A stable lyophilized composition having anti-wrinkle repair efficacy and a method of making the same

Abstract

The present application relates to the technical field of vacuum freeze-drying, and discloses a vacuum freeze-drying device, which comprises a freeze vacuum drying cavity, one side of the freeze vacuum drying cavity is provided with a normal-temperature vacuum crushing cavity, a groove is formed in the bottom of the inner cavity of the freeze vacuum drying cavity, the groove extends to the inside of the normal-temperature vacuum crushing cavity, a placing plate is arranged in the freeze vacuum drying cavity, a quick-assembly component for mounting a vial is arranged above the placing plate, and the bottom of the placing plate is in sliding connection with the groove. The present application also discloses a stable freeze-drying composition with anti-wrinkle repair effect and a preparation method thereof. Since the placing plate is in a low-temperature state when the freeze vacuum drying cavity is in a frozen state, the placing plate is not easy to contact, and in the process of pushing the placing plate from the freeze vacuum drying cavity into the normal-temperature vacuum crushing cavity, the placing plate needs to pass over the groove, and the arrangement of the at least two rollers can smoothly pass over the groove, so that the placing plate will not shake when being pushed, and in turn, the vial in a frozen state is prevented from being broken.

Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of cosmetics, and particularly relates to a freeze-dried composition with anti-wrinkle repair effect and stability and a preparation method thereof. BACKGROUND

[0002] In recent years, people have gradually paid attention to cosmetics with lower preservatives, higher activity, convenient storage, and better skin adhesion, which will not cause skin problems. The top three skin allergens are pollen, dust, and cosmetics, especially cosmetics that directly contact the skin. Once the quality changes, the skin will be damaged, and the face will be seriously damaged. Therefore, some natural skin care materials with good biocompatibility, such as truncated collagen, soluble collagen, and whey protein, have become the focus of cosmetic research.

[0003] The vacuum freeze-drying process can be simply divided into pre-freezing, primary drying, and analytical drying. Its advantage lies in that the drying process is carried out under low temperature and high vacuum conditions, and the dehydration is efficient. The thermal denaturation of biological materials is small, which can maximize the biological activity of the materials, and prolong the long-term storage of the freeze-dried powder obtained after vacuum freeze-drying treatment. The vacuum freeze-drying product equipment is complex and has high energy consumption, resulting in high production cost. Further optimization of this technology for use in the field of cosmetic preparation can improve its biological activity and prolong its shelf life.

[0004] The vacuum freeze-drying equipment is suitable for drying of high-grade raw materials, traditional Chinese medicine decoction pieces, biology, wild vegetables, dehydrated vegetables, food, fruits, chemicals, pharmaceutical intermediates, and other materials. The equipment can combine a refrigeration system, a vacuum system, a heat conducting oil heating system, and a dehumidification system into one body, and a new type of box structure is pushed out. The freezing vacuum drying greatly utilizes the material storage space in the box for drying. The vacuum freeze-drying equipment is commonly used in the manufacture of skin care products.

[0005] After the preparation of the freeze-dried powder, it needs to be filled into a Westlin bottle. However, when the blended collagen glue powder is filled, the amount of the blended collagen glue powder in each portion is too small, making it difficult to control the amount of the blended collagen glue powder in the Westlin bottle. Therefore, the blended collagen glue is first filled into the Westlin bottle, and then vacuum freeze-dried, which can avoid the above problems.

[0006] However, it is difficult to crush the blended collagen glue freeze-dried in the Westlin bottle. After the preparation of the blended collagen glue freeze-dried, it needs to be crushed and transported, which can easily contaminate the blended collagen glue powder. When the blended collagen glue freeze-dried is completed, a large amount of fine pores will be generated in the blended collagen glue freeze-dried product, forming a "sponge" material. When the product is transferred to the next step from the freezing vacuum environment, the moisture in the normal temperature air will be absorbed in the "sponge" blended collagen glue freeze-dried product, which will affect the quality of the blended collagen glue freeze-dried powder. SUMMARY

[0007] To solve the above technical problems, the application provides the following technical scheme: a preparation method of a freeze-dried composition with anti-wrinkle repair effect and stability, comprising the following steps:

[0008] Step one, deionized water is added to a stirred tank, and sodium citrate and whey protein are sequentially added, and stirred uniformly at room temperature; end-lacking collagen, soluble collagen and mannitol are added, and stirred uniformly at room temperature, to obtain a blended collagen glue.

[0009] Step two, the blended collagen glue is perfused into a test tube, and freeze-drying is performed in the vacuum freeze-drying equipment, and the product is obtained after the box is taken out.

[0010] Preferably, in the step one, the stirring condition is 40 r / min-50 r / min, and the stirring time is 15-20 min; the stirring condition is 40 r / min-50 r / min again, and the stirring time is 30-50 min.

[0011] Preferably, in the step one, the mass ratio of deionized water, end-lacking collagen, soluble collagen, whey protein, sodium citrate and mannitol is (93.1-98.3):(0.1-0.3):(0.1-0.3):(0.4-1):(0.1-0.3):(1-5).

[0012] Preferably, in the step two, the vacuum freeze-drying specifically comprises the following steps:

[0013] S1, pre-freezing: the test tube containing the blended collagen glue is frozen at 0℃~-10℃ for 1-2 h, and then cooled to a temperature of-30℃~-50℃, and frozen for 2-3 h;

[0014] S2, primary drying: primary drying is performed at a temperature of 5℃-10℃ for 30-40 h;

[0015] S3, resolution drying: resolution drying is performed at a temperature of 30℃-35℃ for 2-3 h.

[0016] The utility model provides a kind of vacuum freeze drying equipment, including freeze vacuum drying chamber, one side of the freeze vacuum drying chamber is equipped with normal temperature vacuum crushing chamber, the inner chamber bottom of the freeze vacuum drying chamber is equipped with recess, the recess extends to the inside of the normal temperature vacuum crushing chamber, the freeze vacuum drying chamber is equipped with placement plate, the placement plate top is equipped with quick-mounting assembly for installing vial, the placement plate bottom is slidably connected with the recess, the recess middle is equipped with notch, the partition door is matched with the notch;The outside of the freeze vacuum drying chamber is equipped with freezing layer, the freezing layer outside is connected with refrigeration assembly, the refrigeration assembly is located at the back of the freeze vacuum drying chamber, the refrigeration assembly one side is equipped with vacuum pump, the vacuum pump is respectively communicated with the freeze vacuum drying chamber and the normal temperature vacuum crushing chamber;The inside of the normal temperature vacuum crushing chamber top is equipped with linear drive crushing mechanism, the linear drive crushing mechanism includes several vibration crushing components, the vibration crushing component corresponds with the vial on the placement plate.

