CN113499279B - Whitening, repairing and anti-aging freeze-dried small milk tablet and preparation process thereof - Google Patents

Whitening, repairing and anti-aging freeze-dried small milk tablet and preparation process thereof Download PDF

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Publication number
CN113499279B
CN113499279B CN202110671538.5A CN202110671538A CN113499279B CN 113499279 B CN113499279 B CN 113499279B CN 202110671538 A CN202110671538 A CN 202110671538A CN 113499279 B CN113499279 B CN 113499279B
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freeze
drying
dried small
parts
filtering
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CN113499279A (en
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邓科宏
范凌志
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Guangdong Hongyi Cosmetics Co ltd
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Guangdong Hongyi Cosmetics Co ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • A61K8/737Galactomannans, e.g. guar; Derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/0208Tissues; Wipes; Patches
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/24Phosphorous; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34Alcohols
    • A61K8/345Alcohols containing more than one hydroxy group
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/36Carboxylic acids; Salts or anhydrides thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/36Carboxylic acids; Salts or anhydrides thereof
    • A61K8/362Polycarboxylic acids
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/36Carboxylic acids; Salts or anhydrides thereof
    • A61K8/365Hydroxycarboxylic acids; Ketocarboxylic acids
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/40Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
    • A61K8/44Aminocarboxylic acids or derivatives thereof, e.g. aminocarboxylic acids containing sulfur; Salts; Esters or N-acylated derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/49Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
    • A61K8/4973Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with oxygen as the only hetero atom
    • A61K8/498Cosmetics 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
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/60Sugars; Derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/64Proteins; Peptides; Derivatives or degradation products thereof
    • A61K8/65Collagen; Gelatin; Keratin; Derivatives or degradation products thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • A61K8/735Mucopolysaccharides, e.g. hyaluronic acid; Derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/84Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/88Polyamides
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/02Preparations for care of the skin for chemically bleaching or whitening the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/08Anti-ageing preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/59Mixtures
    • A61K2800/592Mixtures of compounds complementing their respective functions
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/805Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/84Products or compounds obtained by lyophilisation, freeze-drying

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  • Cosmetics (AREA)
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Abstract

The application relates to the technical field of skin care, in particular to a whitening, repairing and anti-aging freeze-dried small milk tablet and a preparation process thereof. The application provides a whitening, repairing and anti-aging freeze-dried small milk tablet, which is prepared from, by weight, 6-10 parts of an excipient, 0.1-2 parts of a stabilizer, 0.06-0.2 part of a buffer, 0.1-2 parts of a humectant, 1-5 parts of maltose, 0.1-2 parts of a nano-microemulsion and 0.1-2 parts of a mitochondrial activator. By preparing raw materials; preparing a mould; proportioning and filtering; precise sterile filtration; filling; freezing the organism to sleep; drying at low temperature; and (5) demolding to obtain the freeze-dried small milk tablet. The milk slices which cannot be made into the shape of the milk slices by freeze-drying technology in the prior art are easy to break, the complete milk slices can be made into the shape by the application, and the milk slices made by the technology are easy to dissolve in the solvent.

Description

Whitening, repairing and anti-aging freeze-dried small milk tablet and preparation process thereof
Technical Field
The application relates to the technical field of skin care, in particular to a whitening, repairing and anti-aging freeze-dried small milk tablet and a preparation process thereof.
Background
Skin is a barrier for blocking permeation of various molecules, and can prevent invasion of harmful substances or unwanted substances from the outside, and people's skin ages with age and increased environmental irritation, so that skin is dark yellow, has no luster, and has increased wrinkles. Along with the increase of skin aging phenomena of people, various cosmetics in the market are layered endlessly, more than one are skin care products in the form of emulsion and paste, the skin care products in the form of emulsion and paste contain water, the preservation time is very short, and in order to ensure that the skin care products are preserved for a long time, preservatives are often added into the skin care products, but the preservatives have certain stimulation effect on the skin of people and cannot be used for a long time.
With the importance of people on skin care phenomenon, skin care is carried out anytime and anywhere, in order to prepare a skin care product which is convenient to carry and has no preservative, the freeze-drying technology is adopted to solve the problems, but the existing freeze-dried skin care product prepared by the freeze-drying technology is mainly prepared by freeze-dried powder, the active ingredients in the components are less reserved in the process of preparing the freeze-dried powder, the skin care effect of the freeze-dried powder is reduced, and the skin care product is rarely prepared into a small milk tablet shape, mainly because the raw materials and the technology are not mature, and the shape of the prepared freeze-dried small milk tablet is incomplete.
