CN112294702A - Macromolecular carrier composition and preparation method and application thereof - Google Patents

Macromolecular carrier composition and preparation method and application thereof Download PDF

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CN112294702A
CN112294702A CN201910703852.XA CN201910703852A CN112294702A CN 112294702 A CN112294702 A CN 112294702A CN 201910703852 A CN201910703852 A CN 201910703852A CN 112294702 A CN112294702 A CN 112294702A
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sodium
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CN112294702B (en
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孟宏
刘盼玉
曲召辉
刘有停
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Taihe Kangmei Beijing Research Institute of Traditional Chinese Medicine 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
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9706Algae
    • A61K8/9717Rhodophycota or Rhodophyta [red algae], e.g. Porphyra
    • 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

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Abstract

The invention provides a macromolecular carrier composition, which comprises the following components: sodium polyglutamate, Chondrus crispus and sodium hyaluronate. The carrier composition obtained by the preparation process has strong loading capacity, good skin feel and long-acting slow-release effect, can greatly improve the skin care effect and the utilization rate of active ingredients through the slow-release effect, and can be widely applied to cosmetics.

Description

Macromolecular carrier composition and preparation method and application thereof
Technical Field
The invention relates to a macromolecular carrier composition, a preparation method and application thereof.
Background
Controlled release of active substances such as functional factors in pharmaceuticals, cosmetics and food has been a major research point in the field of materials, and long-lasting release of active substances has many advantages compared to systems without sustained release function. The sustained release can not only improve the effectiveness and safety of the activity of the active substance, but also obviously reduce the side effect and improve the utilization rate of the active substance, thereby reducing the use cost. The material used as the slow release carrier is an important component of a slow release system and is an important factor influencing the slow release effect. Natural materials have received much attention from researchers at home and abroad because of their advantages such as good biocompatibility, safety, reliability, wide sources, and many varieties.
The long-term effect of the active ingredients is an important concern in the cosmetic market, because some active ingredients added in the cosmetics are expensive, and some active ingredients need a long time to permeate into the surface layer of the skin to exert the effect. In order to delay the release and loss of effective components, the existing methods mostly add macromolecular substances such as sodium hyaluronate or cellulose and the like into skin care products to form a film on the surface of skin, so that the effect of prolonging the products is achieved. However, most of these methods only slow down the loss of active ingredients on the skin and have the effect of prolonging the efficacy of the product for a short time; moreover, the macromolecular substance only containing a single component has a single spatial structure, can not load and release various micromolecular substances like a carrier composite system, and simultaneously, the release of the effective component is difficult to control, so that the ideal skin care component slow-release effect is difficult to achieve.
By mixing various macromolecular substances, a crossed space network structure can be formed in an aqueous solution, and by the structure, various components can be loaded in the network space to form a carrier composite system and can be released under certain conditions. The carrier composite system can load various small molecular components to achieve effective release of active small molecular components. The carrier compounding technology is a better method for solving the problem of slow release of active ingredients. However, the viscosity of various macromolecular components is high, the fluidity is poor, the components are difficult to be uniformly mixed in the compounding process, the product system is unstable, and the macromolecular carrier compounding technology still has great technical challenges. On the other hand, part of the carrier composite system adopts various chemical synthesis raw materials, and potential hazards exist in safety and biocompatibility.
Safe, effective and stable carrier compositions for application to the surface of human skin are technical problems that need to be addressed by researchers in the field.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide a macromolecular carrier composition with a long-acting slow-release effect, which has higher loading capacity, can provide a long-acting slow-release effect of a loaded component, is safe, efficient and good in skin feel, and can be widely applied to the field of cosmetics.
In order to achieve the purpose, the invention idea is as follows: firstly, macromolecular substances with long-chain linear structures with moldability, ionicity or strong water absorption are screened, and the components, the dosage and the preparation process are optimized, so that the macromolecular substances are interacted and crossed to form a composition with a stable space net structure, and other small molecular substances can be loaded due to the anionic property of the composition, thereby playing a role in slow release.
Based on this, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a macromolecular composition comprising the following ingredients: polyglutamic acid sodium, Chondrus crispus, and sodium hyaluronate.
The Chondrus crispus is a linear hydrophilic high molecular polymer, has a repeated alpha- (1 → 4) -D-galactopyranose-beta- (1 → 3) -D-galactopyranose (or 3, 6-inner ether-D-galactopyranose) disaccharide unit skeleton structure, wherein a galactose residue has a half-ester sulfate group, has strong anionic activity and is a typical anionic polysaccharide. Due to its strong anionic properties, it was screened as the main component of the carrier structure. The polyglutamic acid is formed by condensing a D-type glutamic acid monomer and an L-type glutamic acid monomer, is a linear molecule, and has strong water absorption because the structure of the polyglutamic acid contains a large amount of free carboxyl. Meanwhile, the structure of the antibacterial agent contains carboxyl, so that the antibacterial agent also has certain anionic property. The two structures can form a space net structure after being carried and interacted with the sodium hyaluronate, and a large number of loose porous structures are contained in the space net structure. The porous network structure can increase the loading capacity of the loading component and has the effect of long-acting slow release.
According to an embodiment of the present invention, the sodium polyglutamate is 0.01% to 2.0% by weight, for example, 0.01%, 0.02%, 0.04%, 0.05%, 0.1%, 0.15%, 0.18%, 0.2%, 0.21%, 0.25%, 0.27%, 0.3%, 0.34%, 0.35%, 0.36%, 0.38%, 0.39%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, 1.3%, 1.4%, 1.5%, 1.6%, 1.7%, 1.8%, 1.9%, or 2.0% by weight, based on the total weight of the composition, and points therebetween are limited to the brevity and conciseness of the list. Preferably, the sodium polyglutamate is 0.2-2.0wt% based on the total weight of the composition.
According to an embodiment of the present invention, the amount of the carrageen is 0.01% to 10.0% by weight, for example, 0.01%, 0.03%, 0.05%, 0.1%, 0.2%, 0.3%, 0.35%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, 2.0%, 3.0%, 3.3%, 3.5%, 4.5%, 5.5%, 6.0%, 6.6%, 7.8%, 8.9%, 9.0%, or 10.0% by weight, based on the total weight of the composition, and the values therebetween are not limited to space and conciseness. Preferably, the Chondrus crispus is present in an amount of 1.0 to 10.0wt%, based on the total weight of the composition.
