CN112930166A

CN112930166A - Water-soluble active substance particle and preparation method and application thereof

Info

Publication number: CN112930166A
Application number: CN201880098878.XA
Authority: CN
Inventors: 袁彦洁; 蒋伺江; 杜森垚; 罗敏
Original assignee: Chongqing Xiaowan Biotechnology Co ltd
Current assignee: Chongqing Xiaowan Biotechnology Co ltd
Priority date: 2018-11-05
Filing date: 2018-11-05
Publication date: 2021-06-08
Also published as: WO2020093192A1

Abstract

A water-soluble active substance particle which can be added into cosmetics and can be dissolved rapidly, and a preparation method and application thereof, wherein the water-soluble active substance particle comprises the following components in percentage by weight: 0.1 to 15 percent of adhesive, 1 to 80 percent of filling agent, 0.1 to 5 percent of disintegrating agent, 0 to 1 percent of proper amount of pigment and the balance of water-soluble active substance powder. The granule can be made from medicinal, edible or cosmetic raw materials.

Description

Water-soluble active substance particle and preparation method and application thereof

Technical Field

The invention relates to the technical field of cosmetics, in particular to a water-soluble active substance particle and a preparation method and application thereof.

Background

The water-soluble active substances have a plurality of effects of whitening, moisturizing, resisting aging, resisting allergy, resisting acne and the like on the skin. However, a considerable number of water-soluble actives are not stable in water for a long period of time, whereas most cosmetic products contain water, which results in the direct addition of these water-soluble actives in aqueous cosmetic products not being stable over shelf-life or use-time. The use of these actives is greatly limited. For example, vitamin C is an active that is very soluble in water but is very unstable in water. Vitamin C is a natural antioxidant, and has antioxidant and cancer preventing effects. Can inhibit the synthesis of melanin, reduce the generated melanin into colorless reduced melanin, promote the synthesis of collagen, has strong physiological functions in skin, such as whitening, anti-aging, acne removing, free radical scavenging, body degeneration delaying, skin aging preventing, damaged and dark skin repairing, pore shrinking and skin tightening effects. Therefore, vitamin C has long been used as a safe and effective whitening ingredient in skin care products. However, vitamin C powder has a large surface area and is easily hygroscopic and oxidizable, and is oxidized more rapidly in aqueous products, i.e., vitamin C cannot be stably stored for 2-3 years in the aqueous cosmetic formulation when it is directly added to the formulation. Therefore, the acidic and easily-oxidizable properties of vitamin C limit the application of vitamin C directly added into cosmetics.

At present, vitamin C derivatives such as vitamin C ethyl ether, vitamin C palmitate, vitamin C glucoside and vitamin C phosphate are mainly used in skin care products, and although the derivatives are decomposed by enzyme systems in the skin and reduced into vitamin C, the physiological activity of the derivatives is far lower than that of vitamin C. In addition, since the vitamin C powder has no fluidity, dust emission and strong moisture absorption, the vitamin C powder is difficult to be canned. Therefore, how to realize the stability and the fluidity of the vitamin C in the formula of the skin care product is a problem to be solved urgently, and the attention of researchers at home and abroad is also increased more and more.

Disclosure of Invention

Aiming at the defects of the prior art, the invention aims to provide a water-soluble active substance particle, which solves the problems that the water-soluble active substance is easy to oxidize and absorb moisture during storage, and the particle is easy to fly dust, fluffy and poor in fluidity during canning; such water-soluble active particles are commonly used in cosmetic products where the particles are packaged separately from the base, and when used, the particles are mixed into the cosmetic base and the particles rapidly disperse and dissolve, releasing the water-soluble active. Immediate fresh use avoids the problem of instability of direct active addition.

The invention provides a preparation method of the particle. The invention also provides the use of water-soluble active particles in cosmetics.

In order to solve the technical problems, the invention adopts the following technical scheme: a water-soluble active particle, wherein a water-soluble active powder is encapsulated in a fast dissolving shell to form a fine particle; wherein the mass percentage of the water-soluble active substance powder to the instant shell is 20-99: 80-1; the instant shell includes a binder, an instant filler, and a disintegrant. The content of the instant shell containing the granular water-soluble active matter can be up to 99%, and the instant filling agent can be added to reduce the content proportion of the water-soluble active matter according to application requirements.

Further, the instant shell further comprises a pigment, and the pigment accounts for 0-1% of the water-soluble active substance particles.

Further, the water-soluble active substance is a water-soluble active substance having moisturizing, whitening, anti-aging or anti-allergic effects in cosmetics. Wherein the water solubility of the active is defined as a 1% by mass aqueous solution of the active, which is a homogeneous clear aqueous solution or a homogeneous dispersion at 25 ℃.