Disclosure of Invention
In order to solve the technical problems, the first aspect of the application provides a whitening and repairing anti-aging freeze-dried small milk tablet, which is prepared from, by weight, 6-10 parts of an excipient, 0.1-2 parts of a stabilizer, 0.06-0.2 parts of a buffering agent, 0.1-2 parts of a humectant, 1-5 parts of maltose, 0.1-2 parts of nano-microemulsion and 0.1-2 parts of a mitochondrial activator.
As a preferred embodiment of the present application, the excipient is at least one selected from mannitol, glycine, glucose, and sucrose.
As a preferable technical scheme of the application, the stabilizer is at least one selected from glycine, guar gum, sucrose, lactose and dextran.
As a preferable technical scheme of the application, the weight ratio of the stabilizer to the excipient is (0.5-8): 40.
as a preferable technical scheme of the application, the buffering agent is at least one selected from acetic acid, succinic acid, glutamic acid, glutaric acid, disodium hydrogen phosphate and citric acid.
In a preferred embodiment of the present application, the humectant is at least one selected from 1, 3-butanediol, 1, 2-hexanediol, octanediol, glycerol, polyglutamic acid, sodium hyaluronate, and collagen.
The second aspect of the application provides a preparation process of a whitening, repairing and anti-aging freeze-dried small milk tablet, which comprises the following preparation steps:
(1) Preparation of raw materials: accurately weighing the raw materials of the freeze-dried small milk slices according to parts by weight for later use;
(2) Preparing a mould: performing die arrangement, pure water die washing, sterilization and drying on the die to obtain a precise die;
(3) Proportioning and filtering: the freeze-dried small milk slices are subjected to burdening and filtering by pure water to obtain a mixed material A;
(4) Precise sterile filtration: performing precise sterile filtration on the mixture A to obtain a mixture B;
(5) And (3) filling: filling the mixed material B by using a precision die to obtain a filling material A;
(6) Frozen organisms sleep: freezing and biological dormancy treatment is carried out on the filling material A;
(7) And (3) drying at low temperature: drying the filling material A subjected to dormancy of the frozen organisms at a low temperature;
(8) Demolding: and demolding the filling material A after low-temperature drying to obtain the freeze-dried small milk tablets.
As a preferable technical scheme of the application, the batching and filtering are divided into two steps, namely coarse batching and filtering in the first step and fine batching and filtering in the second step.
As a preferable technical scheme of the application, a precise flat filter is adopted to carry out precise sterile filtration on the mixed materials.
As a preferred embodiment of the present application, the freezing mode for freezing the dormancy of the living beings is a very rapid freezing mode.
The beneficial effects are that:
1. the transdermal permeability of the specific nano-microemulsion is utilized in the system, so that the mitochondrial activating factor can well permeate the skin, the whitening effect is good in a short time after the freeze-dried small milk tablet is used, and the deep cells of the skin can be activated, repaired and updated, so that the long-term anti-aging and whitening effect can be achieved;
2. the milk slices which cannot be made into the shape of the milk slices by freeze-drying technology in the prior art are easy to break, the shape of the complete milk slices can be made by the application, and the milk slices made by the technology are very easy to dissolve in the solvent;
3. under the action of the specific excipient, stabilizer, buffer and other components, the application has good activation effect on the skin by mitochondrial exciting factors and nano-micro emulsion;
4. the effective components of the mitochondrial activator and the humectant can be well frozen for fresh-keeping after a specific freezing biological dormancy step in the system, so that the survival of the effective components is ensured.
Detailed Description
The disclosure of the present application will be further understood in conjunction with the following detailed description of the preferred embodiments of the application, including examples. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. If the definition of a particular term disclosed in the prior art is inconsistent with any definition provided in the present application, the definition of the term provided in the present application controls.