According to an embodiment of the present invention, the sodium hyaluronate is 0.01% to 2.0% by weight, for example, 0.01%, 0.03%, 0.05%, 0.1%, 0.13%, 0.18%, 0.22%, 0.25%, 0.27%, 0.33%, 0.34%, 0.35%, 0.36%, 0.38%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, 1.3%, 1.4%, 1.5%, 1.6%, 1.7%, 1.8%, or 2.0% by weight, based on the total weight of the composition, and point values therebetween are not limited to space and simplicity, and are not limited thereto. Preferably, the sodium hyaluronate is 0.1 to 2.0wt% based on the total weight of the composition.
According to some preferred embodiments of the invention the sodium polyglutamate has a molecular weight of 50 Da or more, for example in the range of 50-300 Da, such as 50 Da, 80 Da, 100 Da, 150 Da, 250 Da, etc.
According to some preferred embodiments of the invention the Chondrus crispus has a molecular weight ≧ 80 ten thousand Da, such as in the range of 80-600 ten thousand Da, such as 100 ten thousand Da, 150 ten thousand Da, 200 ten thousand Da, 500 ten thousand Da, etc.
According to some preferred embodiments of the invention, the sodium hyaluronate has a molecular weight of 5 ten thousand Da or more, for example, it may be in the range of 5 to 250 ten thousand Da, such as 50 ten thousand Da, 100 ten thousand Da, 150 ten thousand Da, 190 ten thousand Da, etc.
According to a more preferred embodiment of the invention, the molecular weight of the sodium polyglutamate is 100-150 kilodaltons.
According to a more preferred embodiment of the present invention, the molecular weight of the Chondrus crispus is 150-250 ten thousand Da.
According to a more preferred embodiment of the invention, the molecular weight of the sodium hyaluronate is 100-150 ten thousand Da.
According to some embodiments of the invention, the carrier composition further comprises water and a preservative. Preservatives conventional in the art may be used in the present invention without particular limitation.
According to some embodiments of the invention, the preservative is present in an amount of ≦ 1wt% based on the total weight of the carrier composition, with the balance being water.
According to some preferred embodiments of the invention, the preservative is phenoxyethanol/ethylhexyl glycerol, and/or caprylyl glycol.
According to some preferred embodiments of the invention, the preservative is caprylyl glycol.
According to some preferred embodiments of the present invention, the caprylyl glycol is 0.1wt% based on the total weight of the carrier composition.
According to an embodiment of the invention, water is the balance.
In a second aspect, the present invention provides a method for preparing the macromolecular carrier composition, which comprises the steps of 1) mixing the polyglutamic acid sodium, the carrageen crispa, the sodium hyaluronate and the water, stirring and heating to 70-90 ℃, and completely dissolving.
According to the invention, the temperature of the stirring heating is 70-90 ℃, and may be, for example, 70 ℃, 71 ℃, 72 ℃, 73 ℃, 75 ℃, 76 ℃, 77 ℃, 78 ℃, 79 ℃, 80 ℃, 81 ℃, 82 ℃, 83 ℃, 84 ℃, 85 ℃, 87 ℃, 88 ℃, 89 ℃, 90 ℃ and specific values between the above temperature values.
Preferably, the heating temperature is 80-85 ℃.
Preferably, the preparation method further comprises a step 2): adding a preservative into the mixture obtained in the step 1), stirring, cooling to room temperature, and filtering to obtain the carrier composition. Preservatives conventional in the art may be used in the present invention without particular limitation.
Preferably, the stirring is mechanical stirring, and the stirring speed is 200-400 r/min.
According to some embodiments of the invention, the preservative is present in an amount of ≦ 1wt% based on the total weight of the carrier composition.
According to some preferred embodiments of the invention, the preservative is phenoxyethanol/ethylhexyl glycerol, and/or caprylyl glycol.
Further preferably, the preservative is caprylyl glycol.
According to some embodiments of the invention, the preservative is 0.3wt% based on the total weight of the carrier composition.
The normal temperature of the invention means that the temperature is 25 +/-5 ℃.
The raw materials and the proportion of the composition are obtained by repeated screening, the obtained composition has a synergistic enhanced loading capacity and a good slow release effect, and the raw materials are safe and are tried on skin, so that the composition has a wide application prospect.
In a third aspect, the present invention provides a composition according to the first aspect of the present invention and a macromolecular carrier composition or carrier composition prepared by a method according to the second aspect of the present invention for use in cosmetics. The composition disclosed by the invention is applied to the field of cosmetics, and the skin care effect of the active ingredients can be greatly improved through a slow release effect.
The invention has the advantages of
Compared with the prior art, the composition has the following beneficial effects:
(1) overcomes the technical defects of the prior product, and avoids the defect that the prior single macromolecular carrier does not have a slow release function;
(2) through repeated screening and testing, the composition has proper fluidity in water environment, good film forming property and good skin feel, and can be widely used in the field of skin care products;
(3) the carrier structure of the invention contains various groups, can adsorb various small molecular substances, and has strong loading capacity, good slow release effect and good application prospect.
Drawings
FIG. 1 is a picture of a freeze-dried sample of the macromolecular composition in a vacuum freeze-dryer according to example 1;
FIG. 2 is a 100-fold scanning electron microscope photograph of the macromolecular composition according to example 1;
FIG. 3 is a graph showing the water absorption effect of the macromolecular composition according to example 1;
fig. 4 is the sensory evaluation results of the test samples according to example 1; sensory evaluation results of the test samples according to example 20; sensory evaluation results of the test sample according to example 21;
FIG. 5 is a result of the change of the permeation amount per unit area of L-serine according to the experimental group of example 1 with time; results of the change over time in the permeation amount per unit area of L-serine of the control group 1 according to example 21; results of the change over time in the permeation amount per unit area of L-serine of the control group 2 according to example 20;
FIG. 6 shows the results of the change of the permeability per unit area of betaine in the experimental group according to example 1 with time; results of change over time in the permeability per unit area of betaine according to control 1 of example 21; the results of the change in the permeability per unit area of betaine according to control 2 of example 20 with time;
FIG. 7 shows the results of the permeability per unit area of the test group PCA-Na according to example 1 as a function of time; results of change over time in the permeability per unit area of PCA-Na of control 1 according to example 21; the results of the change in the permeability per unit area of PCA-Na according to control 2 of example 20 with time.
The specific implementation mode is as follows:
to further illustrate the technical means and effects of the present invention, the present invention will be further described with reference to the following specific embodiments. It is to be understood that the specific embodiments described herein are merely illustrative of the invention and are not limiting of the invention. The examples, which are not specifically shown for the specific methods, are all routine in the art or according to the product specifications. The reagents or apparatus used are conventional products commercially available from normal sources, not indicated by the manufacturer.
Tables 1 and 2 below show the raw materials used, the equipment used and the suppliers of the invention, respectively.
