CN115770197A - Preparation method of freeze-dried tablet and freeze-dried tablet - Google Patents

Preparation method of freeze-dried tablet and freeze-dried tablet Download PDF

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Publication number
CN115770197A
CN115770197A CN202211737731.5A CN202211737731A CN115770197A CN 115770197 A CN115770197 A CN 115770197A CN 202211737731 A CN202211737731 A CN 202211737731A CN 115770197 A CN115770197 A CN 115770197A
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freeze
drying
vacuum
raw materials
tablet
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钱永常
秦倩茹
李立山
李彤彤
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Hangzhou Neuropeptide Biological Science And Technology Inc Ltd
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Hangzhou Neuropeptide Biological Science And Technology Inc Ltd
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Abstract

The invention provides a preparation method of a freeze-dried tablet and the freeze-dried tablet, and belongs to the technical field of cosmetics. The invention comprises the steps of raw material preparation, pre-freezing process, vacuum drying and analysis drying. According to the invention, most of moisture in the product is removed through the freeze-drying process, so that atrophy in the storage process is prevented, the damage of oxygen and hydrolysis is isolated, functional components which cannot bear high temperature in the freeze-dried sheet do not pass through a high-temperature process in the whole process, the components can be well stored, the atrophy is prevented, and the functional components in the product can be well stored, so that the functional components can be better exerted, and can be dissolved in water to activate the moisture and nutrients in the freeze-dried sheet, thereby achieving the effects of repairing skin, resisting wrinkle and tightening and enabling the skin to be fresh.