As used herein, unless the context clearly indicates otherwise, the absence of a limitation to a plurality of features is also intended to include the plurality of features. It will be further understood that the terms "made of …" and "comprising," "including," "having," "including," and/or "containing," as used herein, are synonymous with "including," "having," "containing," and/or "containing," and when used in this specification, mean the stated composition, step, method, article, or apparatus, but do not preclude the presence or addition of one or more other compositions, steps, methods, articles, or apparatus. Furthermore, when describing embodiments of the present application, the use of "preferred," "more preferred," etc. refers to embodiments of the present application that may provide certain benefits in some instances. However, other embodiments may be preferred under the same or other circumstances. In addition, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the application.
In order to solve the technical problems, the first aspect of the application provides a whitening and repairing anti-aging freeze-dried small milk tablet, which is prepared from, by weight, 6-10 parts of an excipient, 0.1-2 parts of a stabilizer, 0.06-0.2 parts of a buffering agent, 0.1-2 parts of a humectant, 1-5 parts of maltose, 0.1-2 parts of nano-microemulsion and 0.1-2 parts of a mitochondrial activator.
In one embodiment, the freeze-dried small milk tablet is prepared from 7-9 parts of excipient, 0.8-1.6 parts of stabilizer, 0.01-0.15 parts of buffer, 1-1.8 parts of humectant, 2-4 parts of maltose, 1-1.5 parts of nano-microemulsion and 0.5-1 part of mitochondrial activating factor by weight.
In one embodiment, the preparation raw materials of the freeze-dried small milk tablet comprise, by weight, 8 parts of an excipient, 1.2 parts of a stabilizer, 0.12 part of a buffer, 1.5 parts of a humectant, 3 parts of maltose, 1.3 parts of a nano-microemulsion and 0.8 part of a mitochondrial activator.
Excipient
To enable the active ingredient to be present in the system, an amount of excipient is selected, which in one embodiment is selected from at least one of mannitol, glycine, glucose, sucrose.
In order to obtain a better shaping effect of the lyophilized pellet, in a preferred embodiment, the excipient is mannitol with a CAS number of 1707-77-3.
Stabilizing agent
In order to enable a good synergy of the excipient and the stabilizer in the system, in one embodiment, the weight ratio of stabilizer to excipient is (1-9): 40, preferably (2-8): 40, a step of performing a; further preferably 6:40.
in order to increase the stability of the system, in one embodiment, the stabilizer is selected from at least one of glycine, guar gum, sucrose, lactose, dextran.
In order to ensure the integrity and smoothness of the lyophilized pellet, in a preferred embodiment, the stabilizer is guar gum having a CAS number of 9000-30-0.
At present, the shape of milk tablets made by freeze-drying technology is not nearly available on the market, and milk tablets made by some experiments are extremely easy to break, mainly because the raw materials and process conditions are not well controlled. In the application, the applicant finds that the freeze-dried small milk tablet prepared by selecting guar gum as a stabilizer can be well molded and is not easy to break through a large amount of researches. The application is likely to be because the guar gum is a specific stabilizer, the guar gum mainly comprises polysaccharide, the guar gum can well interact with mannitol and maltose to increase the stability of a system, and the application also researches and discovers that the ratio of the guar gum to mannitol needs to be controlled to ensure that the integrity of the freeze-dried small milk slices is better, and the application is likely to be because the stabilizing effect cannot be well exerted when the amount of the guar gum is too small, but the viscosity of the system is increased when the amount of the guar gum is too large, and the shearing force in the processing process is easier to act on an excipient to ensure that the freeze-dried small milk slices are easier to break.
Buffering agents
In order to make the nanoemulsion, the mitochondrial activator exist more stably in the system, in one embodiment, the buffer is selected from at least one of acetic acid, succinic acid, glutamic acid, glutaric acid, disodium hydrogen phosphate, citric acid.
In a preferred embodiment, the buffer is disodium hydrogen phosphate with CAS number 7558-80-7.
Maltose
In one embodiment, the maltose is purchased from a color field hive product factory in the south sea area of the bergamot city.
The unit structure of the maltose is glucose, which can well interact with other components in the system, has good stability, ensures that the nano-microemulsion and the mitochondrial activator can stably exist in the system, and the addition of the maltose ensures that the forming effect of the lyophilized milk tablet is better, probably because the maltose contains a large amount of dextrin, the system is not easy to crystallize in the lyophilization process.
Humectant type
In order to provide a good moisturizing effect to the lyophilized minimilk tablets, in one embodiment, the humectant is selected from at least one of 1,3 butylene glycol, 1, 2-hexanediol, octylglycol, glycerin, polyglutamic acid, sodium hyaluronate, collagen.
