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CN-121971344-A - Collagen composite freeze-dried powder for line desalination and preparation and application thereof

CN121971344ACN 121971344 ACN121971344 ACN 121971344ACN-121971344-A

Abstract

The invention relates to the field of freeze-dried powder, and discloses collagen composite freeze-dried powder for fading lines, and a preparation method and application thereof, wherein the collagen composite freeze-dried powder comprises recombinant XVII type humanized collagen, chitosan derivatives, superoxide dismutase, mannitol, plant extracts, palmitoyl pentapeptide-4 and water, wherein the chitosan derivatives are prepared by amidation reaction of carboxymethyl cellulose quaternary ammonium salt and amino chitosan by using 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and N-hydroxysuccinimide as cross-linking agents; the carboxymethyl cellulose quaternary ammonium salt is synthesized by utilizing carboxymethyl cellulose and 3-chloro-2-hydroxypropyl trimethyl ammonium chloride to react in aqueous solution; the amino chitosan is prepared by utilizing the acryloyl chloride to react with chitosan to prepare the acryl chitosan which is continuously subjected to thiol-ene click reaction with beta-mercaptoethylamine, the collagen composite freeze-dried powder prepared by the invention has good anti-wrinkle and tightening effects and antibacterial properties.

Inventors

  • MA PANDENG
  • Liao Xijiao

Assignees

  • 四平华科生物技术有限责任公司

Dates

Publication Date
20260505
Application Date
20260317

Claims (10)

  1. 1. The collagen composite freeze-dried powder for line desalination is characterized by comprising, by weight, 20-30 parts of recombinant XVII type humanized collagen, 10-20 parts of chitosan derivatives, 3-9 parts of superoxide dismutase, 2-5 parts of mannitol, 1-5 parts of plant extracts, 0.5-2 parts of palmitoyl pentapeptide-4, and 60-85 parts of water, The chitosan derivative is prepared by using 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and N-hydroxysuccinimide as cross-linking agents and carrying out amidation reaction on carboxymethyl cellulose quaternary ammonium salt and amino chitosan, wherein the carboxymethyl cellulose quaternary ammonium salt is prepared by using carboxymethyl cellulose as a raw material and using 3-chloro-2-hydroxypropyl trimethyl ammonium chloride as an etherifying agent to react in aqueous solution, and the amino chitosan is prepared by using acryloyl chloride to carry out substitution reaction with chitosan to prepare acrylated chitosan, and then using acrylated chitosan and beta-mercaptoethylamine to carry out thiol-ene click reaction.
  2. 2. The collagen composite freeze-dried powder for line desalination according to claim 1, wherein the plant extract is prepared by mixing black tea extract, red axle extract and pomegranate fruit extract according to a mass ratio of 1-2:1-1.5:1-1.5.
  3. 3. The collagen composite freeze-dried powder for line desalination according to claim 1, wherein the preparation method of the chitosan derivative comprises the following steps: A. adding chitosan and methanesulfonic acid into a reactor under the ice water bath condition, stirring and dissolving, then dropwise adding acryloyl chloride for reaction for 8 hours, and then separating out a reaction solution by using a mixed solution of diethyl ether and acetone to obtain acrylated chitosan; B. Adding acrylated chitosan, beta-mercaptoethylamine and deionized water into a reactor at room temperature, stirring and dissolving, then adding a photoinitiator 2-hydroxy-4' - (2-hydroxyethoxy) -2-methyl propiophenone, reacting for 1h under 365nm ultraviolet lamp irradiation, and then dialyzing with a dialysis bag to obtain aminated chitosan; C. Dispersing carboxymethyl cellulose into a medium of isopropanol and water, adding a sodium hydroxide aqueous solution for alkalizing reaction for 30min, then adding 3-chloro-2-hydroxypropyl trimethyl ammonium chloride, stirring at 60 ℃ for reaction for 2h, cooling the reaction liquid, dialyzing the reaction liquid with distilled water for three days, concentrating by rotary evaporation, and vacuum drying to obtain carboxymethyl cellulose quaternary ammonium salt; D. Adding 2- (N-morpholino) ethanesulfonic acid buffer solution with pH of=6.5 and carboxymethyl cellulose quaternary ammonium salt into a reactor, stirring and mixing, then adding 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and N-hydroxysuccinimide, continuously stirring for 1h, adding aminated chitosan, stirring and reacting for 20-24 h at 35-55 ℃, cooling the reaction liquid, dialyzing the reaction liquid for three days by using distilled water, concentrating by rotary evaporation, and drying in vacuum to obtain the chitosan derivative.
  4. 4. The collagen composite freeze-dried powder for line desalination according to claim 3, wherein the addition ratio of chitosan, methanesulfonic acid and acryloyl chloride in the step a is 4g:30ml:15ml.
  5. 5. The collagen composite freeze-dried powder for line desalination according to claim 3, wherein the mass ratio of the acrylated chitosan, the beta-mercaptoethylamine and the 2-hydroxy-4' - (2-hydroxyethoxy) -2-methylpropenone in the step B is 2:3:0.5.
  6. 6. The collagen composite freeze-dried powder for line desalination according to claim 3, wherein the concentration of the sodium hydroxide aqueous solution in the step C is 0.35-0.4 g/mL, and the addition ratio of the carboxymethyl cellulose, the isopropanol, the water, the sodium hydroxide aqueous solution and the 3-chloro-2-hydroxypropyl trimethyl ammonium chloride is 6g:75mL:25mL:10 mL:5-8 g.
  7. 7. A collagen composite freeze-dried powder for lightening lines according to claim 3, wherein the molar ratio of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride to N-hydroxysuccinimide in the step D is 2:1.
  8. 8. The collagen composite freeze-dried powder for line desalination according to claim 3, wherein the mass ratio of the carboxymethyl cellulose quaternary ammonium salt to the aminated chitosan in the step D is 1:2-3.
  9. 9. A preparation method of the collagen composite freeze-dried powder for desalinating lines according to any one of claims 1-8 is characterized by comprising the steps of weighing all components in parts by weight, uniformly stirring and mixing recombinant XVII type human collagen, chitosan derivatives, superoxide dismutase, mannitol, plant extracts and palmitoyl pentapeptide-4, freezing at-25 to-20 ℃ for 6-10 hours, then freezing at-10 to-5 ℃ for 8-12 hours, then freezing at-22 ℃ for 2-6 hours, finally maintaining at 25-33 ℃ for 4-6 hours, and obtaining the collagen composite freeze-dried powder for desalinating lines, wherein the vacuum degree in the freeze-drying process is 0.6-0.8 mbar.
  10. 10. The use of the collagen composite freeze-dried powder for line desalination according to any one of claims 1 to 8, wherein the collagen composite freeze-dried powder for line desalination is used in skin care products.