[0017] Preferably, one side of the freeze vacuum drying chamber is provided with a cold air pipe in communication with the freezing layer, the cold air pipe is internally provided with a spring air valve, the spring air valve has a spring force directed towards the outlet of the cold air pipe, one side of the placement plate is provided with a needle tube corresponding to the cold air pipe.

[0018] Preferably, the bottom of the placement plate is provided with a plurality of pulley seats, the pulley seats are rotatably provided with rollers, each pulley seat is provided with at least two rollers, the pulley seats are matched with the recess, the rollers are slidably located in the recess, the quick-mounting assembly includes a plurality of fixed bases, the fixed bases are respectively located on the upper surface of the placement plate, the fixed bases are provided with a neck portion above, and the neck portion is used for fixing the vial.

[0019] Preferably, the outside of the freeze vacuum drying chamber is provided with a freeze-drying sealing door, the inside of the freeze-drying sealing door is provided with a profiled sealing rubber strip, one side of the inner wall of the freeze-drying sealing door is provided with a wedge-shaped push block corresponding to the placement plate body, the other side of the freeze-drying sealing door is rotatably connected with the outer wall of the freeze vacuum drying chamber, when the freeze-drying sealing door is closed, the wedge-shaped push block is in contact with the placement plate and pushes the placement plate to move towards the side surface of the freeze vacuum drying chamber, and the needle tube extends into the cold air pipe.

[0020] Preferably, the linear drive crushing mechanism further includes a linear drive rod, the normal temperature vacuum crushing chamber is provided with a mounting groove above, the linear drive rod is mounted at the top of the mounting groove, the linear drive rod is provided with a mounting carrier plate at the bottom, and the vibration crushing component is mounted at the bottom of the mounting carrier plate.

[0021] Preferably, the vibration crushing assembly comprises a vibration motor, the vibration motor is located at the bottom of the mounting plate, the bottom of the mounting plate is provided with a connecting rod, the bottom of the connecting rod is provided with a crushing mounting plate, a circular hole is formed in the crushing mounting plate, a vibration rod is arranged in the circular hole, a vibration spring is arranged on the side of the vibration rod, a vibration plate is arranged above the vibration rod, and the vibration spring is located between the vibration plate and the crushing mounting plate.

[0022] Preferably, the bottom of the vibration rod is provided with a rubber layer, the outer side of the rubber layer is provided with a rubber brush, the rubber brush does not contact the vial during the vial insertion process; and the circular hole is a narrow-necked circular hole.

[0023] Preferably, the refrigeration assembly comprises a throttling expansion valve, an evaporator, a compressor and a condenser, one end of the throttling expansion valve is connected with the freezing layer, the other end of the throttling expansion valve is connected with the evaporator, the other end of the evaporator is connected with the compressor, the other end of the compressor is connected with the condenser, and the condenser is connected with the freezing layer through a connecting pipe.

[0024] Preferably, the vacuum pump is connected with the freezing vacuum drying cavity and the normal-temperature vacuum crushing cavity through pipelines respectively, and a control valve is arranged in the middle of the pipeline, and the control valve is used for controlling the vacuum treatment of the freezing vacuum drying cavity and the normal-temperature vacuum crushing cavity by the vacuum pump.

[0025] Compared with the prior art, the vacuum freezing drying equipment has the following beneficial effects:

[0026] 1. The vacuum freezing drying equipment drives the mounting plate to move through the linear driving rod, so that the vibration crushing assembly at the bottom of the mounting plate contacts the vial above the mounting plate, then the mounting plate is vibrated by the vibration motor, the mounting plate drives the crushing mounting plate at the bottom thereof through the connecting rod, at this time, the vibration rod on the crushing mounting plate drives the vibration plate to shake under the action of the vibration spring, then the vibration plate transmits the vibration force generated by the shaking to the vibration rod, the vibration rod vibrates in the vial, and the blended collagen gel is crushed by freezing; the rubber layer and the rubber brush at the bottom of the vibration rod crush the blended collagen gel by freezing when the vibration rod vibrates, and the rubber brush does not damage the vial, and the circular hole is a narrow-necked circular hole, so that the vibration rod is in curved surface contact with the circular hole when the vibration rod vibrates, and the vibration rod vibrates better.

[0027] 2、the vacuum freeze-drying equipment, through vacuum pump and pipeline are connected with freeze vacuum drying cavity and normal temperature vacuum crushing cavity respectively, and the freeze vacuum drying cavity and normal temperature vacuum crushing cavity are independently vacuumized, wherein when the normal temperature vacuum crushing cavity is vacuumized, the inside of the normal temperature vacuum crushing cavity is in a vacuum normal temperature state, at this time the blended collagen gel in the vial is freeze-dried in a vacuum normal temperature state, gradually heated, and due to the vacuum state, the blended collagen gel is prevented from absorbing normal temperature water vapor in the heating process, resulting in that the blended collagen gel is crushed into powder and then humidified.

[0028] 3、the vacuum freeze-drying equipment, through at least two rollers are arranged at the bottom of each pulley seat, since the setting plate is in a low temperature state in the freeze vacuum drying cavity, the setting plate is not easy to contact, and in the process of pushing the setting plate from the freeze vacuum drying cavity into the normal temperature vacuum crushing cavity, the setting plate needs to pass through the groove, and the arrangement of the at least two rollers can smoothly pass through the groove, so that the setting plate does not shake when pushing, and the vial in a frozen state is prevented from being broken. BRIEF DESCRIPTION OF DRAWINGS

[0029] Figure 1 the whole of the present application is a schematic diagram of the freeze-drying sealing door assembly structure;

[0030] Figure 2 the freeze vacuum drying cavity and the normal temperature vacuum crushing cavity of the present application are schematic diagrams of internal partial structures;

[0031] Figure 3 the linear drive crushing mechanism structure of the present application is a schematic diagram;

[0032] Figure 4 the freeze vacuum drying cavity and the normal temperature vacuum crushing cavity of the present application are schematic diagrams of internal partial structures;

[0033] Figure 5 the setting plate of the present application is a partial structure schematic diagram;

[0034] Figure 6 the refrigeration assembly and vacuum pump of the present application are partial structure schematic diagrams;

[0035] Figure 7 is a column chart of the skin horny layer water content using 0-8 weeks of the freeze-dried composition samples prepared in examples 1-3 and comparative example 1 of the present application. DETAILED DESCRIPTION

[0036] With reference to the drawings of the embodiments of the present application, the technical solutions in the embodiments of the present application will be described clearly and completely. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments of the present application. Based on the embodiments of the present application, all the other embodiments obtained by those of ordinary skill in the art without creative work fall within the scope of the present application.