In a preferred embodiment, the humectant is sodium hyaluronate.
In one embodiment, the sodium hyaluronate is purchased from Shandong An Hua Biometrics Inc.
Nanometer microemulsion
In order to enable better skin action of the active ingredient in the lyophilized minitablets, in one embodiment, the nanoemulsion is purchased from nexname H, inc.
The nano-microemulsion has large surface area, low surface tension and a 'patch effect' on skin, so that the permeation effect of active ingredients is better, the absorption is faster, and the system is more stable by the synergistic effect of the active ingredients and other ingredients in the system.
Mitochondrial activator
In one embodiment, the mitochondrial activator is purchased from university of nude.
The main component Forskolin composite essence of the mitochondrial activator can activate the increase of the level of cyclic adenosine monophosphate (cAMP) in cells, thereby inhibiting the biological activity of Stress Activated Protein (SAPK) in cells, further activating the biosynthesis of mitochondria in cells, supplying nutrients such as intracellular energy ATP and the like, promoting the endogenous growth of skin and the repair and renewal of deep layers, and finally playing an anti-aging role.
The second aspect of the application provides a preparation process of a whitening, repairing and anti-aging freeze-dried small milk tablet, which comprises the following preparation steps:
(1) Preparation of raw materials: accurately weighing the raw materials of the freeze-dried small milk slices according to parts by weight for later use;
(2) Preparing a mould: performing die arrangement, pure water die washing, sterilization and drying on the die to obtain a precise die;
(3) Proportioning and filtering: the freeze-dried small milk slices are subjected to burdening and filtering by pure water to obtain a mixed material A;
(4) Precise sterile filtration: performing precise sterile filtration on the mixture A to obtain a mixture B;
(5) And (3) filling: filling the mixed material B by using a precision die to obtain a filling material A;
(6) Frozen organisms sleep: freezing and biological dormancy treatment is carried out on the filling material A;
(7) And (3) drying at low temperature: drying the filling material A subjected to dormancy of the frozen organisms at a low temperature;
(8) Demolding: and demolding the filling material A after low-temperature drying to obtain the freeze-dried small milk tablets.
And (5) sealing and packaging the demolded freeze-dried small milk slices by using the sterilized aluminum film, labeling, boxing and warehousing.
Specifically, the batching and filtering are divided into two steps, namely coarse batching and filtering in the first step and fine batching and filtering in the second step; more specifically, the process of coarse batching and filtering is as follows: mixing and filtering the raw materials of the freeze-dried small milk slices by using pure water, wherein the weight ratio of the pure water to the raw materials of the freeze-dried small milk slices is 100 (15-30); the fine batching and filtering processes are as follows: filtering the filter cake obtained by coarse ingredients and filtering by using pure water, wherein the weight ratio of the pure water to the raw materials of the freeze-dried small milk slices is 80 (15-30).
Specifically, the precise flat plate filter is adopted to carry out precise sterile filtration on the mixed materials, and more specifically, the filtration precision of the precise flat plate filter is 2 microns.
Specifically, the frozen biological dormancy treatment is carried out by adopting a rapid frozen square hair; more specifically, the filling A is put into a refrigerating device for refrigeration; more specifically, the cooling procedure of the refrigerating device is as follows: cooling to-50deg.C at 2.5deg.C/min-5deg.C/min, and maintaining at-50deg.C for 80-120min.
At present, people pursue portable cosmetics, which are prepared into freeze-dried powder, but the use effect of the freeze-dried powder is relatively poor, some effective components are lost in the preparation process and cannot survive well, and the prepared effective components of the freeze-dried powder have relatively poor efficacy.
Through a great deal of researches, the applicant finds that the effective components of the mitochondrial activator and the humectant can be frozen well for preservation after a specific freezing biological dormancy step in the system of the application, and the survival of the effective components is ensured.
Specifically, the low-temperature drying is performed in a freeze-drying box capable of automatically controlling the temperature; more specifically, an automatic temperature control curve of a freeze-drying box is set, so that the temperature of the freeze-drying box is increased to 0 ℃ and then to 35 ℃; specifically, the time for low-temperature drying is 16h, and the pressure is 30pa; more specifically, the heating rate of the mixture after heating to 35 ℃ is 0.1-0.6 ℃/min;
more specifically, the low-temperature drying step is to put the filling material A after the frozen organism dormancy into a freeze-drying box capable of automatically controlling the temperature, set an automatic temperature control curve of the dry box to heat the filling material A to 0 ℃, and then heat the filling material A to 35 ℃ at a heating rate of 0.4 ℃/min, wherein the time for low-temperature drying is 16h and the pressure is 30pa.