Table 1 raw materials and list of suppliers thereof
Figure 493496DEST_PATH_IMAGE002
TABLE 2 Instrument information List
Figure 332008DEST_PATH_IMAGE004
Example 1: preparation of macromolecular carrier composition with long-acting slow-release function
1) Weighing 0.2 part by weight of poly-sodium glutamate (molecular weight of 100 ten thousand Da), 1 part by weight of Chondrus crispus (molecular weight of 200 ten thousand Da) and 0.1 part by weight of sodium hyaluronate (molecular weight of 100 ten thousand Da), adding into 98.7 parts by weight of water, stirring at the rotating speed of 300r/min by using a stirrer, and simultaneously heating to 80 ℃ until the sodium polyglutamate, the Chondrus crispus and the sodium hyaluronate are completely dissolved;
2) after complete dissolution, adding preservative octyl glycol into the system 1) according to the proportion of 0.3 percent of the weight fraction of the composition, and uniformly stirring at the rotating speed of a stirrer of 300 r/min; cooling to normal temperature, filtering and discharging.
Example 2: preparation of macromolecular carrier composition with long-acting slow-release function
1) Weighing 0.2 part by weight of poly-sodium glutamate (molecular weight of 100 ten thousand Da), 1 part by weight of Chondrus crispus (molecular weight of 200 ten thousand Da) and 0.1 part by weight of sodium hyaluronate (molecular weight of 100 ten thousand Da), adding into 98.7 parts by weight of water, stirring at the rotating speed of 300r/min by using a stirrer, and simultaneously heating to 90 ℃ until the solution is completely dissolved;
2) after complete dissolution, adding preservative octyl glycol into the system 1) according to the proportion of 0.3 percent of the weight fraction of the composition, and uniformly stirring at the rotating speed of a stirrer of 300 r/min; cooling to normal temperature, filtering and discharging.
Example 3: preparation of macromolecular carrier composition with long-acting slow-release function
1) Weighing 0.2 part by weight of poly-sodium glutamate (molecular weight of 100 ten thousand Da), 1 part by weight of Chondrus crispus (molecular weight of 200 ten thousand Da) and 0.1 part by weight of sodium hyaluronate (molecular weight of 100 ten thousand Da), adding into 98.7 parts by weight of water, stirring at the rotating speed of 300r/min by using a stirrer, and simultaneously heating to 70 ℃ until the sodium polyglutamate, the Chondrus crispus and the sodium hyaluronate are completely dissolved;
2) after complete dissolution, adding preservative octyl glycol into the system 1) according to the proportion of 0.3 percent of the weight fraction of the composition, and uniformly stirring at the rotating speed of a stirrer of 300 r/min; cooling to normal temperature, filtering and discharging.
Example 4: preparation of macromolecular carrier composition with long-acting slow-release function
1) Weighing 0.2 part by weight of poly-sodium glutamate (with the molecular weight of 50 ten thousand Da), 1 part by weight of Chondrus crispus (with the molecular weight of 200 ten thousand Da) and 0.1 part by weight of sodium hyaluronate (with the molecular weight of 100 ten thousand Da), adding the materials into 98.7 parts by weight of water, stirring at the rotating speed of a stirrer of 300r/min, and simultaneously heating to 80 ℃ until the materials are completely dissolved;
2) after complete dissolution, adding preservative octyl glycol into the system 1) according to the proportion of 0.3 percent of the weight fraction of the composition, and uniformly stirring at the rotating speed of a stirrer of 300 r/min; cooling to normal temperature, filtering and discharging.
Example 5: preparation of macromolecular carrier composition with long-acting slow-release function
1) Weighing 0.2 part by weight of poly-sodium glutamate (with the molecular weight of 250 ten thousand Da), 1 part by weight of Chondrus crispus (with the molecular weight of 200 ten thousand Da) and 0.1 part by weight of sodium hyaluronate (with the molecular weight of 100 ten thousand Da), adding the materials into 98.7 parts by weight of water, stirring at the rotating speed of 300r/min by using a stirrer, and simultaneously heating to 80 ℃ until the materials are completely dissolved;
2) after complete dissolution, adding preservative octyl glycol into the system 1) according to the proportion of 0.3 percent of the weight fraction of the composition, and uniformly stirring at the rotating speed of a stirrer of 300 r/min; cooling to normal temperature, filtering and discharging.
Example 6: preparation of macromolecular carrier composition with long-acting slow-release function
1) Weighing 0.2 part by weight of poly-sodium glutamate (molecular weight 100 ten thousand Da), 1 part by weight of Chondrus crispus (molecular weight 100 ten thousand Da) and 0.1 part by weight of sodium hyaluronate (molecular weight 100 ten thousand Da), adding into 98.7 parts by weight of water, stirring at the rotating speed of 300r/min by using a stirrer, and simultaneously heating to 80 ℃ until the sodium polyglutamate, the Chondrus crispus and the sodium hyaluronate are completely dissolved;
2) after complete dissolution, adding preservative octyl glycol into the system 1) according to the proportion of 0.3 percent of the weight fraction of the composition, and uniformly stirring at the rotating speed of a stirrer of 300 r/min; cooling to normal temperature, filtering and discharging.
Example 7: preparation of macromolecular carrier composition with long-acting slow-release function
1) Weighing 0.2 part by weight of poly-sodium glutamate (molecular weight of 100 ten thousand Da), 1 part by weight of Chondrus crispus (molecular weight of 500 ten thousand Da) and 0.1 part by weight of sodium hyaluronate (molecular weight of 100 ten thousand Da), adding into 98.7 parts by weight of water, stirring at the rotating speed of 300r/min by using a stirrer, and simultaneously heating to 80 ℃ until the sodium polyglutamate, the Chondrus crispus and the sodium hyaluronate are completely dissolved;
2) after complete dissolution, adding preservative octyl glycol into the system 1) according to the proportion of 0.3 percent of the weight fraction of the composition, and uniformly stirring at the rotating speed of a stirrer of 300 r/min; cooling to normal temperature, filtering and discharging.
Example 8: preparation of macromolecular carrier composition with long-acting slow-release function
1) Weighing 0.2 part by weight of poly-sodium glutamate (molecular weight of 100 ten thousand Da), 1 part by weight of Chondrus crispus (molecular weight of 80 ten thousand Da) and 0.1 part by weight of sodium hyaluronate (molecular weight of 100 ten thousand Da), adding into 98.7 parts by weight of water, stirring at the rotating speed of 300r/min by using a stirrer, and simultaneously heating to 80 ℃ until the sodium polyglutamate, the Chondrus crispus and the sodium hyaluronate are completely dissolved;
2) after complete dissolution, adding preservative octyl glycol into the system 1) according to the proportion of 0.3 percent of the weight fraction of the composition, and uniformly stirring at the rotating speed of a stirrer of 300 r/min; cooling to normal temperature, filtering and discharging.