[0037] Please refer to Figures 1-6 A vacuum freeze-drying equipment, comprising a freeze vacuum drying chamber 1, one side of the freeze vacuum drying chamber 1 is provided with a normal temperature vacuum crushing chamber 2, the inner cavity bottom of the freeze vacuum drying chamber 1 is provided with a groove 3, the groove 3 extends to the inside of the normal temperature vacuum crushing chamber 2, the freeze vacuum drying chamber 1 is provided with a placement plate 4, a plurality of quick mounting assemblies 5 for installing the vials are arranged above the placement plate 4, the bottom of the placement plate 4 is in sliding connection with the groove 3, a closable partition door 6 is arranged between the freeze vacuum drying chamber 1 and the normal temperature vacuum crushing chamber 2, a notch 31 is arranged in the middle of the groove 3, and the partition door 6 is matched with the notch 31; a freezing layer 11 is arranged outside the freeze vacuum drying chamber 1, a refrigeration assembly 7 is connected outside the freezing layer 11, the refrigeration assembly 7 is located at the back of the freeze vacuum drying chamber 1, a vacuum pump 8 is arranged on one side of the refrigeration assembly 7, and the vacuum pump 8 is in communication with the freeze vacuum drying chamber 1 and the normal temperature vacuum crushing chamber 2 respectively; a linear drive crushing mechanism 9 is arranged above the inside of the normal temperature vacuum crushing chamber 2, the linear drive crushing mechanism 9 comprises a plurality of vibrating crushing assemblies 91, and the vibrating crushing assemblies 91 correspond to the vials on the placement plate 4.

[0038] In use, first, the blended collagen glue is installed in the vials, then the vials are fixed on the installation plate 4 through the quick mounting assembly 5 respectively, and then the installation plate 4 is pushed into the refrigerated vacuum drying cavity 1; at this time, the partition door 6 between the refrigerated vacuum drying cavity 1 and the normal-temperature vacuum crushing cavity 2 falls, and the refrigerated vacuum drying cavity 1 is in a closed state, then the refrigeration assembly 7 is started to perform refrigeration treatment on the refrigeration layer 11, and the vacuum pump 8 is started to perform vacuum treatment on the inside of the refrigerated vacuum drying cavity 1, so that the blended collagen glue in the vials is sublimated in a vacuum refrigeration environment to lose moisture and obtain blended collagen glue freeze-dried; then the partition door 6 between the refrigerated vacuum drying cavity 1 and the normal-temperature vacuum crushing cavity 2 is opened, and the installation plate 4 carrying the blended collagen glue freeze-dried in the vials enters the normal-temperature vacuum crushing cavity 2, at this time, another set of installation plate 4 carrying the blended collagen glue and vials are put into the refrigerated vacuum drying cavity 1 again, and the partition door 6 is lowered, so that the refrigerated vacuum drying cavity 1 and the normal-temperature vacuum crushing cavity 2 are in two independent vacuum spaces, at this time, the refrigerated vacuum drying cavity 1 performs vacuum refrigeration drying treatment on another set of blended collagen glue, while the normal-temperature vacuum crushing cavity 2 performs crushing on the blended collagen glue freeze-dried through the linear driving crushing mechanism 9, wherein the vibration crushing assembly 91 performs crushing on the blended collagen glue freeze-dried in the vials in a vibrating manner, and after crushing, the vibration crushing assembly 91 is raised in a vibrating state, at this time, the blended collagen glue freeze-dried powder on the vibration crushing assembly 91 can be shaken off, and the vibration can also cause the vials to be separated from the quick mounting assembly 5, so that the vials containing the blended collagen glue freeze-dried powder can be conveniently taken out.

[0039] Preferably, the refrigerated vacuum drying cavity 1 is provided with a cold air pipe 12 on one side, the cold air pipe 12 is in communication with the refrigeration layer 11, the cold air pipe 12 is provided with a spring air valve inside, the spring air valve is forced away from the outlet direction of the cold air pipe 12, and the installation plate 4 is provided with a needle tube 41 on one side, the needle tube 41 corresponds to the cold air pipe 12; through the cold air pipe 12 provided on one side of the refrigerated vacuum drying cavity 1, the needle tube 41 on the installation plate 4 pushes the spring air valve away from the outlet direction of the cold air pipe 12 during the process of extending into the cold air pipe 12, so that the cold air pipe 12 is in communication with the needle tube 41, and then the cold air in the refrigeration layer 11 cools the installation plate 4, so that the cooling and refrigeration effect is better, and a longitudinal covering plate is further provided above the inner cavity of the refrigerated vacuum drying cavity 1, which can better transfer the refrigeration effect, so that the inner cavity of the refrigerated vacuum drying cavity 1 quickly enters a low-temperature refrigeration state.

[0040] Preferably, the bottom of the setting plate 4 is provided with a plurality of pulley seats 42, and a plurality of rollers 43 are rotatably arranged in each pulley seat 42, and at least two rollers 43 are arranged in each pulley seat 42, the pulley seat 42 is matched with the groove 3, and the roller 43 slides in the groove 3, the quick-mounting assembly 5 comprises a plurality of fixed bases 51 arranged on the upper surface of the setting plate 4, and a neck 52 is arranged above the fixed base 51 for fixing a penicillin bottle; since the setting plate 4 is in a low-temperature state when it is pushed into the normal-temperature vacuum crushing cavity 2 from the freezing vacuum drying cavity 1, it is not easy to touch, and at least two rollers 43 are arranged at the bottom of each pulley seat 42, so that the setting plate 4 can smoothly pass through the groove 3, and the setting plate 4 does not shake when it is pushed, thereby avoiding the breakage of the penicillin bottle in a frozen state.