Description

Preparation method of freeze-dried tablet and freeze-dried tablet
Technical Field
The invention relates to the technical field of cosmetics, in particular to a preparation method of a freeze-dried tablet and the freeze-dried tablet prepared by the preparation method.
Background
The cosmetic industry focuses on the efficacy, and along with the modernization process, the demand of people on skin care products tends to be more and more effective, and the most important of the skin care products with the efficacy is the efficacy of the skin care products.
The conventional skin care products mostly adopt essence cream as a main component, so the efficacy active substances in the skin care products cannot fully play a role, and in order to achieve the efficacy of the skin care products and improve the skin condition, the preparation process of the skin care products needs to be changed.
Most of the existing functional skin care products are active substances stored in a liquid state for a long time, the preparation method of the skin care products can cause that some active ingredients which are easy to degrade and oxidize are difficult to store, the long-term activity of the active substances can not be guaranteed, the active substances are difficult to store and have low absorption rate, the storage process is easy to shrink, the using effect is influenced, and the aim of improving the skin can not be finally achieved.
Disclosure of Invention
In view of this, in order to solve the technical problems that in the prior art, skin care products mostly adopt essence cream as a main component, and active substances are stored in a liquid state for a long time, so that some active ingredients which are easy to degrade and oxidize are difficult to store, the long-term activity of the active substances cannot be guaranteed, the active substances are difficult to store, the absorption rate is low, and the storage process is easy to shrink, the invention provides a preparation method of a freeze-dried tablet.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a freeze-dried tablet comprises the following steps:
1) Preparing raw materials: adding mannitol, pullulanase polysaccharide, sodium alginate, sodium hyaluronate, superoxide dismutase and type III collagen into water, putting into a stirrer, fully mixing and stirring, and filtering to obtain a mixed raw material;
2) The filling process comprises the following steps: filling the mixed raw materials in the step 1) into a mould;
3) Pre-freezing process: putting the mixed raw materials in the step 2) into a vacuum freeze dryer, wherein the pre-freezing temperature is-45-40 ℃, and the maintaining time is 90-180 min;
4) And (3) vacuum drying: controlling the vacuum degree in the vacuum freeze dryer to be 10-30Pa, the drying temperature to be-10-0 ℃, and controlling the drying time to be 10-20h to dry the mixed raw materials;
5) And (3) resolving and drying: adjusting the vacuum degree in the vacuum freeze dryer to 0-30Pa, gradually increasing the drying temperature to 25-35 deg.C, and drying for 120-240min to obtain block lyophilized tablet;
6) Packaging: and (4) packaging the blocky freeze-dried tablets obtained in the step 5) in a vacuum sealing manner.
Preferably, in step 1), mannitol, pullulanase, sodium alginate and sodium hyaluronate are added into water and heated to 65-85 ℃ for stirring for 40-60min, and superoxide dismutase and type III collagen are added when the temperature is reduced to below 40 ℃ for stirring for 3-5min.
Preferably, in step 2), the mold is a silicone mold or a PET plastic mold.
Preferably, in step 6), the packaging is vacuum sealed by using a PET/PE film bag or an aluminum foil film bag.
Preferably, in the step 1), the mannitol is 0.8-1.5%, the pullulanase polysaccharide is 0.2-2.2%, the sodium alginate is 0-0.4%, the sodium hyaluronate is 0-0.5%, the superoxide dismutase is 0.001-0.02%, and the type III collagen is 0.05-0.2% by mass percentage.
The invention provides a freeze-dried tablet which is prepared by adopting the preparation method of the freeze-dried tablet.
Preferably, small peptides are also included.
Preferably, the small peptide is acetyl hexapeptide-8 and/or tripeptide-1.
Compared with the prior art, the invention has the following beneficial effects:
1) Most of moisture in the product is removed through a freeze-drying process, the storage process is not easy to shrink, the damage of oxygen and hydrolysis is isolated through a cosmetic solid dosage form which is freeze-dried and packaged and stored in a vacuum sealing mode, functional components which cannot bear high temperature in the freeze-dried sheet do not pass through a high-temperature process in the whole process, the components can be well stored, the shrinkage is prevented, meanwhile, the functional components can be dissolved in water, the moisture and the nutrients in the freeze-dried sheet are activated, and therefore the effects of repairing skin, resisting wrinkles and tightening and enabling the skin to be fresh are achieved.
2) The freeze-dried tablet obtained by the invention is not easy to shrink in the storage process, has obvious advantages compared with the same type of products, well keeps the activity of active substances, and enables the skin to absorb more effective active ingredients. The formed product is widely used in the cosmetic industry, and provides safe and effective products for consumers.
3) The invention can resist skin oxidation, brighten skin color, effectively prevent skin aging, resist wrinkle and tighten skin by adding superoxide dismutase, and can lock water, repair skin and make skin smooth and tender by adding collagen component.
Detailed Description
The invention provides a preparation method of a freeze-dried tablet, which comprises the following steps:
1) Preparing raw materials: adding mannitol, pullulanase polysaccharide, sodium alginate, sodium hyaluronate, superoxide dismutase and type III collagen into water, putting the mixture into a stirrer to be fully mixed and stirred, and filtering to obtain a mixed raw material, wherein the addition of the superoxide dismutase can resist skin oxidation, brighten skin color, effectively prevent skin aging, resist wrinkle and tighten skin, and can lock water and repair skin by adding collagen components so as to ensure that the skin achieves the effect of smoothing and tendering the skin;
2) The filling process comprises the following steps: filling the mixed raw materials in the step 1) into a mould;
3) Pre-freezing process: putting the mixed raw materials in the step 2) into a vacuum freeze dryer, wherein the pre-freezing temperature is-45-40 ℃, and the maintaining time is 90-180 min, wherein the pre-freezing time (set time) can be adjusted according to the thickness of a freeze-dried piece, preferably 2min in the invention, and can be selected by a person skilled in the art according to actual needs, such as 5min, 8min and the like;
4) And (3) vacuum drying: controlling the vacuum degree in a vacuum freeze dryer to be 10-30Pa, the drying temperature to be-10-0 ℃, and controlling the drying time to be 10-20h to dry the mixed raw material, wherein the drying time refers to the sum of the set time and the holding time, the preset drying degree is reached in the set time, and then the drying time is kept for a certain time to complete the whole vacuum drying process, and the specific time of the set time and the holding time has no special requirements, and can be selected by a person skilled in the art according to actual needs;