Example 9: preparation of macromolecular carrier composition with long-acting slow-release function
1) Weighing 0.2 part by weight of poly-sodium glutamate (molecular weight 100 ten thousand Da), 1 part by weight of Chondrus crispus (molecular weight 200 ten thousand Da) and 0.1 part by weight of sodium hyaluronate (molecular weight 5 ten thousand Da), adding into 98.7 parts by weight of water, stirring at the rotating speed of 300r/min by a stirrer, and simultaneously heating to 80 ℃ until the solution is completely dissolved;
2) after complete dissolution, adding preservative octyl glycol into the system 1) according to the proportion of 0.3 percent of the weight fraction of the composition, and uniformly stirring at the rotating speed of a stirrer of 300 r/min; cooling to normal temperature, filtering and discharging.
Example 10: preparation of macromolecular carrier composition with long-acting slow-release function
1) Weighing 0.2 part by weight of poly-sodium glutamate (molecular weight 100 ten thousand Da), 1 part by weight of Chondrus crispus (molecular weight 200 ten thousand Da) and 0.1 part by weight of sodium hyaluronate (molecular weight 190 ten thousand Da), adding into 98.7 parts by weight of water, stirring at the rotating speed of 300r/min by a stirrer, and simultaneously heating to 80 ℃ until the solution is completely dissolved;
2) after complete dissolution, adding preservative octyl glycol into the system 1) according to the proportion of 0.3 percent of the weight fraction of the composition, and uniformly stirring at the rotating speed of a stirrer of 300 r/min; cooling to normal temperature, filtering and discharging.
Example 11: preparation of macromolecular carrier composition with long-acting slow-release function
1) Weighing 1 part by weight of poly-sodium glutamate (molecular weight 100 ten thousand Da), 5 parts by weight of Chondrus crispus (molecular weight 200 ten thousand Da) and 1 part by weight of sodium hyaluronate (molecular weight 100 ten thousand Da) and adding the materials into 93 parts by weight of water, stirring at the rotating speed of a stirrer of 300r/min and simultaneously heating to 85 ℃ until the materials are completely dissolved;
2) after complete dissolution, adding preservative octyl glycol into the system 1) according to the proportion of 0.3 percent of the weight fraction of the composition, and uniformly stirring at the rotating speed of a stirrer of 300 r/min; cooling to normal temperature, filtering and discharging.
Example 12: preparation of macromolecular carrier composition with long-acting slow-release function
1) Weighing 2 parts by weight of sodium polyglutamate (molecular weight of 100 ten thousand Da), 10 parts by weight of Chondrus crispus (molecular weight of 200 ten thousand Da) and 2 parts by weight of sodium hyaluronate (molecular weight of 100 ten thousand Da), adding into 86 parts by weight of water, stirring at the rotating speed of a stirrer of 300r/min, and simultaneously heating to 85 ℃ until the sodium polyglutamate, the Chondrus crispus and the sodium hyaluronate are completely dissolved;
2) after the complete dissolution, adding the preservative octyl glycol into the system 1) according to the proportion of 0.3 percent of the weight fraction of the composition, uniformly stirring at the rotating speed of 300r/min by a stirrer, cooling to normal temperature, filtering and discharging.
Example 13: preparation of macromolecular carrier composition with long-acting slow-release function
1) Weighing 0.5 part by weight of poly-sodium glutamate (molecular weight 100 ten thousand Da), 5 parts by weight of Chondrus crispus (molecular weight 200 ten thousand Da) and 0.5 part by weight of sodium hyaluronate (molecular weight 100 ten thousand Da), adding into 94 parts by weight of water, stirring at the rotating speed of a stirrer of 300r/min, and simultaneously heating to 80 ℃ until the solution is completely dissolved;
2) after the complete dissolution, adding the preservative octyl glycol into the system 1) according to the proportion of 0.3 percent of the weight fraction of the composition, uniformly stirring at the rotating speed of 300r/min by a stirrer, cooling to normal temperature, filtering and discharging.
Example 14: preparation of macromolecular carrier composition with long-acting slow-release function
1) Weighing 0.2 part by weight of poly-sodium glutamate (with the molecular weight of 150 ten thousand Da), 1 part by weight of Chondrus crispus (with the molecular weight of 150 ten thousand Da) and 0.1 part by weight of sodium hyaluronate (with the molecular weight of 150 ten thousand Da), adding the materials into 98.7 parts by weight of water, stirring at the rotating speed of a stirrer of 300r/min, and simultaneously heating to 80 ℃ until the materials are completely dissolved;
2) after the complete dissolution, adding the preservative octyl glycol into the system 1) according to the proportion of 0.3 percent of the weight fraction of the composition, uniformly stirring at the rotating speed of 300r/min by a stirrer, cooling to normal temperature, filtering and discharging.
Example 15: preparation of macromolecular carrier composition with long-acting slow-release function
1) Weighing 1 part by weight of poly-sodium glutamate (with the molecular weight of 50 ten thousand Da), 10 parts by weight of Chondrus crispus (with the molecular weight of 80 ten thousand Da) and 2 parts by weight of sodium hyaluronate (with the molecular weight of 50 ten thousand Da), adding the materials into 87 parts by weight of water, stirring at the rotating speed of a stirrer of 300r/min, and simultaneously heating to 85 ℃ until the materials are completely dissolved;
2) adding preservative phenoxyethanol/ethylhexyl glycerol into the system 1) according to the proportion of 0.8 percent of the weight fraction of the composition after complete dissolution, uniformly stirring at the rotating speed of 300r/min of a stirrer, cooling to normal temperature, filtering and discharging.
Example 16: preparation of macromolecular carrier composition with long-acting slow-release function
1) Weighing 1 part by weight of poly-sodium glutamate (molecular weight 100 ten thousand Da), 10 parts by weight of Chondrus crispus (molecular weight 150 ten thousand Da) and 1 part by weight of sodium hyaluronate (molecular weight 150 ten thousand Da) and adding the materials into 88 parts by weight of water, stirring at the rotating speed of a stirrer of 300r/min, and simultaneously heating to 85 ℃ until the materials are completely dissolved;
2) adding preservative phenoxyethanol/ethylhexyl glycerol into the system 1) according to the proportion of 0.8 percent of the weight fraction of the composition after complete dissolution, uniformly stirring at the rotating speed of 300r/min of a stirrer, cooling to normal temperature, filtering and discharging.