[0041] Preferably, the outer side of the freezing vacuum drying cavity 1 is provided with a freeze-drying sealing door 14, the inner side of the freeze-drying sealing door 14 is provided with a profiled sealing rubber strip 15, one side of the inner wall of the freeze-drying sealing door 14 is provided with a wedge-shaped push block corresponding to the body of the setting plate 4, and the other side of the freeze-drying sealing door 14 is rotatably connected with the outer wall of the freezing vacuum drying cavity 1; when the freeze-drying sealing door 14 is closed, the wedge-shaped push block contacts the setting plate 4 and pushes the setting plate 4 to move to the side of the freezing vacuum drying cavity 1, and the needle tube 41 extends into the cold air pipe 12; the profiled sealing rubber strip 15 arranged on the inner side of the freeze-drying sealing door 14 is in the shape of a “mountain”, and the good sealing effect of the profiled sealing rubber strip 15 is utilized; when the freezing vacuum drying cavity 1 is in deep space negative pressure, the profiled sealing rubber strip 15 is adsorbed on the flange surface of the freezing vacuum drying cavity 1, so that the higher the negative pressure intensity is, the tighter the adsorption is, and the better the sealing effect is; when the freeze-drying sealing door 14 moves to the entrance of the freezing vacuum drying cavity 1, the wedge-shaped push block first contacts the setting plate 4, and then the wedge-shaped push block pushes the setting plate 4 to move to the direction of the cold air pipe 12 arranged on the side of the freezing vacuum drying cavity 1 as the freeze-drying sealing door 14 is closed, so that the needle tube 41 on the setting plate 4 extends into the cold air pipe 12 and communicates with the cold air pipe 12, and the setting plate 4 is further provided with a cavity for storing cold air.

[0042] Preferably, the linear drive crushing mechanism 9 further comprises a linear drive rod 92, an installation groove 21 is arranged above the normal temperature vacuum crushing cavity 2, the linear drive rod 92 is installed at the top of the installation groove 21, the linear drive rod 92 is provided with an installation carrier plate 93 at the bottom, and the vibration crushing assembly 91 is installed at the bottom of the installation carrier plate 93; the vibration crushing assembly 91 at the bottom of the installation carrier plate 93 is contacted with the vial above the installation plate 4 by moving the installation carrier plate 93 driven by the linear drive rod 92, so that the blended collagen gel freeze-dried in the vial is crushed by vibration.

[0043] Preferably, the vibration crushing assembly 91 comprises a vibration motor 911, the vibration motor 911 is located at the bottom of the installation carrier plate 93, the bottom of the installation carrier plate 93 is provided with a connecting rod 94, the bottom of the connecting rod 94 is provided with a crushing installation plate 95, a circular hole 912 is arranged on the crushing installation plate 95, a vibration rod 913 is arranged in the circular hole 912, vibration springs 914 are arranged on the periphery of the vibration rod 913, a vibration plate 915 is arranged above the vibration rod 913, and the vibration springs 914 are located between the vibration plate 915 and the crushing installation plate 95; the installation carrier plate 93 is vibrated by the vibration motor 911, the crushing installation plate 95 at the bottom of the installation carrier plate 93 is driven by the connecting rod 94, at this time, the vibration rod 913 on the crushing installation plate 95 drives the vibration plate 915 to shake under the action of the vibration springs 914, and then the vibration plate 915 transmits the vibration force generated by the shaking to the vibration rod 913, the vibration rod 913 vibrates in the vial, and then the blended collagen gel freeze-dried is crushed.

[0044] Preferably, the vibration rod 913 is provided with a rubber layer 916 at the bottom, and a rubber brush 917 is arranged outside the rubber layer 916, the rubber brush 917 does not contact the vial during being put into the vial; the circular hole 912 is a narrow-necked circular hole; the rubber layer 916 and the rubber brush 917 arranged at the bottom of the vibration rod 913, when the vibration rod 913 vibrates, the rubber brush 917 crushes the blended collagen gel freeze-dried, and does not cause damage to the vial, and the circular hole 912 is arranged as a narrow-necked circular hole, so that the vibration rod 913 is in curved surface contact with the circular hole 912 when vibrating, so that the vibration rod 913 vibrates better.

[0045] Preferably, the refrigeration assembly 7 comprises a throttling expansion valve 71, an evaporator 72, a compressor 73, and a condenser 74, one end of the throttling expansion valve 71 is connected with the freezing layer 11, the other end of the throttling expansion valve 71 is connected with the evaporator 72, the other end of the evaporator 72 is connected with the compressor 73, the other end of the compressor 73 is connected with the condenser 74, and the condenser 74 is communicated with the freezing layer 11 through a connecting pipe; the refrigerant in a gaseous state from the evaporator 72 is compressed adiabatically by the compressor 73, and then becomes a high-temperature and high-pressure state; the compressed gaseous refrigerant is cooled and condensed at constant pressure in the condenser 74, and then changes into a liquid state refrigerant; the condensed liquid state refrigerant is expanded to a low pressure by the throttling expansion valve 71, and becomes a gas-liquid mixture; the low-temperature and low-pressure liquid state refrigerant absorbs heat of the heat pipe in the evaporator 72, and becomes a gaseous refrigerant again; the gaseous refrigerant reenters the compressor 73 through the pipeline to start a new cycle; the refrigerant is transferred to the heat pipe, and the freezing layer 11 is cooled by temperature conduction of the heat pipe.

[0046] Preferably, the vacuum pump 8 is connected with the freezing vacuum drying cavity 1 and the normal temperature vacuum crushing cavity 2 through pipelines 81 respectively, and a control valve 82 is arranged in the middle of the pipeline 81, which is used to control the vacuum treatment of the freezing vacuum drying cavity 1 and the normal temperature vacuum crushing cavity 2 by the vacuum pump 8; the freezing vacuum drying cavity 1 and the normal temperature vacuum crushing cavity 2 are separately vacuum treated through the vacuum pump 8 and the pipelines 81; when the normal temperature vacuum crushing cavity 2 is vacuum treated, the inside of the normal temperature vacuum crushing cavity 2 is in a vacuum normal temperature state, at this time, the blended collagen gel in the vial is gradually warmed in the vacuum normal temperature state, and since it is in a vacuum state, the blended collagen gel is prevented from absorbing normal temperature water vapor in the warming process, so that the blended collagen gel is not humid after being crushed into powder.

[0047] Working principle: in use, first, the blended collagen gel is loaded into the vial, then the vial is fixed on the installation plate 4 through the quick mounting assembly 5, and then the installation plate 4 is pushed into the freezing vacuum drying cavity 1; at this time, the partition door 6 between the freezing vacuum drying cavity 1 and the normal temperature vacuum crushing cavity 2 falls down, and the freezing vacuum drying cavity 1 is in a closed state, then the refrigeration assembly 7 is started to cool the freezing layer 11, and the vacuum pump 8 is started to vacuum treat the inside of the freezing vacuum drying cavity 1, so that the blended collagen gel in the vial is sublimed in a vacuum freezing environment, loses moisture, and obtains blended collagen gel freeze-dried.