Researches show that the freeze-drying process has a certain influence on the integrity of the freeze-dried milk let, the time and the speed of low-temperature drying are required to be strictly controlled, the integrity of the freeze-dried milk let is influenced when the time and the speed of drying are too high or too high, and the problem that the moisture in the freeze-dried milk let cannot be completely dried when the speed of low-temperature drying is too high and the time is too short, the moisture cannot be volatilized due to the fact that the moisture is blocked by the overdry part, so that the freeze-dried milk let cannot be molded and shrink, and the smoothness of the surface is reduced when the freeze-dried milk let is completely dried when the freeze-drying speed is too slow and the time is too long.
Specific examples of the present application are given below, but the present application is not limited by the examples.
In addition, the raw materials in the present application are commercially available unless otherwise specified.
Examples
Example 1
The embodiment 1 of the application provides a whitening and repairing anti-aging freeze-dried small milk tablet, which is prepared from the following raw materials in parts by weight;
the weight ratio of guar gum to mannitol is 6:40, a step of performing a;
the nano-microemulsion is purchased from Nexsome H of the Chemie Limited company in Guangzhou City; the mitochondrial activator was purchased from university of nula.
The preparation process of the whitening, repairing and anti-aging freeze-dried small milk tablet comprises the following preparation steps of:
(1) Preparation of raw materials: accurately weighing the raw materials of the freeze-dried small milk slices according to parts by weight for later use; (2) preparation of a mold: performing die arrangement, pure water die washing, sterilization and drying on the die to obtain a precise die; (3) batching and filtering: the freeze-dried small milk slices are subjected to burdening and filtering by pure water to obtain a mixed material A; (4) precise sterile filtration: performing precise sterile filtration on the mixture A to obtain a mixture B; and (5) filling: filling the mixed material B by using a precision die to obtain a filling material A; (6) frozen biological dormancy: freezing and biological dormancy treatment is carried out on the filling material A; (7) drying at low temperature: drying the filling material A subjected to dormancy of the frozen organisms at a low temperature; (8) demolding: and demolding the filling material A after low-temperature drying to obtain the freeze-dried small milk tablets.
The material mixing and filtering are divided into two steps, namely coarse material mixing and filtering in the first step and fine material mixing and filtering in the second step; the coarse batching and filtering processes are as follows: mixing and filtering the raw materials of the freeze-dried small milk slices by using pure water, wherein the weight ratio of the pure water to the raw materials of the freeze-dried small milk slices is 100:22; the fine batching and filtering processes are as follows: filtering a filter cake obtained by coarse batching and filtering by using pure water, wherein the weight ratio of the pure water to the raw materials of the freeze-dried small milk slices is 80:25;
the method comprises the steps of freezing biological dormancy treatment by adopting a rapid freezing method, and putting the filling A into a freezing device for freezing, wherein the cooling program of the freezing device is as follows: 3.5 ℃/min to be cooled to-50 ℃ and kept at-50 ℃ for 100min;
the low-temperature drying is carried out in a freeze-drying box capable of automatically controlling the temperature, and the specific steps are as follows: setting an automatic temperature control curve of a freeze-drying box, heating the freeze-drying box to 0 ℃, and then heating the freeze-drying box to 35 ℃; the time for low-temperature drying is 16h, and the pressure is 30pa; the heating rate of the mixture to 35 ℃ is 0.35 ℃/min;
the method comprises the specific steps of low-temperature drying, namely placing the filling material A subjected to dormancy of frozen organisms into a freeze-drying box capable of automatically controlling temperature, setting an automatic temperature control curve of the freeze-drying box, heating to 0 ℃, and then heating to 35 ℃ at a heating rate of 0.4 ℃/min, wherein the time for low-temperature drying is 16h, and the pressure is 30pa.