Example 17: preparation of macromolecular carrier composition with long-acting slow-release function
1) Weighing 2 parts by weight of poly-sodium glutamate (with the molecular weight of 50 ten thousand Da), 5 parts by weight of Chondrus crispus (with the molecular weight of 80 ten thousand Da) and 2 parts by weight of sodium hyaluronate (with the molecular weight of 50 ten thousand Da), adding the materials into 91 parts by weight of water, stirring at the rotating speed of a stirrer of 300r/min, and simultaneously heating to 85 ℃ until the materials are completely dissolved;
2) adding preservative phenoxyethanol/ethylhexyl glycerol into the system 1) according to the proportion of 0.8 percent of the weight fraction of the composition after complete dissolution, uniformly stirring at the rotating speed of 300r/min of a stirrer, cooling to normal temperature, filtering and discharging.
Example 18: preparation of macromolecular carrier composition with long-acting slow-release function
1) Weighing 1 part by weight of poly-sodium glutamate (molecular weight 100 ten thousand Da), 4 parts by weight of Chondrus crispus (molecular weight 200 ten thousand Da) and 1 part by weight of sodium hyaluronate (molecular weight 100 ten thousand Da), adding into 94 parts by weight of water, stirring at the rotating speed of a stirrer of 300r/min, and simultaneously heating to 80 ℃ until the solution is completely dissolved;
2) adding preservative phenoxyethanol/ethylhexyl glycerol into the system 1) according to the proportion of 0.8 percent of the weight fraction of the composition after complete dissolution, uniformly stirring at the rotating speed of 300r/min of a stirrer, cooling to normal temperature, filtering and discharging.
Example 19: preparation of macromolecular carrier composition with long-acting slow-release function
1) Weighing 0.2 part by weight of poly-sodium glutamate (molecular weight of 80 ten thousand Da), 6 parts by weight of Chondrus crispus (molecular weight of 200 ten thousand Da) and 0.2 part by weight of sodium hyaluronate (molecular weight of 100 ten thousand Da), adding into 93.6 parts by weight of water, stirring at the rotating speed of 300r/min by using a stirrer, and simultaneously heating to 80 ℃ until the sodium glutamate, the Chondrus crispus and the sodium hyaluronate are completely dissolved;
2) adding preservative phenoxyethanol/ethylhexyl glycerol into the system 1) according to the proportion of 0.8 percent of the weight fraction of the composition after complete dissolution, uniformly stirring at the rotating speed of 300r/min of a stirrer, cooling to normal temperature, filtering and discharging.
Example 20:
1) weighing 5 parts by weight of poly-sodium glutamate (molecular weight 100 ten thousand Da), 15 parts by weight of Chondrus crispus (molecular weight 200 ten thousand Da) and 5 parts by weight of sodium hyaluronate (molecular weight 100 ten thousand Da), adding the materials into 80 parts by weight of water, stirring at the rotating speed of a stirrer of 300r/min, and simultaneously heating to 80 ℃ until the materials are completely dissolved;
2) after the complete dissolution, adding the preservative octyl glycol into the system 1) according to the proportion of 0.3 percent of the weight fraction of the composition, uniformly stirring at the rotating speed of 300r/min by a stirrer, cooling to normal temperature, filtering and discharging.
Example 21:
1) weighing 0.2 part by weight of poly-sodium glutamate (with the molecular weight of 30 ten thousand Da), 1 part by weight of Chondrus crispus (with the molecular weight of 50 ten thousand Da) and 0.1 part by weight of sodium hyaluronate (with the molecular weight of 3 ten thousand Da), adding the materials into 98.7 parts by weight of water, stirring at the rotating speed of 300r/min by using a stirrer, and simultaneously heating to 80 ℃ until the materials are completely dissolved;
2) after the complete dissolution, adding the preservative octyl glycol into the system 1) according to the proportion of 0.3 percent of the weight fraction of the composition, uniformly stirring at the rotating speed of 300r/min by a stirrer, cooling to normal temperature, filtering and discharging.
Example 22:
1) weighing 0.2 part by weight of poly-sodium glutamate (molecular weight 100 ten thousand Da), 1 part by weight of Chondrus crispus (molecular weight 200 ten thousand Da) and 0.1 part by weight of sodium hyaluronate (molecular weight 100 ten thousand Da) and adding the materials into 98.7 parts by weight of water, and uniformly stirring at the rotating speed of a stirrer of 300 r/min;
2) adding preservative octyl glycol according to the proportion of 0.3 percent of the weight fraction of the composition in the system 1), uniformly stirring at the rotating speed of a stirrer of 300r/min, filtering and discharging.
Comparative example 1:
1) weighing 0.2 part by weight of sodium polyglutamate (molecular weight of 100 ten thousand Da) and 1 part by weight of Chondrus crispus (molecular weight of 200 ten thousand Da), adding into 98.8 parts by weight of water, stirring at the rotating speed of 300r/min by a stirrer, and simultaneously heating to 80 ℃ until the sodium polyglutamate and the Chondrus crispus are completely dissolved;
2) after the complete dissolution, adding the preservative octyl glycol into the system 1) according to the proportion of 0.3 percent of the weight fraction of the composition, uniformly stirring at the rotating speed of 300r/min by a stirrer, cooling to normal temperature, filtering and discharging.
Comparative example 2:
1) weighing 0.2 part by weight of sodium polyglutamate (with a molecular weight of 100 ten thousand Da) and 0.1 part by weight of sodium hyaluronate (with a molecular weight of 100 ten thousand Da), adding the sodium polyglutamate and the sodium hyaluronate into 99.7 parts by weight of water, stirring at the rotating speed of a stirrer of 300r/min, and simultaneously heating to 80 ℃ until the sodium polyglutamate and the sodium hyaluronate are completely dissolved;
2) after the complete dissolution, adding the preservative octyl glycol into the system 1) according to the proportion of 0.3 percent of the weight fraction of the composition, uniformly stirring at the rotating speed of 300r/min by a stirrer, cooling to normal temperature, filtering and discharging.
Comparative example 3:
1) weighing 1 part by weight of Chondrus crispus (molecular weight 200 ten thousand Da) and 0.1 part by weight of sodium hyaluronate (molecular weight 100 ten thousand Da) into 98.9 parts by weight of water, stirring at the rotating speed of 300r/min by a stirrer, and simultaneously heating to 80 ℃ until the Chondrus crispus and the sodium hyaluronate are completely dissolved;
2) after the complete dissolution, adding the preservative octyl glycol into the system 1) according to the proportion of 0.3 percent of the weight fraction of the composition, uniformly stirring at the rotating speed of 300r/min by a stirrer, cooling to normal temperature, filtering and discharging.