5) And (3) resolving and drying: adjusting the vacuum degree in a vacuum freeze dryer to 0-30Pa, gradually raising the drying temperature to 25-35 ℃, and then drying for 120-240min to obtain a blocky freeze-dried tablet, wherein the drying time refers to the setting time and the holding time, the preset drying degree is reached within the setting time, and then the drying time is kept for a certain time to complete the whole analysis and drying process, and the specific time of the setting time and the holding time has no special requirements, and the technicians in the field can select the drying time according to actual needs;
6) Packaging: and (5) packaging the blocky freeze-dried tablets obtained in the step 5) in a vacuum sealing manner.
In the invention, in the step 1), mannitol, pullulanase, sodium alginate and sodium hyaluronate are added into water and heated to 65-85 ℃ and stirred for 40-60min, and superoxide dismutase and type III collagen are added after the temperature is reduced to below 40 ℃ and stirred for 3-5min.
In the invention, in the step 2), the mold is a silica gel mold or a PET plastic mold.
In the invention, in the step 6), a PET/PE film bag or an aluminum foil film bag is adopted for vacuum sealing and packaging.
In the invention, in the step 1), according to the mass percentage, the mannitol is 0.8-1.5%, the pullulanase is 0.2-2.2%, the sodium alginate is 0-0.4%, the sodium hyaluronate is 0-0.5%, the superoxide dismutase is 0.001-0.02%, and the type III collagen is 0.05-0.2%.
The invention provides a freeze-dried tablet which is prepared by adopting the preparation method of the freeze-dried tablet.
In the present invention, small peptides are also included according to efficacy.
In the present invention, the small peptide is acetyl hexapeptide-8 and/or tripeptide-1.
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Example 1
A method for preparing a lyophilized tablet, comprising the steps of:
1) Preparing raw materials: adding mannitol and pullulanase polysaccharide into water, heating to 75 deg.C, stirring for 60min, adding superoxide dismutase (SOD) and type III collagen at a temperature below 40 deg.C, stirring for 3min, and filtering to obtain mixed raw materials, wherein the mixed raw materials comprise, by mass, 1.0% mannitol, 2.0% pullulanase polysaccharide, 0.001% superoxide dismutase (SOD), and 0.05% type III collagen;
2) The filling process comprises the following steps: filling the mixed raw materials in the step 1) into a PET plastic mould.
3) Pre-freezing process: putting the mixed raw materials in the step 2) into a vacuum freeze dryer for pre-freezing;
4) And (3) vacuum drying: controlling the vacuum drying condition in the vacuum freeze dryer to dry the mixed raw materials;
5) And (3) resolving and drying: after vacuum drying is finished, carrying out resolution drying to obtain a massive freeze-dried tablet;
6) Packaging: and (4) packaging the blocky freeze-dried tablets obtained in the step 5) in a vacuum sealing manner by adopting an aluminum foil film bag.
The lyophilization process for the prefreezing process, vacuum drying and desorption drying is as follows:
Figure BDA0004028181770000051
example 2
A method for preparing a lyophilized tablet, comprising the steps of:
1) Preparing raw materials: adding mannitol, pullulanase polysaccharide, sodium alginate and sodium hyaluronate into water, heating to 65 ℃, stirring for 50min, adding superoxide dismutase (SOD) and type III collagen below 40 ℃, stirring for 5min, and filtering to obtain a mixed raw material, wherein the mass percentage of the mannitol is 0.8%, the mass percentage of the pullulanase polysaccharide is 0.25%, the mass percentage of the sodium alginate is 0.25%, the mass percentage of the sodium hyaluronate is 0.2%, the mass percentage of the superoxide dismutase (SOD) is 0.01%, and the mass percentage of the type III collagen is 0.05%.
2) The filling process comprises the following steps: filling the mixed raw materials in the step 1) into a PET plastic mould.
3) Pre-freezing process: putting the mixed raw materials in the step 2) into a vacuum freeze dryer for pre-freezing;
4) And (3) vacuum drying: controlling the vacuum drying condition in the vacuum freeze dryer to dry the mixed raw materials;
5) And (3) resolving and drying: after vacuum drying is finished, carrying out resolution drying to obtain a massive freeze-dried tablet;
6) Packaging: and (3) carrying out vacuum sealing packaging on the blocky freeze-dried tablets obtained in the step 5) by adopting an aluminum foil film bag.
The lyophilization process for the prefreezing process, vacuum drying and desorption drying is as follows:
Figure BDA0004028181770000061
example 3
A method for preparing a lyophilized tablet, comprising the steps of:
1) Preparing raw materials: adding mannitol, pullulanase polysaccharide and sodium hyaluronate into water, heating to 85 ℃, stirring for 40min, adding superoxide dismutase (SOD), type III collagen and acetyl hexapeptide-8 at the temperature below 40 ℃, stirring for 4min, and filtering to obtain a mixed raw material, wherein the mannitol, the pullulanase polysaccharide, the sodium hyaluronate, the superoxide dismutase (SOD) are 0.5%, the sodium hyaluronate, the superoxide dismutase (SOD), the type III collagen and the acetyl hexapeptide-8 are respectively 1.4%, 0.005%, 0.05% and 0.02% in percentage by mass.
2) The filling process comprises the following steps: filling the mixed raw materials in the step 1) into a PET plastic mould.
3) Pre-freezing process: putting the mixed raw materials in the step 2) into a vacuum freeze dryer for pre-freezing;
4) And (3) vacuum drying: controlling the vacuum drying condition in the vacuum freeze dryer to dry the mixed raw materials;
5) And (3) resolving and drying: after vacuum drying is finished, carrying out resolution drying to obtain a massive freeze-dried tablet;
6) Packaging: and (3) carrying out vacuum sealing packaging on the blocky freeze-dried tablets obtained in the step 5) by adopting a PET/PE film bag.
The lyophilization process for the prefreezing process, vacuum drying and desorption drying is as follows:
Figure BDA0004028181770000071
in addition, the above examples 1 to 3 and some of the commercially available lyophilized sheets were subjected to an atrophy test, and the degree of atrophy of the lyophilized sheets was judged by the atrophy rate.
Figure BDA0004028181770000072
A0-0 day the length (cm) of the longest straight line segment of the freeze-dried tablet
An-length of longest straight line segment (cm) of freeze-dried piece on nth day
The freeze-dried tablet has a certain atrophy under the daily standing condition, the atrophy condition is greatly influenced by temperature and humidity, and the atrophy rate is continuously increased along with the increase of the temperature. Thus, the collected lyophilized pieces were left for 1 month at 60 ℃. + -. 2 ℃ and humidity of 47-57%.
Figure BDA0004028181770000073
It can be seen that the examples claimed in this patent have significant advantages in combating atrophy.
The invention is subjected to vacuum freeze-drying and vacuum sealing packaging to isolate moisture and air, and is convenient to carry. The skin care product can efficiently preserve the activity and stability of active ingredients in the skin care product, contains high-concentration active factors, can repair damaged barriers, reduces water loss of the skin, improves the skin, and guarantees the efficacy and safety of efficacy raw materials through a vacuum freeze-drying technology.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (8)