Mannitol has a CAS number of 1707-77-3; the CAS number of the guar gum is 9000-30-0; the buffering agent is disodium hydrogen phosphate with CAS number of 7558-80-7; maltose is purchased from Beehive product factories in the color field in the south sea area of the Buddha city; sodium hyaluronate was purchased from Shandong An Hua Biometrics Inc.
Example 2
The embodiment 2 of the application provides a whitening, repairing and anti-aging freeze-dried small milk tablet, which is different from the embodiment 1 in that chitosan is used for replacing mannitol.
Example 3
The embodiment 3 of the application provides a whitening, repairing and anti-aging freeze-dried small milk tablet, which is different from the embodiment 1 in that the specific steps of low-temperature drying are that a filling material A after freezing biological dormancy is placed into a freeze-drying box capable of automatically controlling temperature, an automatic temperature control curve of the dry box is set, the temperature of the dry box is increased to 0 ℃, then the temperature is increased to 35 ℃ at a heating rate of 0.4 ℃/min, and the time for low-temperature drying is 10h and the pressure is 30pa.
Example 4
The embodiment 4 of the application provides a whitening, repairing and anti-aging freeze-dried small milk tablet, which is different from the embodiment 1 in that the specific steps of low-temperature drying are that a filling material A after freezing biological dormancy is placed into a freeze-drying box capable of automatically controlling temperature, an automatic temperature control curve of the dry box is set, the temperature of the dry box is increased to 0 ℃, then the temperature is increased to 35 ℃ at a heating rate of 0.4 ℃/min, and the time for low-temperature drying is 5h and the pressure is 30pa.
Example 5
The embodiment 5 of the application provides a whitening, repairing and anti-aging freeze-dried small milk tablet, which is different from the embodiment 1 in that the guar gum is 0.6 part, and the weight ratio of the guar gum to mannitol is 3:40.
example 6
The embodiment 6 of the application provides a whitening repair anti-aging freeze-dried small milk tablet, which is different from the embodiment 1 in that guar gum is 2 parts, and the weight ratio of guar gum to mannitol is 10:40.
performance testing
1. Skin firmness R0, skin gloss, skin brightness ITA and wrinkle area ratio test
The testing method comprises the following steps:
selecting uneven, dull and shiny face skin; facial skin meets the eye corner wrinkle level 2-5; the facial skin is loose and 33 Chinese healthy female subjects lack of elasticity, and the age range is 25-55 years. Skin firmness R0, skin gloss, skin brightness ITA, and wrinkle area ratio were tested before use of the test product, immediately after use, 7 days after continuous use of the product, 14 days, respectively. The evaluation results before and after the product is used are compared by a statistical test method so as to judge whether the statistical difference exists. Wherein: the measuring instrument of the skin tightness R0 is a skin elasticity tester Cutometer dual MPA580, and the test area is a cheek; the skin gloss measuring instrument is a skin gloss test probe Gloymeter GL200, and the test area is cheek; the measuring instrument of the skin brightness ITA is a skin color test probe Colorimeter CL400, and the test area is a cheek; the measuring instrument of the wrinkle area ratio is a facial image analyzer VISLA-CR, and the test area is a full face.
Test conditions:
the environmental temperature of the test is 20.1-21.2 ℃, and the relative humidity is 42.1-51.0%.
Test sample product:
the lyophilized pellet prepared in example 1 was used in combination with a type of essence.
The using method comprises the following steps:
2 times daily, 1 time each in the morning and evening.
The statistical method comprises the following steps:
the statistical analysis software is SPSS. If the numerical value is normally distributed, adopting a t-test method to carry out statistical analysis; if the numerical value is in non-normal distribution, adopting a rank sum test method to carry out statistical analysis;
the statistical methods all used a two-tailed test, level=0.05.
The security evaluation adopts a statistical description method, and the adverse event degree and the duration of the adverse event are analyzed example by example.
The change rate is the change rate before use, and the calculation formula is as follows:
use product immediate delta (difference) =t15 min-D0;
delta (difference) =d7-D0 on day 7 of the use of the product;
delta (difference) =d14-D0 on day 14 of the use of the product;
in the formula, D0 is the basic value of the skin parameter before the product is used in the tested area.
T15 min-the skin parameter values are measured immediately upon application of the product to the test area.
D7—product used in test area day 7, skin parameter values.
D14—product used in test area day 14, skin parameter values.
N—number of subjects.