First, the preparation process is optimized
The researchers of the invention study the preparation process of the composition, and comparatively study the influence of different temperatures (normal temperature, 40 ℃, 50 ℃, 60 ℃, 70 ℃, 80 ℃, 90 ℃ and 95 ℃) on the performance of the composition.
The experimental method comprises the following steps:
1) weighing 0.2 part by weight of poly-sodium glutamate (molecular weight 100 ten thousand Da), 1 part by weight of Chondrus crispus (molecular weight 200 ten thousand Da) and 0.1 part by weight of sodium hyaluronate (molecular weight 100 ten thousand Da), adding into 98.7 parts by weight of water, stirring at a stirrer rotation speed of 300r/min, and stirring the system at a set temperature (normal temperature, 40 ℃, 50 ℃, 60 ℃, 70 ℃, 80 ℃, 90 ℃ and 95 ℃);
2) adding preservative octyl glycol according to the proportion of 0.1 percent of the weight fraction of the composition in the system 1), and uniformly stirring at the rotating speed of a stirrer of 300 r/min; cooling to normal temperature (if the temperature is higher than normal temperature), filtering and discharging.
The product state and stability of the compositions prepared at different temperatures were observed and the results were as follows:
Figure DEST_PATH_IMAGE006A
from the above experimental results, it can be seen that when the heating temperature is lower than 60 ℃, the obtained composition has poor stability, uniformity and the like, and when the heating temperature is higher than 70 ℃, the stability and the product state are good, and the stability, uniformity, fluidity, moldability and the like of the composition have a great influence on the performance of the carrier, and the heating temperature is preferably higher than 70 ℃, and is preferably 70-90 ℃ in the preparation process of the carrier composition of the present invention.
Second, efficacy experiment test
(1) Freeze-drying experiment of macromolecular carrier composition
The experimental method comprises the following steps: the sample prepared in step (1) of example 1 was lyophilized in a vacuum freeze dryer, and the sample was lyophilized as shown in fig. 1. The sample was observed under a scanning electron microscope, and the state of 100 times is shown in FIG. 2. As can be seen from fig. 1, the support phase of example 1 can form a loose porous sponge-like structure. As can be seen from FIG. 2, the macromolecular samples of the carrier in example 1 can form a honeycomb-shaped space network structure, and the structure has a large specific surface area and can be loaded with a large amount of small molecular component substances.
(2) Water absorption test
The experimental method comprises the following steps: the sample prepared in step (1) of example 1 was lyophilized in a vacuum freeze dryer. The sample state is shown in FIG. 3 a;
after the sample was taken out, it was left at room temperature (relative humidity 50%) and observed for water absorption, and the state of the sample after 300min is shown in FIG. 3 b.
Comparing fig. 3a and fig. 3b, it can be seen that after freeze-drying, the sample is placed at normal temperature (relative humidity 50%) for 300min, and the sample absorbs a great amount of water from the solid network structure and gradually becomes transparent liquid, which intuitively proves that the carrier sample of the present invention has strong water absorption effect.
(3) Product State and stability Observation
The test samples in Table 3 were observed for their respective states and stabilities, and the results are shown in the following table:
TABLE 3
Figure DEST_PATH_IMAGE008
From the observation results, it was found that the compositions obtained in examples 1, 5, 7, 10 and 15 had appropriate viscosity, good transparency, fine texture, appropriate fluidity and good film-forming property. Example 20 the composition of the sample had a higher amount of raw materials added, resulting in a composition with a higher viscosity, a lower flowability, a poor composition state, but a good stability. Example 21 had a high flow, a suitable viscosity and a good transparency.
Example 22 the sample after filtration and discharge, after a short period of standing, partially different transparent suspended components appeared, the sample had poor homogeneity, and after a long period of standing, the transparent particulate matter accumulated at the bottom of the liquid, and the stability was poor, indicating that the composition obtained by simply combining macromolecular components did not meet the carrier performance standard and had no load potential. The inventors repeated the same experiment with other examples and obtained samples of the composition with suitable viscosity, good clarity, gummy texture, suitable flowability and good moldability, which were not shown one by one without space limitations.
Meanwhile, the comparative examples 1, 2 and 3 are different from the composition of the invention, and the observation results of the product state and stability show that the film forming property is poor, the fluidity is too strong, and long-time coverage on the skin surface is difficult to realize, so that the slow-release carrier has no performance required by a strong slow-release carrier, and the obtained composition has no potential of slow release and long-acting moisturizing effect.
(4) Sensory evaluation test
The sensory evaluation experiment strictly carries out volunteer screening, group training, test result investigation and the like according to the flow of sensory evaluation.
Sensory evaluation samples: 15wt% example composition + balance water.
Figure DEST_PATH_IMAGE009
Preparation of a test sample:
the compositions of example 1, example 20 and example 21 were respectively added to water and stirred uniformly to obtain test samples.
The inventors carried out sensory evaluation tests on the samples of example 1, example 20 and example 21: the tested product is smeared on the skin surface of a tested subject, the tested subject scores the products from moistening feeling, soft feeling, moistening feeling after absorption, film forming property and smooth feeling, wherein, the score of 5 is best, the score of 0 is worst, and the use sense of the tested product is evaluated, and the result is shown in figure 4:
the results of the investigation show that the samples of example 1 are superior to the products of examples 20 and 21 in both the feeling of use and the skin feel. The product of example 1 has good film forming property and strong moistening feeling, and is more suitable for being applied to slow-release skin care products.
The smaller the molecular weight of the raw material of the composition, the more difficult it is to form a stable spatial network structure, which affects the sustained release effect and skin feel thereof. The product prepared with the larger molecular weight has better lubrication and skin feel experience, and the film forming property of the product with the larger molecular weight is better, so that the moisturizing effect of the product is more favorable. According to repeated experimental screening, researchers of the invention determine that the molecular weight of the raw materials of the composition is as follows: the polyglutamic acid sodium is more than or equal to 50 ten thousand Da, the Phragmites communis is more than or equal to 80 ten thousand Da and the hyaluronic acid sodium is more than or equal to 5 ten thousand Da. Within the molecular weight range, a stable spatial structure can be formed and good use experience is provided, and meanwhile, the carrier structure has good performance of containing small molecular substances and good slow release performance.
Meanwhile, the addition amount and the proportion of the raw materials of the composition have great influence on the product state and the skin feel of the composition, and the excessive or insufficient addition amount can influence the product fluidity and the skin feel, so that the state and the skin feel of the composition obtained within the addition amount and the proportion range of the raw materials are optimal.
