, and stirred for 7min at the speed of 60r/min, so that 1375g of silymarin meglumine deionized water solution is obtained.
(4) Adding 400g gelatin and 1000g glycerol into 1375g silymarin meglumine deionized water solution, stirring to obtain emulsion, and controlling rotation speed at 170r/min for 13 min;
(5) adding 1g of sodium benzoate into 2775g of the emulsion liquid, and putting into an ultrasonic mixer; regulating frequency to 40Hz, temperature to 30 deg.C, and ultrasonic controlling for 30min to obtain herba Silybi Mariani skin care product 2776 g.
Example 3:
a method for preparing silymarin skin care product comprises the following steps:
silymarin: 100g
Meglumine: 50g
Anhydrous ethanol: 750g
Deionized water: 1800g
Gelatin: 450g
Glycerol: 1050g
Sodium benzoate: 0.45 g;
the process comprises the following steps:
(1) weighing 100g silymarin and 50g meglumine, dissolving in 750g anhydrous ethanol, and slightly boiling for 50 min;
(2) recovering absolute ethyl alcohol in the silymarin meglumine absolute ethyl alcohol solution:
A) adding silymarin meglumine solution into a rotary water bath film evaporator, heating at 100 deg.C while rotating at 100r/min until the solution begins to reflux, opening vacuum degree of-0.08 MPa, recovering ethanol, heating and selecting simultaneously;
B) heating at 100 deg.C, rotating at a rotating speed until the silymarin meglumine solution becomes paste, and vacuum filtering to remove all ethanol in the silymarin meglumine solution;
C) taking completely dried crisp silymarin meglumine, and crushing to 80-mesh water to obtain a silymarin meglumine fine powder raw material for later use to obtain 145g of silymarin meglumine raw material;
(3) 145g of silymarin meglumine raw material and 1800g of deionized water are added into a stirrer at the same time, and stirred for 10min at the speed of 70r/min, so that 1940g of silymarin meglumine deionized water solution is obtained.
(4) Adding 450g gelatin and 1050g glycerol into 1940g silymarin meglumine deionized water solution, stirring to obtain emulsion, and controlling rotation speed at 200r/min for 15 min;
(5) adding 3440g of the above emulsion into 0.45g of sodium benzoate, and placing into an ultrasonic mixer; regulating frequency to 45Hz, temperature to 35 deg.C, and ultrasonic controlling for 40min to obtain skin care product 3440g of herba Silybi Mariani.
Comparative example 1:
the amount of the selected materials and the preparation method are the same as those in example 1, except that meglumine is not used, which is as follows:
(1) weighing 100g of completely dried silymarin, and crushing to 60-mesh water to obtain a silymarin fine powder raw material for later use;
(2) 100g of silymarin raw material and 575g of deionized water are added into a stirrer at the same time, and stirred for 5min at the speed of 50r/min, so that 675g of silymarin deionized water solution is obtained.
(3) Adding 240g of gelatin and 600g of glycerin into 675g of silymarin deionized water solution, and stirring to obtain emulsion, wherein the rotation speed is controlled at 150r/min for 10 min;
(4) adding 1515g of the above milky liquid into 1.2g of sodium benzoate, and placing into an ultrasonic mixer; regulating frequency to 35Hz, temperature to 25 deg.C, and ultrasonic controlling for 20min to obtain silymarin skin care product 1515 g.
Comparative example 2:
the amount of the selected materials and the preparation method are the same as those in example 2, except that the ultrasonic time, frequency and temperature in step (5) are different, as follows:
(1) weighing 100g of dried silymarin, and crushing to 70-mesh water to obtain a silymarin raw material for later use;
(2) adding silymarin 100g and deionized water 1200g into a stirrer simultaneously, and stirring at 60r/min for 7min to obtain silymarin deionized water solution 1300 g.
(4) Adding 300g of gelatin and 700g of glycerol into 1300g of silymarin deionized water solution, and stirring to obtain emulsion, wherein the rotation speed is controlled at 170r/min and the time is 13 min;
(5) adding 1g of sodium benzoate into 2300g of the emulsion, and putting into an ultrasonic mixer; regulating frequency to 50Hz, temperature to 20 deg.C, and ultrasonic controlling for 45min to obtain herba Silybi Mariani skin care product 2301 g.