[0048] The special-shaped sealing rubber strip 15 arranged inside the freeze-drying sealing door 14 is in the shape of "mountain", and the special-shaped sealing rubber strip 15 is adsorbed on the flange surface of the freeze-vacuum drying cavity 1 when the inside of the freeze-vacuum drying cavity 1 is in deep vacuum negative pressure, so that the higher the negative pressure intensity is, the tighter the adsorption is, and the better the sealing effect is; when the freeze-drying sealing door 14 moves towards the entrance of the freeze-vacuum drying cavity 1, the wedge-shaped push block first contacts the setting plate 4, and then the wedge-shaped push block pushes the setting plate 4 to move towards the cold air pipe 12 arranged on the side of the freeze-vacuum drying cavity 1, so that the needle pipe 41 on the setting plate 4 extends into the cold air pipe 12 and the needle pipe 41 communicates with the cold air pipe 12, and the setting plate 4 is further provided with a cavity for storing cold air;

[0049] After the setting plate 4 is placed in the freeze-vacuum drying cavity 1, the needle pipe 41 pushes the spring air valve away from the outlet direction of the cold air pipe 12 in the process that the needle pipe 41 on the setting plate 4 extends into the cold air pipe 12, so that the cold air pipe 12 communicates with the needle pipe 41, and then the cold air in the freeze layer 11 cools the setting plate 4, so that the cooling effect is better, and a longitudinal covering plate is further arranged above the inner cavity of the freeze-vacuum drying cavity 1, so that the refrigeration effect is better transmitted, and the inner cavity of the freeze-vacuum drying cavity 1 is quickly in a low-temperature freezing state;

[0050] During the freezing process, the refrigerant in the gaseous state from the evaporator 72 is adiabatically compressed by the compressor 73, and then becomes in a high-temperature and high-pressure state. The gaseous refrigerant after compression is cooled and condensed in the condenser 74, and then changes into liquid-state refrigerant. The liquid-state refrigerant is expanded to low pressure by the throttling expansion valve 71, and then becomes a gas-liquid mixture. The liquid-state refrigerant at low temperature and low pressure absorbs the heat of the heat pipe in the evaporator 72, and then changes into gaseous refrigerant again. The gaseous refrigerant reenters the compressor 73 through the pipeline, and starts a new cycle. The refrigerant is transmitted to the heat pipe, and the heat pipe conducts the temperature to the freeze layer 11, so that the freeze layer is cooled;

[0051] After vacuum freeze-drying, open the partition door 6 between the freeze vacuum drying chamber 1 and the normal temperature vacuum crushing chamber 2, and place the setting plate 4 carrying the blended collagen gel in the vials into the normal temperature vacuum crushing chamber 2. At this time, put another group of setting plates 4 carrying blended collagen gel into the freeze vacuum drying chamber 1, and lower the partition door 6, so that the freeze vacuum drying chamber 1 and the normal temperature vacuum crushing chamber 2 are in two independent vacuum spaces. At this time, the freeze vacuum drying chamber 1 carries out vacuum freeze-drying treatment on another group of blended collagen gel, while the normal temperature vacuum crushing chamber 2 carries out crushing on the blended collagen gel freeze-dried by the linear drive crushing mechanism 9. The vacuum pump 8 and the pipeline 81 are connected with the freeze vacuum drying chamber 1 and the normal temperature vacuum crushing chamber 2 respectively to carry out vacuum treatment on the freeze vacuum drying chamber 1 and the normal temperature vacuum crushing chamber 2 separately. When the normal temperature vacuum crushing chamber 2 is treated in vacuum, the inside of the normal temperature vacuum crushing chamber 2 is in a vacuum normal temperature state. At this time, the blended collagen gel freeze-dried in the vials gradually warms up in the vacuum normal temperature state. Since it is in a vacuum state, the blended collagen gel freeze-dried does not absorb normal temperature water vapor in the warming process, so that the blended collagen gel freeze-dried is not humid after being crushed into powder.

[0052] When the setting plate 4 is moved from the freeze vacuum drying chamber 1 to the normal temperature vacuum crushing chamber 2, at least two rollers 43 are arranged at the bottom of each pulley seat 42. Since the setting plate 4 is in a low temperature state in the freeze vacuum drying chamber 1, it is not easy to touch. When the setting plate 4 is pushed from the freeze vacuum drying chamber 1 to the normal temperature vacuum crushing chamber 2, it needs to pass through the groove 3. The arrangement of at least two rollers 43 can smoothly pass through the groove 3, so that the setting plate 4 does not shake when it is pushed, thereby avoiding the breakage of the vials in the frozen state.

[0053] The linear drive rod 92 drives the installation carrier plate 93 to move, so that the vibration crushing assembly 91 at the bottom of the installation carrier plate 93 contacts the vials above the setting plate 4. The vibration motor 911 drives the installation carrier plate 93 to vibrate. The installation carrier plate 93 drives the crushing installation plate 95 at the bottom thereof through the connecting rod 94. At this time, the vibration rod 913 on the crushing installation plate 95 shakes under the action of the vibration spring 914, and the vibration plate 915 further transmits the vibration force generated by the shaking to the vibration rod 913. The vibration rod 913 vibrates in the vial, and the blended collagen gel freeze-dried is crushed. The rubber layer 916 and the rubber brush 917 arranged at the bottom of the vibration rod 913 crush the blended collagen gel freeze-dried when the vibration rod 913 vibrates, and do not harm the vials. The round hole 912 is arranged as a thin-necked round hole, so that the vibration rod 913 is in curved surface contact with the round hole 912 when it vibrates, so that the vibration rod 913 vibrates better.

[0054] When vacuum crushing at room temperature, the vibration crushing assembly 91 crushes the blended collagen gel freeze-dried in the vial in a vibrating manner, and after crushing, the vibration crushing assembly 91 is lifted in a vibrating state, at which time the blended collagen gel freeze-dried powder on the vibration crushing assembly 91 can be shaken off, and the vibration can also cause the vial to be separated from the quick-assembly component 5, so that the vial containing the blended collagen gel freeze-dried powder can be conveniently removed.