(5) Amino acid small molecule substance diffusion cell release experiment
Through a diffusion cell experiment, the characteristics that the amino acid micromolecule substances exist on the reticular structure due to the reticular structure and interaction of the product, and the effect of slowly releasing the amino acid micromolecule components is achieved. The experiment uses the small molecule amino acid L-serine to measure the slow release.
The experimental method comprises the following steps:
the soaked and wiped-dry artificial membrane was sandwiched between diffusion cells (5 mL diffusion cells), 50% ethanol was filled in both the supply chamber and the receiving chamber, and the sample addition port and the sampling port were sealed with sealing films and equilibrated overnight. The liquid (50% ethanol) in the supply chamber was removed and the residual liquid in the supply chamber was wiped dry with paper and then the supply chamber was filled with supply liquid (samples, 2 in parallel per sample). A rotor is added into the diffusion cell, and the sample adding port and the sampling port are sealed by sealing films. 0.8mL of the receiving chamber was sampled at 2, 6, 9, 24, 48 and 54 hours, and the receiving chamber was filled with a blank receiving solution preheated to 37 ℃ and sampled with a long-headed sampling needle. Filtering with 0.45 μm microporous membrane, sampling the filtrate, and detecting content by HPLC. The content of the humectant in the sample, the control group 1 and the control group 2 at different time points through the artificial membrane is respectively measured, and the content of the L-serine is measured by an HPLC method.
The preparation method of the experimental group comprises the following steps: (example 1 test with serine added to the composition)
1) Weighing 0.2g of poly-sodium glutamate (molecular weight of 100 ten thousand Da), 1g of Chondrus crispus (molecular weight of 200 ten thousand Da), 0.1g of sodium hyaluronate (molecular weight of 100 ten thousand Da) and 0.1g of L-serine, adding into 98.6 g of water, stirring at the rotating speed of 300r/min by using a stirrer, and simultaneously heating to 80 ℃ until the sodium glutamate, the sodium hyaluronate and the L-serine are completely dissolved; 2) after the dissolution is completed, adding preservative octyl glycol according to the mass fraction of 0.3 percent into the system, uniformly stirring at the rotating speed of 300r/min by a stirrer, cooling to normal temperature, filtering and discharging.
Control 1 preparation method: (example 21 test with serine added to the composition)
1) Weighing 0.2g of poly-sodium glutamate (with the molecular weight of 30 ten thousand Da), 1g of Chondrus crispus (with the molecular weight of 50 ten thousand Da), 0.1g of sodium hyaluronate (with the molecular weight of 3 ten thousand Da) and 0.1g of L-serine, adding the materials into 98.6 g of water, stirring at the rotating speed of 300r/min by using a stirrer, and simultaneously heating to 80 ℃ until the materials are completely dissolved; 2) after the dissolution is completed, adding preservative octyl glycol according to the mass fraction of 0.3 percent into the system, uniformly stirring at the rotating speed of 300r/min by a stirrer, cooling to normal temperature, filtering and discharging.
Control 2 preparation method: (example 20 test with serine added to the composition)
1) Weighing 5g of poly-sodium glutamate (molecular weight 100 ten thousand Da), 15g of Chondrus crispus (molecular weight 200 ten thousand Da), 5g of sodium hyaluronate (molecular weight 100 ten thousand Da) and 0.1g of L-serine, adding the materials into 74.9 g of water, stirring at the rotating speed of a stirrer of 300r/min, and simultaneously heating to 80 ℃ until the materials are completely dissolved; 2) after the dissolution is completed, adding preservative octyl glycol according to the mass fraction of 0.3 percent into the system, uniformly stirring at the rotating speed of 300r/min by a stirrer, cooling to normal temperature, filtering and discharging.
The results of the diffusion cell experiments are shown in figure 5.
FIG. 5 shows that the composition sample prepared in the experimental group 1 of the present invention has a significant effect of slowly releasing L-serine compared to the control groups 1 and 2. The result shows that the composition maintains relatively stable slow release efficiency for a long time and has good slow release effect, and the performance has important significance for slow release of the functional components, maintenance and promotion of the efficacy and efficient utilization of the functional substances.
(6) Quaternary ammonium salt small molecular substance diffusion cell release experiment
The experimental method is the same as (5).
The sample preparation method is as follows:
the preparation method of the experimental group comprises the following steps: 1) weighing 0.2g of poly-sodium glutamate (molecular weight of 100 ten thousand Da), 1g of Chondrus crispus (molecular weight of 200 ten thousand Da), 0.1g of sodium hyaluronate (molecular weight of 100 ten thousand Da) and 5g of betaine into 93.7g of water, stirring at the rotating speed of 300r/min by using a stirrer, and simultaneously heating to 80 ℃ until the sodium glutamate, the sodium hyaluronate and the betaine are completely dissolved; 2) after the dissolution is completed, adding preservative octyl glycol according to the mass fraction of 0.3 percent into the system, uniformly stirring at the rotating speed of 300r/min by a stirrer, cooling to normal temperature, filtering and discharging.
Control 1 preparation method: (example 21 test with betaine added to the composition)
1) Weighing 0.2g of poly-sodium glutamate (with the molecular weight of 30 ten thousand Da), 1g of Chondrus crispus (with the molecular weight of 50 ten thousand Da), 0.1g of sodium hyaluronate (with the molecular weight of 3 ten thousand Da) and 5g of betaine into 93.7g of water, stirring at the rotating speed of 300r/min by using a stirrer, and simultaneously heating to 80 ℃ until the sodium glutamate, the sodium hyaluronate and the betaine are completely dissolved; 2) after the dissolution is completed, adding the preservative octyl glycol according to the mass fraction of 0.3% in the system, uniformly stirring at the rotating speed of 300r/min of a stirrer, uniformly stirring at the rotating speed of 300r/min of the stirrer, cooling to normal temperature, filtering and discharging.
Control 2 preparation method: (example 20 test with betaine added to the composition)
1) Weighing 5g of poly-sodium glutamate (molecular weight 100 ten thousand Da), 15g of Chondrus crispus (molecular weight 200 ten thousand Da), 5g of sodium hyaluronate (molecular weight 100 ten thousand Da) and 5g of betaine into 70g of water, stirring at the rotating speed of 300r/min by a stirrer, and simultaneously heating to 80 ℃ until the sodium hyaluronate is completely dissolved; 2) after the dissolution is completed, adding preservative octyl glycol according to the mass fraction of 0.3 percent into the system, uniformly stirring at the rotating speed of 300r/min by a stirrer, cooling to normal temperature, filtering and discharging.
The experimental results are shown in FIG. 6.