Test results:
TABLE 1 skin firmness R0 test results
TABLE 2 skin firmness R0 test results
The statistical method comprises the following steps: analysis was performed using the t-test method, with a test level α=0.05.
The significance labeling method comprises the following steps: (n.s. "means no statistical difference, p.gtoreq.0.05; p <0.05 means significant difference (". Times. "means 0.01.ltoreq.p < 0.05;". Times. "means 0.001.ltoreq.p < 0.01;". Times. "means p < 0.001).
Number of product used = 33.
From the test results of tables 1 and 2, it can be seen that: subject's skin firmness R0 was significantly reduced compared to basal value (p < 0.001), with a reduction rate of 14.69%; 7 days in the continuous product samples, the skin firmness R0 of the subjects was significantly reduced (p < 0.001) compared to the basal value, at a reduction rate of 6.53%; the skin firmness R0 of the subjects was significantly reduced (p < 0.001) from the basal value by 13.82% for 14 days with continuous use of the test product.
Measurement value: the lower the skin firmness R0 value, the tighter the skin.
TABLE 3 skin gloss test results
TABLE 4 skin gloss test results
The statistical method comprises the following steps: analysis was performed using the t-test method, with a test level α=0.05.
The significance labeling method comprises the following steps: (n.s. "means no statistical difference, p.gtoreq.0.05; p <0.05 means significant difference (". Times. "means 0.01.ltoreq.p < 0.05;". Times. "means 0.001.ltoreq.p < 0.01;". Times. "means p < 0.001).
Number of product used = 33.
From the test results of tables 3 and 4, it can be seen that: the single use of the test product sample immediately showed a significant increase in skin gloss of the subject as compared to the base value ((p < 0.001), the rate of increase was 10.97%, the continuous use of the test product sample for 7 days showed a significant increase in skin gloss of the subject as compared to the base value (p < 0.001), the rate of increase was 15.03%, the continuous use of the test product for 14 days showed a significant increase in skin gloss of the subject as compared to the base value (p < 0.001), the rate of increase was 22.44%.
Measurement value: the greater the skin gloss value, the more shiny the skin.
TABLE 5 Visia-CR skin Brightness ITA degree value detection results
TABLE 6 Visia-CR skin Brightness ITA degree value detection results
The statistical method comprises the following steps: analysis was performed using the t-test method, with a test level α=0.05.
The significance labeling method comprises the following steps: (n.s. "means no statistical difference, p.gtoreq.0.05; p <0.05 means significant difference (". Times. "means 0.01.ltoreq.p < 0.05;". Times. "means 0.001.ltoreq.p < 0.01;". Times. "means p < 0.001).
Number of product used = 33.
From the test results of tables 5 and 6, it can be seen that: the visual-CR skin brightness ITA degree value of the test product sample is obviously increased (p is more than or equal to 0.001 and less than or equal to 0.01) compared with that of the test product sample for single use, and the rising rate is 2.50%; the test product samples were used continuously for 7 days, and the visual-CR skin brightness ITA degree value of the subject was significantly increased (p < 0.001) compared with the basal value, with an increase rate of 2.35%; the test product was used continuously for 14 days, and the visual-CR skin brightness ITA DEG value of the subject was significantly increased (p < 0.001) from the basal value, with an increase rate of 3.02%.
Measurement value: the higher the skin brightness ITA DEG value, the brighter the skin.
TABLE 7 Visia-CR wrinkle area ratio detection results
TABLE 8 Visia-CR wrinkle area ratio detection results
The statistical method comprises the following steps: analysis was performed using the t-test method, with a test level α=0.05.
The significance labeling method comprises the following steps: (n.s. "means no statistical difference, p.gtoreq.0.05; p <0.05 means significant difference (". Times. "means 0.01.ltoreq.p < 0.05;". Times. "means 0.001.ltoreq.p < 0.01;". Times. "means p < 0.001).
Number of product used = 33.
From the test results of tables 5 and 6, it can be seen that: the single use test product sample HY21L988 shows that the ratio of the area of the Visia-CR wrinkles of the subject is obviously reduced (p is more than or equal to 0.001 and less than or equal to 0.01) compared with the basic value, and the reduction rate is 8.21%; the test product sample is continuously used for 7 days, the Visia-CR wrinkle area of the subject is obviously reduced (p is more than or equal to 0.001 and less than or equal to 0.01) compared with a basic value, and the reduction rate is 11.03%; the test product was used continuously for 14 days, and the ratio of the area of the Visia-CR wrinkles of the subject was significantly reduced (p < 0.001) compared with the basal value, and the reduction rate was 13.74%.