1. The preparation method of the freeze-dried tablet is characterized by comprising the following steps:
1) Preparing raw materials: adding mannitol, pullulanase polysaccharide, sodium alginate, sodium hyaluronate, superoxide dismutase and type III collagen into water, putting into a stirrer, fully mixing and stirring, and filtering to obtain a mixed raw material;
2) The filling process comprises the following steps: filling the mixed raw materials in the step 1) into a mould;
3) Pre-freezing process: putting the mixed raw materials in the step 2) into a vacuum freeze dryer, wherein the pre-freezing temperature is-45-40 ℃, and the maintaining time is 90-180 min;
4) And (3) vacuum drying: controlling the vacuum degree in the vacuum freeze dryer to be 10-30Pa, the drying temperature to be-10-0 ℃, and controlling the drying time to be 10-20h to dry the mixed raw materials;
5) And (3) resolving and drying: adjusting the vacuum degree in the vacuum freeze dryer to 0-30Pa, gradually increasing the drying temperature to 25-35 deg.C, and drying for 120-240min to obtain block lyophilized tablet;
6) Packaging: and (4) packaging the blocky freeze-dried tablets obtained in the step 5) in a vacuum sealing manner.
2. The method for preparing a lyophilized tablet according to claim 1, wherein in step 1), mannitol, pullulanase, sodium alginate and sodium hyaluronate are added to water and heated at 65-85 ℃ with stirring for 40-60min, and superoxide dismutase and type III collagen are added after the temperature is reduced to below 40 ℃ with stirring for 3-5min.
3. The method for preparing a lyophilized tablet as claimed in claim 1, wherein in step 2), the mold is a silicone mold or a PET plastic mold.
4. The method for preparing a lyophilized tablet as claimed in claim 1, wherein in step 6), the tablet is vacuum sealed and packaged by using a PET/PE film bag or an aluminum foil film bag.
5. The process of preparing a lyophilized tablet according to any one of claims 1 to 4, wherein in step 1), mannitol is 0.8 to 1.5%, pullulanase is 0.2 to 2.2%, sodium alginate is 0 to 0.4%, sodium hyaluronate is 0 to 0.5%, superoxide dismutase is 0.001 to 0.02%, and collagen type III is 0.05 to 0.2% by mass.
6. A lyophilized tablet produced by the method for producing a lyophilized tablet according to any one of claims 1 to 5.
7. A lyophilized tablet according to claim 6, further comprising small peptides.
8. A lyophilized tablet according to claim 7, wherein the small peptide is acetyl hexapeptide-8 and/or tripeptide-1.
CN202211737731.5A 2022-12-30 2022-12-30 Preparation method of freeze-dried tablet and freeze-dried tablet Pending CN115770197A (en)

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Publication number Priority date Publication date Assignee Title
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