As can be seen from FIG. 6, the sample of the experimental group 1 has stronger loading capacity and obvious slow release effect compared with the control group to the quaternary ammonium salt micromolecular substance betaine, and maintains more stable slow release efficiency for a longer time, and the carrier composition of the invention has the slow release effect to the quaternary ammonium salt micromolecular substance. The performance has important significance for the slow release of the functional components, the maintenance and the promotion of the functions and the high-efficiency utilization of the functional substances.
(7) Release experiment of sodium pyrrolidone carboxylate micromolecular substance diffusion cell
The experimental method is the same as (5).
The sample preparation method is as follows:
the preparation method of the experimental group comprises the following steps: (example 1 test with the composition having sodium pyrrolidone carboxylate added thereto)
1) 0.2g of sodium polyglutamate (with the molecular weight of 100 ten thousand Da), 1g of carrageen crispatus (with the molecular weight of 200 ten thousand Da), 0.1g of sodium hyaluronate (with the molecular weight of 100 ten thousand Da) and 5g of sodium pyrrolidone carboxylate (PCA-Na) are weighed and added into 93.7g of water, and the stirrer is stirred at the rotating speed of 300r/min and is heated to 80 ℃ at the same time until the sodium polyglutamate, the sodium hyaluronate and the sodium pyrrolidone carboxylate are completely dissolved; 2) after the dissolution is completed, adding preservative octyl glycol according to the mass fraction of 0.3 percent into the system, uniformly stirring at the rotating speed of 300r/min by a stirrer, cooling to normal temperature, filtering and discharging.
Control 1 preparation method: (example 21 test with addition of sodium pyrrolidone carboxylate to the composition)
1) 0.2g of sodium polyglutamate (with the molecular weight of 30 ten thousand Da), 1g of carrageen crispatus (with the molecular weight of 50 ten thousand Da), 0.1g of sodium hyaluronate (with the molecular weight of 3 ten thousand Da) and 5g of sodium pyrrolidone carboxylate (PCA-Na) are weighed and added into 93.7g of water, and the stirrer is stirred at the rotating speed of 300r/min and is heated to 80 ℃ at the same time until the sodium polyglutamate, the sodium hyaluronate and the sodium pyrrolidone carboxylate are completely dissolved; 2) after the dissolution is completed, adding preservative octyl glycol according to the mass fraction of 0.3 percent into the system, uniformly stirring at the rotating speed of 300r/min by a stirrer, cooling to normal temperature, filtering and discharging.
Control 2 preparation method: (example 20 test with addition of sodium pyrrolidone carboxylate to the composition)
1) Weighing 5g of poly-sodium glutamate (molecular weight 100 ten thousand Da), 15g of Chondrus crispus (molecular weight 200 ten thousand Da), 5g of sodium hyaluronate (molecular weight 100 ten thousand Da) and 5g of sodium pyrrolidone carboxylate (PCA-Na) into 70g of water, stirring at the rotating speed of 300r/min by a stirrer, and simultaneously heating to 80 ℃ until the solution is completely dissolved; 2) after the dissolution is completed, adding preservative octyl glycol according to the mass fraction of 0.3 percent into the system, uniformly stirring at the rotating speed of 300r/min by a stirrer, cooling to normal temperature, filtering and discharging.
The results of the experiment are shown in FIG. 7.
The experimental results are as follows: as can be seen from FIG. 7, the composition sample of the present invention has a more significant sodium pyrrolidone carboxylate (PCA-Na) loading capacity and transdermal absorption sustained-release effect than the control group, and maintains a more stable sustained-release efficiency for a longer time, which indicates that the product of the present invention has a sustained-release effect on amino acid derived substances.
The experiments prove that the carrier composition has proper fluidity, good film forming property and stability, and good skin feel, and can be widely used in the field of skin care products; the carrier structure of the invention contains various groups, can form a stable carrier structure, can adsorb various micromolecular substances, and has strong loading capacity, good slow release effect and good application prospect.
It should be noted that the above-mentioned embodiments are only for explaining the present invention, and do not constitute any limitation to the present invention. The present invention has been described with reference to exemplary embodiments, but the words which have been used herein are words of description and illustration, rather than words of limitation. The invention can be modified, as prescribed, within the scope of the claims and without departing from the scope and spirit of the invention. Although the invention has been described herein with reference to particular means, materials and embodiments, the invention is not intended to be limited to the particulars disclosed herein, but rather extends to all other methods and applications having the same functionality.

Claims (10)

1. A composition comprising sodium polyglutamate, carrageen crispa and sodium hyaluronate.
2. A macromolecular carrier composition characterized in that said composition has a spatial network structure formed from sodium polyglutamate, carrageen crispa and sodium hyaluronate.
3. The composition of claim 1 or 2, wherein the sodium polyglutamate is 0.01% to 2wt%, and/or the Chondrus crispus is 0.01% to 10wt%, and/or the sodium hyaluronate is 0.01% to 2wt%, based on the total weight of the composition.
4. The composition of claim 3, wherein the molecular weight of the sodium polyglutamate is greater than or equal to 50 ten thousand Da, and/or the molecular weight of the Chondrus crispus is greater than or equal to 80 ten thousand Da, and/or the molecular weight of the sodium hyaluronate is greater than or equal to 5 ten thousand Da; preferably, the molecular weight of the sodium polyglutamate is more than or equal to 100 ten thousand Da, and/or the molecular weight of the Chondrus crispus is more than or equal to 200 ten thousand Da, and/or the molecular weight of the sodium hyaluronate is more than or equal to 100 ten thousand Da.
5. A carrier composition comprising a composition according to any one of claims 1 to 4 and water and/or a preservative.
6. The carrier composition of claim 5 wherein the preservative is present in an amount of 1wt% or less based on the total weight of the composition.
7. A method of preparing a macromolecular carrier composition comprising step 1): mixing sodium polyglutamate, Chondrus crispus, sodium hyaluronate and water at 70-90 deg.C.
8. A method of preparing a carrier composition comprising step 1): mixing sodium polyglutamate, Chondrus crispus, sodium hyaluronate and water at 70-90 deg.C; and optionally, step 2) adding a preservative to the mixture prepared in step 1) for mixing.
9. The method of claim 8, wherein the preservative is used in an amount of 1wt% or less in step 2), based on the total weight of the carrier composition.
10. Use of a composition according to any one of claims 1 to 6 or of a macromolecular carrier composition obtained by the preparation process according to claim 7 or of a carrier composition obtained by the preparation process according to claim 8 or 9 in cosmetics.
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CN106667842A (en) * 2017-01-22 2017-05-17 泉州师范学院 Face repair liquid rich in ginseng-seaweed essence and preparation method of face repair liquid

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