The silymarin skin care products prepared in examples 1-3 and comparative examples 1-2 were analyzed as shown in table 1:
TABLE 1 analytical comparison of example 2 with comparative examples 1-2
And (4) supplementary notes: the method for detecting the content of the silibinin soluble in water comprises the following steps: mixing 30g of silymarin skin care product and 100g of water uniformly, stirring (rotating speed of 100r/min) for 10min, standing for half an hour, placing the upper layer solution in a vacuum drying oven to dry, measuring the mass of the dried substance, and measuring the content of silybin (the effective component in silymarin is silybin) which can also be dissolved in water according to the weight ratio (the weight ratio of silybin to 30g of cosmetics) to calculate the content of water-soluble silybin in the cosmetics.
As can be seen from the table 1, the preparation method of the silymarin skin care product solves the defects that the facial skin is too greasy and pores are blocked due to long-term use of the skin care product caused by directly adopting silymarin to prepare the related skin care product in the prior art. The silymarin meglumine and sodium benzoate are uniformly distributed in other matrixes by an ultrasonic mixing technology, the silymarin meglumine cannot be decomposed and damaged, and the ultrasonic frequency, the ultrasonic temperature control and the stirring time control also play the best role in ensuring the stability and the mixing degree of the matrixes. The finished skin care product obtained by not adding meglumine in comparative example 1 has poor water solubility, and the ultrasonic treatment parameters of comparative example 2 also have adverse effects on the water solubility characteristics of the silybin skin care product.
Claims (4)
1. A preparation method of a silymarin skin care product is characterized by comprising the following steps:
(1) firstly, weighing 1 part of silymarin and 0.2-0.5 part of meglumine by weight, dissolving in absolute ethyl alcohol which is 3-5 times of the total weight of the silymarin and the meglumine, heating to slightly boil, and keeping for 40-50 min to obtain a solution A;
(2) recovering absolute ethyl alcohol in the solution A to obtain a silymarin meglumine raw material;
(3) weighing the silymarin meglumine raw material and deionized water according to the weight ratio of 1 (5-12), uniformly mixing, and placing in a stirrer for stirring for 5-10 min to obtain a solution B;
(4) adding gelatin and glycerol into the solution B, wherein the weight of the gelatin is 2-3 times that of silymarin meglumine, and the gelatin is 5-7 times that of the silymarin meglumine, and stirring for 10-15 min;
(5) adding sodium benzoate with the weight of 0.01-0.003 times of that of silymarin meglumine into the stirred solution, and putting the solution into an ultrasonic mixer for ultrasonic treatment for 20-40 min to obtain the silymarin skin care product; the ultrasonic treatment frequency is 35-45 Hz, and the ultrasonic treatment temperature is 25-35 ℃.
2. The method for preparing a silymarin skin care product according to claim 1, wherein the silymarin skin care product comprises the following steps: the method for recovering the absolute ethyl alcohol in the step (2) is as follows:
A. adding the solution A into a rotary water bath film evaporator, heating at 70-100 ℃ and rotating at the rotating speed of 60-100 r/min; after the solution starts to reflux, opening vacuum with the vacuum degree of more than-0.06 MPa, recovering ethanol, and heating and rotating simultaneously;
B. closing vacuum, heating at 100 deg.C, rotating at a rotating speed until the silymarin meglumine solution becomes pasty, and vacuum filtering to remove all ethanol in the silymarin meglumine solution;
C. taking the completely dried crisp silymarin meglumine, and crushing to 60-80 meshes to obtain a fine silymarin meglumine powder raw material for later use.
3. The method for preparing a silymarin skin care product according to claim 1, wherein the silymarin skin care product comprises the following steps: in the step (3), the stirring speed is 50-70 r/min.
4. The method for preparing a silymarin skin care product according to claim 1, wherein the silymarin skin care product comprises the following steps: in the step (4), the stirring speed is 150-200 r/min.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101019859A (en) * | 2007-03-16 | 2007-08-22 | 李宝 | Water soluble silymarin and its prepn |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101019859A (en) * | 2007-03-16 | 2007-08-22 | 李宝 | Water soluble silymarin and its prepn |
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