Description

Collagen composite freeze-dried powder for line desalination and preparation and application thereof Technical Field The invention belongs to the technical field of freeze-dried powder, and particularly relates to collagen composite freeze-dried powder for grain desalination, and preparation and application thereof. Background Skin protects the human body from harmful and exogenous substances and is the main anatomical barrier of the human body. Skin aging is a biological process in which the skin undergoes degradation, loses physiological function and destroys structural integrity, and presents signs of aging under the influence of internal aging factors and the external environment. External environmental factors such as ultraviolet rays, tobacco, alcohol, diet, etc. can accelerate aging of skin, wherein ultraviolet rays are main factors causing skin damage, which are manifested by skin becoming loose, wrinkles increasing, and elasticity decreasing. The freeze-dried powder is taken as a novel skin care product form, and is favored because of the characteristics of high activity, high stability and the like. However, the existing freeze-dried powder product still has defects in anti-wrinkle and tightening effects, and the effect of skin microecology balance in the anti-aging process is increasingly emphasized, and the colonization and propagation of harmful bacteria can trigger skin micro-inflammatory states, activate inflammatory pathways, accelerate the degradation of collagen and elastin, form malignant circulation of 'inflammation-aging', and the existing freeze-dried powder has no good antibacterial performance, so that the product is limited to be widely applied. Disclosure of Invention In order to solve the defects in the background art, the invention aims to provide collagen composite freeze-dried powder for fading lines, and preparation and application thereof, wherein the prepared collagen composite freeze-dried powder has good anti-wrinkle and tightening effects and antibacterial performance. The aim of the invention can be achieved by the following technical scheme: The collagen composite freeze-dried powder for removing lines comprises, by weight, 20-30 parts of recombinant XVII type human collagen, 10-20 parts of chitosan derivatives, 3-9 parts of superoxide dismutase, 2-5 parts of mannitol, 1-5 parts of plant extracts, 0.5-2 parts of palmitoyl pentapeptide-4, and 60-85 parts of water, The chitosan derivative is prepared by using 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and N-hydroxysuccinimide as cross-linking agents and carrying out amidation reaction on carboxymethyl cellulose quaternary ammonium salt and amino chitosan, wherein the carboxymethyl cellulose quaternary ammonium salt is prepared by using carboxymethyl cellulose as a raw material and using 3-chloro-2-hydroxypropyl trimethyl ammonium chloride as an etherifying agent to react in aqueous solution, and the amino chitosan is prepared by using acryloyl chloride to carry out substitution reaction with chitosan to prepare acrylated chitosan, and then using acrylated chitosan and beta-mercaptoethylamine to carry out thiol-ene click reaction. Preferably, the plant extract is prepared by mixing black tea extract, red axle extract and pomegranate fruit extract according to a mass ratio of 1-2:1-1.5:1-1.5. Preferably, the preparation method of the chitosan derivative comprises the following steps: A. adding chitosan and methanesulfonic acid into a reactor under the ice water bath condition, stirring and dissolving, then dropwise adding acryloyl chloride for reaction for 8 hours, and then separating out a reaction solution by using a mixed solution of diethyl ether and acetone to obtain acrylated chitosan; B. Adding acrylated chitosan, beta-mercaptoethylamine and deionized water into a reactor at room temperature, stirring and dissolving, then adding a photoinitiator 2-hydroxy-4' - (2-hydroxyethoxy) -2-methyl propiophenone, reacting for 1h under 365nm ultraviolet lamp irradiation, and then dialyzing with a dialysis bag to obtain aminated chitosan; C. Dispersing carboxymethyl cellulose into a medium of isopropanol and water, adding a sodium hydroxide aqueous solution for alkalizing reaction for 30min, then adding 3-chloro-2-hydroxypropyl trimethyl ammonium chloride, stirring at 60 ℃ for reaction for 2h, cooling the reaction liquid, dialyzing the reaction liquid with distilled water for three days, concentrating by rotary evaporation, and vacuum drying to obtain carboxymethyl cellulose quaternary ammonium salt; D. Adding 2- (N-morpholino) ethanesulfonic acid buffer solution with pH of=6.5 and carboxymethyl cellulose quaternary ammonium salt into a reactor, stirring and mixing, then adding 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and N-hydroxysuccinimide, continuously stirring for 1h, adding aminated chitosan, stirring and reacting for 20-24 h at 35-55 ℃, cooling the reaction liquid, dialyzing the reac