Measurement value: the lower the skin wrinkle area ratio, the fewer skin wrinkles.
2. Integrity test of lyophilized pellet:
the prepared lyophilized milk flakes of examples 1 to 6 were visually inspected for integrity and smoothness, and the test results are shown in Table 9:
TABLE 9
Integrity of
Example 1 The block shape is complete and smooth
Example 2 Incomplete and unsmooth block shape
Example 3 Incomplete and unsmooth block shape
Example 4 Cannot be formed
Example 5 Incomplete and unsmooth block shape
Example 6 Complete and unsmooth block shape
The foregoing examples are illustrative only and serve to explain some features of the method of the application. The appended claims are intended to claim the broadest possible scope and the embodiments presented herein are merely illustrative of selected implementations based on combinations of all possible embodiments. It is, therefore, not the intention of the applicant that the appended claims be limited by the choice of examples illustrating the features of the application. Some numerical ranges used in the claims also include sub-ranges within which variations in these ranges should also be construed as being covered by the appended claims where possible.

Claims (1)

1. The preparation raw materials of the freeze-dried small milk tablet comprise, by weight, 8 parts of mannitol, 1.2 parts of guar gum, 0.12 part of disodium hydrogen phosphate, 1.5 parts of sodium hyaluronate, 3 parts of maltose, 1.3 parts of nano-microemulsion and 0.8 part of mitochondrial activating factor;
the weight ratio of guar gum to mannitol is 6:40, a step of performing a;
the preparation process of the whitening, repairing and anti-aging freeze-dried small milk tablet comprises the following preparation steps of:
(1) Preparation of raw materials: accurately weighing the raw materials of the freeze-dried small milk slices according to parts by weight for later use;
(2) Preparing a mould: performing die arrangement, pure water die washing, sterilization and drying on the die to obtain a precise die;
(3) Proportioning and filtering: the freeze-dried small milk slices are subjected to burdening and filtering by pure water to obtain a mixed material A;
(4) Precise sterile filtration: performing precise sterile filtration on the mixture A to obtain a mixture B;
(5) And (3) filling: filling the mixed material B by using a precision die to obtain a filling material A;
(6) Frozen organisms sleep: freezing and biological dormancy treatment is carried out on the filling material A;
(7) And (3) drying at low temperature: drying the filling material A subjected to dormancy of the frozen organisms at a low temperature;
(8) Demolding: demolding the filling material A after low-temperature drying to obtain a freeze-dried small milk tablet;
the material mixing and filtering are divided into two steps, namely coarse material mixing and filtering in the first step and fine material mixing and filtering in the second step; the coarse batching and filtering processes are as follows: mixing and filtering the raw materials of the freeze-dried small milk slices by using pure water, wherein the weight ratio of the pure water to the raw materials of the freeze-dried small milk slices is 100:22; the fine batching and filtering processes are as follows: filtering a filter cake obtained by coarse batching and filtering by using pure water, wherein the weight ratio of the pure water to the raw materials of the freeze-dried small milk slices is 80:25;
the method comprises the steps of freezing biological dormancy treatment by adopting a rapid freezing method, and putting the filling A into a freezing device for freezing, wherein the cooling program of the freezing device is as follows: 3.5 ℃/min to be cooled to-50 ℃ and kept at-50 ℃ for 100min;
the low-temperature drying is carried out in a freeze-drying box capable of automatically controlling the temperature, and the specific steps are as follows: setting an automatic temperature control curve of a freeze-drying box, heating the freeze-drying box to 0 ℃, and then heating the freeze-drying box to 35 ℃; the time for low-temperature drying is 16h, and the pressure is 30pa; the heating rate of the mixture to 35 ℃ is 0.35 ℃/min;
the method comprises the specific steps of low-temperature drying, namely placing the filling material A subjected to dormancy of frozen organisms into a freeze-drying box capable of automatically controlling temperature, setting an automatic temperature control curve of the freeze-drying box, heating to 0 ℃, and then heating to 35 ℃ at a heating rate of 0.4 ℃/min, wherein the time for low-temperature drying is 16h, and the pressure is 30pa.
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