[0055] Embodiment 1

[0056] The embodiment provides a preparation method of a freeze-dried composition with anti-wrinkle repair effect and stability, and the method comprises the following steps:

[0057] 1. Deionized water is added to a stirring kettle, and sodium citrate and whey protein are sequentially added, and stirred at a speed of 50 r / min at room temperature for 20 min; and then, telopeptide collagen, soluble collagen and mannitol are added, and stirred at a speed of 50 r / min at room temperature for 50 min, to obtain blended collagen gel.

[0058] The mass ratio of deionized water, telopeptide collagen, soluble collagen, whey protein, sodium citrate and mannitol is 98.3:0.1:0.1:0.4:0.1:1.

[0059] 2. The blended collagen gel is poured into a vial, and freeze-drying is performed in a vacuum freeze-drying device, and the vial is taken out, to obtain a freeze-dried composition with anti-wrinkle repair effect and stability.

[0060] The vacuum freeze-drying specifically comprises the following steps:

[0061] S1, pre-freezing: the vial containing the blended collagen gel is frozen at 0 ℃ for 2 h, and then the temperature is lowered to -30 ℃ at a pre-freezing speed of -1 ℃ / min, and frozen for 3 h; the pre-freezing pressure is normal pressure.

[0062] S2, primary drying: primary drying is performed at 5 ℃ for 40 h, and the pressure is 20 Pa;

[0063] S3, resolution drying: resolution drying is performed at 30 ℃ for 3 h, and the pressure is 20 Pa.

[0064] Embodiment 2

[0065] The embodiment provides a preparation method of a freeze-dried composition with anti-wrinkle repair effect and stability, and the method comprises the following steps:

[0066] 1. Deionized water is added to a stirring kettle, and sodium citrate and whey protein are sequentially added, and stirred at a speed of 50 r / min at room temperature for 20 min; and then, telopeptide collagen, soluble collagen and mannitol are added, and stirred at a speed of 50 r / min at room temperature for 50 min, to obtain blended collagen gel.

[0067] Deionized water, end-lacking collagen, soluble collagen, whey protein, sodium citrate and mannitol in a mass ratio of 97:0.15:0.15:0.55:0.15:2.

[0068] 2. The blended collagen glue is poured into a vial, and vacuum freeze-drying is performed in a vacuum freeze-drying device, and the vial is taken out, to obtain a freeze-dried composition with anti-wrinkle repair effect and stability.

[0069] The vacuum freeze-drying specifically includes the following steps:

[0070] S1, pre-freezing: the vial containing the blended collagen glue is frozen at a temperature of -3°C for 1.7 h, and then the temperature is lowered to -35°C at a pre-freezing speed of -1°C / min, and frozen for 2.7 h; the pre-freezing pressure is normal pressure;

[0071] S2, primary drying: primary drying is performed at a temperature of 6°C for 37 h, and the pressure is 20 Pa;

[0072] S3, resolution drying: resolution drying is performed at a temperature of 31°C for 2.7 h, and the pressure is 20 Pa.

[0073] Example 3

[0074] The embodiment provides a preparation method of a freeze-dried composition with anti-wrinkle repair effect and stability, including the following steps:

[0075] 1. Deionized water is added to a stirred tank, and sodium citrate and whey protein are sequentially added, and stirred at room temperature at a speed of 50 r / min for 15 min; end-lacking collagen, soluble collagen and mannitol are added, and stirred at room temperature at a speed of 50 r / min for 30 min, to obtain blended collagen glue;

[0076] Deionized water, end-lacking collagen, soluble collagen, whey protein, sodium citrate and mannitol in a mass ratio of 93.1:0.3:0.3:1:0.3:5.

[0077] 2. The blended collagen glue is poured into a vial, and vacuum freeze-drying is performed in a vacuum freeze-drying device, and the vial is taken out, to obtain a freeze-dried composition with anti-wrinkle repair effect and stability.

[0078] The vacuum freeze-drying specifically includes the following steps:

[0079] S1, pre-freezing: the vial containing the blended collagen glue is frozen at a temperature of -3°C for 1.7 h, and then the temperature is lowered to -35°C at a pre-freezing speed of -1°C / min, and frozen for 2.7 h; the pre-freezing pressure is normal pressure;

[0080] S2, primary drying: primary drying is performed at a temperature of 6°C for 37 h, and the pressure is 20 Pa;

[0081] S3, desorption drying: desorption drying at a temperature of 35℃ for 3h, and a pressure of 20Pa.

[0082] Comparative Example 1

[0083] The control sample was prepared in the manner of Reference Example 1, and the control was a mannitol freeze-dried solution alone, i.e., the difference between Example 1 and Comparative Example 1 was the composition of the raw materials, and the raw materials of Comparative Example 1 included deionized water, mannitol, and the mass ratio of deionized water to mannitol was 99:1.

[0084] In the embodiments and comparative examples of the present application, the soluble collagen was collagen DC6 purchased from Wuxi Bedee Biological Engineering Co., Ltd., appearance: white or light yellow solid; the telopeptide-free collagen was collagen KR3 purchased from Wuxi Bedee Biological Engineering Co., Ltd., appearance: white or light yellow solid; the sodium citrate was purchased from Shandong Yingxuan Industry Co., Ltd., CAS: 6132-04-3, appearance: white powder; and the whey protein was Milk Peptide Complex produced by CLR (Chemisches Laboratorium Dr. Kurt Richter GmbH) in Germany, appearance: white powder. The vacuum freeze-drying equipment used in the embodiments and comparative examples of the present application was preferably the vacuum freeze-drying equipment disclosed in the present application.

[0085] Test Example

[0086] The freeze-dried compositions with anti-wrinkle repair efficacy and stability prepared in Examples 1-3 and Comparative Example 1 of the present application were respectively mixed with deionized water at a mass ratio of 1:5, dissolved, numbered, and corresponded to samples 1-4, respectively, and the samples 1-4 were subjected to performance testing.

[0087] (1) The anti-wrinkle performance was tested, and the testing method was as follows: 80 healthy female volunteers aged 30-55 years old were selected, and the volunteers were required to have obvious wrinkles. The volunteers were randomly divided into 4 groups, 20 people in each group, and one of samples 1-4 was used on the cheeks of the volunteers according to the requirements twice a day for 8 consecutive weeks. The volunteers were required to mainly engage in indoor activities during the test period, and avoid long-term unprotected exposure to sunlight. The freeze-dried compositions with anti-wrinkle repair efficacy and stability were used for 0 weeks, 2 weeks, 4 weeks, 6 weeks, and 8 weeks, and a Cutometer MPA 580 skin elasticity tester was selected to test the water content of the skin at the corner of the eye in a 25℃ relative humidity environment, and the average value of each group was taken; the test results are shown in Table 1.

[0088] Table 1

[0089]

[0090] According to the test results in Table 1, it can be seen that after the volunteers used samples 1-3 to wipe the whole face, the skin moisture content at the corner of the eye was significantly increased compared with before using samples 1-3, and the anti-wrinkle performance was good. The comparative example 1 only contains mannitol, and the composition is single, without endocollagen, soluble collagen and whey protein for synergistic anti-wrinkle, and the anti-wrinkle effect is decreased.

[0091] (2) Repair efficacy test, the test method is as follows: 80 healthy female volunteers aged 30-55 years old are selected, and the volunteers are required to have skin problems such as facial dryness, desquamation, redness, itching and stinging, and the volunteers are randomly divided into 4 groups, 20 people in each group, and one of samples 1-4 is used on the cheeks according to the requirements for 8 weeks. The freeze-dried composition product with anti-wrinkle repair efficacy and stability is used for 0 weeks, 2 weeks, 4 weeks, 6 weeks, and 8 weeks, and Tewameter TM210 is selected to measure the trans-epidermal water loss rate TEWL value, and the average value of each group is taken. In order to conveniently and intuitively view the data change, the TEWL ratio of the patch site TEWL value to the normal skin TEWL value is recorded in the table. Self-evaluation is scored, and the evaluation index is: skin moisture, skin softness, skin roughness, skin texture, overall soothing satisfaction, soothing hotness satisfaction, desquamation relief satisfaction, and overall improvement satisfaction of skin after use. The scoring standard is: 1 point for very dissatisfied, 2 points for dissatisfied, 3 points for general, 4 points for satisfied, and 5 points for very satisfied. The scoring of each group is counted, and the percentage of the number of people scoring 3 points or more is counted. The higher the percentage of the number of people scoring 3 points or more, the higher the improvement satisfaction of the corresponding item; the test results are shown in Table 2.

[0092] Table 2

[0093]

[0094] According to the test results in Table 2, it can be seen that after the volunteers used samples 1-3 to wipe the whole face, the skin was repaired compared with before using samples 1-3, and the TEWL ratio can reflect the change of skin barrier function. The smaller the value, the better the skin barrier and the better the repair effect. In the comparative example 3, only the single repair component mannitol is used, without synergistic repair components, and the repair ability is reduced.

[0095] (3) Safety performance test, its test method is as follows: 35 healthy, age 18-60 years old volunteers are selected, and the mildness test is carried out according to the "Cosmetic Safety Technical Specification 2015 Edition" - human skin patch test. According to GB 171492-1997 "Diagnosis standard and treatment principle of contact dermatitis of cosmetics", it is confirmed that the subjects have no serious systemic diseases, no immune deficiency or autoimmune diseases, no active allergic diseases, no history of allergic reactions to skin care cosmetics, no systemic use of hormone drugs and immune suppressants in the past month, non-pregnant or lactating, no ethical taboo. Sample 1-4 are subjected to patch test, wherein the blank sample of the patch tester. With the closed patch test method, about 0.020m of the test object is placed in the patch tester, and the outer low sensitization adhesive tape is attached to the back of the subject, and after 24 hours, the test object is removed, and the skin reaction is observed once at 0h, 0.5h, 24h and 48h respectively; wherein the reaction results are recorded according to the grading standard, 0 level is negative reaction, 1 level is suspicious reaction, only weak erythema, 2 level is weak positive reaction, erythema, infiltration, edema, there may be papules, 3 level is strong positive reaction, erythema, infiltration, edema, papules, vesicular reaction may exceed the test area, 4 level is very strong positive reaction, obvious erythema, severe infiltration, edema, fusion vesicle, reaction beyond the test area; the test results are shown in Table 3;

[0096] Table 3

[0097]

[0098] According to the test results in Table 3, samples 1-4 all meet the composite cosmetic safety standards, and have high safety performance.

[0099] The truncated collagen is a natural extracted collagen, which has good biocompatibility and can quickly enter the deep layer of the skin, has good nutritional effect on the skin. And there are a large number of carboxyl and hydroxyl groups in the collagen, such as hydroxyproline and hydroxylysine, and a large number of natural moisturizing factors such as glycine, which can improve the water storage capacity of tissue cells, and has good promoting effect on the growth, division, proliferation, migration and differentiation of skin cells. Collagen can provide nutrients to the skin, delay skin aging, and promote wound repair of the skin.

[0100] The soluble collagen is subjected to secondary cutting on the basis of the truncated collagen, so that the collagen protein presents a multi-molecular weight distribution and has a certain triple helix structure, so that it can be better absorbed through the skin. The collagen protein can enter the dermis layer and play its biological effects of promoting cell proliferation and migration, regulating tissue repair and regeneration, and delaying skin aging.

[0101] Whey protein can re-activate skin cells and induce extracellular matrix molecules (such as type I collagen, hyaluronic acid, fibronectin) in the dermis layer. It can quickly and efficiently reduce wrinkle depth and improve skin structure. Sodium citrate can make collagen and whey protein better dissolved in the water phase.

[0102] Mannitol is a six-membered alcohol. Its functions currently include inhibiting skin damage, skin allergy, and light damage, maintaining oligopeptide activity, and helping skin conditioning. At the same time, it can also combine with water in the form of hydrogen bonds to play a role in water locking and moisturizing, and can also relieve and repair damaged skin barriers.

[0103] Although embodiments of the present application have been shown and described, it is to be understood that various modifications, substitutions, replacements and changes can be made to these embodiments without departing from the principles and spirit of the present application, and the scope of the present application is defined by the appended claims and their equivalents.

Claims

1. A vacuum freeze-drying apparatus comprising a freeze vacuum drying chamber (1), characterized in that: The side of the freezing vacuum drying cavity (1) is provided with a normal temperature vacuum crushing cavity (2), the bottom of the inner cavity of the freezing vacuum drying cavity (1) is provided with a groove (3), the groove (3) extends to the inside of the normal temperature vacuum crushing cavity (2), the freezing vacuum drying cavity (1) is provided with a placing plate (4), the upper side of the placing plate (4) is provided with a quick mounting assembly (5) for mounting a plurality of penicillin bottles, the bottom of the placing plate (4) is slidably connected with the groove (3), the freezing vacuum drying cavity (1) and the normal temperature vacuum crushing cavity (2) are provided with an openable and closable partition door (6), the middle of the groove (3) is provided with a gap (31), the partition door (6) is matched with the gap (31); the outside of the freezing vacuum drying cavity (1) is provided with a freezing layer (11), the outside of the freezing layer (11) is connected with a refrigeration assembly (7), the refrigeration assembly (7) is located at the back of the freezing vacuum drying cavity (1), the side of the refrigeration assembly (7) is provided with a vacuum pump (8), the vacuum pump (8) is respectively communicated with the freezing vacuum drying cavity (1) and the normal temperature vacuum crushing cavity (2); the inside of the normal temperature vacuum crushing cavity (2) is provided with a linear drive crushing mechanism (9) at the upper side, the linear drive crushing mechanism (9) comprises a plurality of vibrating crushing assemblies (91), the vibrating crushing assemblies (91) correspond to the penicillin bottles on the placing plate (4); the side of the freezing vacuum drying cavity (1) is provided with a cold air pipe (12), the outside of the freezing vacuum drying cavity (1) is provided with a freeze drying sealing door (14), the inside of the freeze drying sealing door (14) is provided with a special-shaped sealing rubber strip (15), the inside wall of the freeze drying sealing door (14) is provided with a wedge-shaped push block, the wedge-shaped push block corresponds to the body of the placing plate (4), the other side of the freeze drying sealing door (14) is rotatably connected with the outer wall of the freezing vacuum drying cavity (1), when the freeze drying sealing door (14) is closed, the wedge-shaped push block is in contact with the placing plate (4) and pushes the placing plate (4) to move to the side of the freezing vacuum drying cavity (1), the side of the placing plate (4) is provided with a needle tube (41), the needle tube (41) corresponds to the cold air pipe (12), the needle tube (41) extends into the cold air pipe (12); The bottom of the placing plate (4) is provided with a plurality of pulley seats (42), the pulley seats (42) are rotatably provided with rollers (43), at least two rollers (43) are arranged in each pulley seat (42), the pulley seats (42) are matched with the groove (3), the rollers (43) are slidably arranged in the groove (3), the quick mounting assembly (5) comprises a plurality of fixed bases (51), the fixed bases (51) are respectively arranged on the upper surface of the placing plate (4), the fixed bases (51) are provided with fine neck portions (52) at the upper side, and the fine neck portions (52) are used for fixing penicillin bottles. The linear drive crushing mechanism (9) further comprises a linear drive rod (92), an installation groove (21) is formed above the normal-temperature vacuum crushing cavity (2), the linear drive rod (92) is installed at the top of the installation groove (21), and the bottom of the linear drive rod (92) is provided with an installation carrier plate (93); the vibration crushing assembly (91) is installed at the bottom of the installation carrier plate (93). The vibration crushing assembly (91) comprises a vibration motor (911), the vibration motor (911) is located at the bottom of the installation carrier plate (93), a connecting rod (94) is arranged on the periphery of the bottom of the installation carrier plate (93), the bottom of the connecting rod (94) is provided with a crushing installation plate (95), a plurality of round holes (912) are formed in the crushing installation plate (95), a vibration rod (913) is arranged in the round hole (912), vibration springs (914) are arranged on the periphery of the vibration rod (913), and a vibration plate (915) is arranged above the vibration rod (913).

2. A vacuum freeze drying apparatus as claimed in claim 1, wherein: The cold gas pipe (12) is communicated with the refrigeration layer (11), and a spring air valve is arranged in the cold gas pipe (12), and the spring air valve is elastically biased towards the outlet of the cold gas pipe (12).

3. The vacuum freeze-drying equipment according to claim 1, characterized in that: The bottom of the vibration rod (913) is provided with a rubber layer (916), the outer side of the rubber layer (916) is provided with a rubber brush (917), the rubber brush (917) is not in contact with the Westlin bottle during the process of being put into the Westlin bottle, and the round hole (912) is a narrow-necked round hole.

4. The vacuum freeze-drying apparatus according to claim 1, characterized in that: The refrigeration assembly (7) comprises a throttling expansion valve (71), an evaporator (72), a compressor (73) and a condenser (74), one end of the throttling expansion valve (71) is connected with the evaporator (72), the other end of the evaporator (72) is connected with the compressor (73), the other end of the compressor (73) is connected with the condenser (74), the condenser (74) is communicated with the throttling expansion valve (71) through a connecting pipe, and a heat pipe is arranged in the refrigeration layer (11) and connected with the evaporator (72) and the compressor (73).

5. Use of the vacuum freeze-drying equipment according to any one of claims 1-4 in the preparation of a freeze-dried composition.

6. A method for preparing a stable lyophilized composition having an anti-wrinkle repair efficacy, characterized in that: The vacuum freeze-drying equipment according to any one of claims 1-4 is used; The method comprises the following steps: Step one, deionized water is added into a stirring kettle, sodium citrate and whey protein are sequentially added, and stirring is uniformly carried out at room temperature; end-lacking collagen, soluble collagen and mannitol are added, and stirring is uniformly carried out at room temperature, so that a blended collagen glue is obtained; Step two, the blended collagen glue is perfused into a Westlin bottle, freeze-drying is carried out in the vacuum freeze-drying equipment, and the product is obtained after being taken out of the box.

7. The method for preparing the stable freeze-dried composition with anti-wrinkle and repair effects according to claim 6, characterized in that: The stirring condition in the step one is 40r / min-50r / min, and the stirring time is 15-20min; the stirring condition in the third stirring is 40r / min-50r / min, and the stirring time is 30-50min; The mass ratio of the deionized water, the end-lacking collagen, the soluble collagen, the whey protein, the sodium citrate and the mannitol is (93.1-98.3):(0.1-0.3):(0.1-0.3):(0.4-1):(0.1-0.3):(1-5); wherein the sodium citrate is dihydrate sodium citrate.

8. The method for preparing the stable freeze-dried composition with anti-wrinkle and repair effects according to claim 6, characterized in that: The vacuum freeze drying in the step two specifically comprises the following steps: S1, pre-freezing: the flask containing the blended collagen glue is frozen at 0℃~-10℃ for 1-2h; then the temperature is decreased to-30℃~-50℃, and the freezing is performed for 2-3h; S2, primary drying: the primary drying is performed at 5℃-10℃ for 30-40h; S3, desorption drying: the desorption drying is performed at 30℃-35℃ for 2-3h. 9.A freeze-dried composition with anti-wrinkle repair effect and stability prepared by a preparation method of the freeze-dried composition with anti-wrinkle repair effect and stability according to any one of claims 7-8.

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