The instant shell comprises a binder, an instant filler, a disintegrating agent, a pigment and the like, which are all raw materials easily dissolved in water, and ensure that no residue is left after the granules are dissolved.

The bulk density of the water-soluble active substance particles is 0.4 g/mL-1.2 g/mL, the range of the common bulk density is 0.6 g/mL-1.0 g/mL, and the water-soluble active substance particles with high bulk density have good fluidity and are easy to pack in a small volume.

The particle size of the water-soluble active substance particles is 100-2000 n microns, so that on one hand, the specific surface area of the water-soluble active substance powder is reduced, and the surface area of the water-soluble active substance powder contacting air is reduced; on the other hand, a quick-dissolving shell layer is formed on the surface of the water-soluble active substance, so that the oxidation speed is delayed.

Further, the binder is sucrose, various cellulose derivatives, or a high molecular material which is easily soluble in water and comprises one or more of carboxymethyl cellulose, hydroxypropyl methyl cellulose, hydroxyethyl cellulose, methyl cellulose, crospovidone, polyvinyl alcohol, sodium alginate, xanthan gum and agar. The fast dissolving filler is an edible dissolvable material comprising glucose, mannitol, sorbitol, fructose or lactose. The disintegrating agent is a high swelling material in water, such as sodium carboxymethyl cellulose, sodium carboxymethyl starch, acrylic starch or agar.

The high polymer material comprises one or more water-soluble high polymer materials selected from carboxymethyl cellulose, hydroxypropyl methyl cellulose, hydroxyethyl cellulose, methyl cellulose, polyvinylpolypyrrolidone, polyvinyl alcohol, sodium alginate, xanthan gum, carrageenan or agar.

Wherein, the sucrose can be dissolved into syrup as a binder in the components, and the water-soluble active substance powder can also be diluted by sucrose powder as a filler to reach the required water-soluble active substance content. The sucrose solution has viscosity and can be used as a bonding agent in the process, the dissolution speed of the sucrose is high, and the dissolution speed of the water-soluble active substance is not influenced. If other water-soluble polymer materials are used, a proper amount of water-soluble fillers such as sucrose, glucose, mannitol, sorbitol, lactose, etc. can be added according to the content requirement. When water-soluble polymer materials are used as adhesives, the dissolution time of water-soluble active substance particles is prolonged, and the purpose of high-speed dissolution cannot be achieved, so that when the water-soluble polymer materials are granulated, proper disintegrating agents, usually some water-soluble colloids with high expansibility, are required to be added, so that the particles are quickly disintegrated into powder, and the water-soluble active substances are quickly dissolved in water. The disintegrating agent comprises carboxymethyl cellulose, carboxymethyl starch, modified starch or agar and the like, which have adhesive force and high expansibility, and the prepared granules can be quickly expanded when meeting water, so that the granules can be instantly disintegrated into powder, and the colloid can be used as the adhesive and also is the disintegrating agent. When other water-soluble colloids with relatively low swelling ratio are used as the binder, such as povidone, polyvinyl alcohol, sodium alginate, xanthan gum, carrageenan, etc., the above disintegrating colloids can be appropriately added to accelerate the dissolution rate. In addition, in the granulating process, the surface of the water-soluble active substance is covered with a layer of film shell by the adhesive liquid, and the water-soluble active substance powder is bonded into firm particles, so that the contact area of the water-soluble active substance and oxygen in the air is greatly reduced, the oxidation speed is reduced, and the water-soluble active substance is easier to store.

The invention also provides a preparation method of the instant water-soluble active substance granule, which comprises the following steps:

1) dosing as a component of said water soluble active particles;

2) dissolving a binder in water to obtain a binder solution;

3) the water soluble active powder is granulated in a tangential spray rotating fluidized bed.

The working principle of the tangential spraying rotary fluidized bed is as follows: the bottom of the raw material container of the fluidized bed is a rotating disc rotating at high speed, a tiny (0.5-5 mm) gap is arranged between the rotating disc and the side wall of the container, and hot air flow rises from the gap at high speed. The water-soluble active substance is driven by the rotating disc to rotate at a high speed in the container, the water-soluble active substance is thrown to the outer wall of the container by centrifugal force, the hot air flow rising in the gap supports the material, and the water-soluble active substance descends to flow to the center of the rotating disc by gravity. Therefore, the water-soluble active substance does a twisted rope-shaped high-speed rotating motion of suspension rolling along the edge of the rotating disc under the action of three external forces, the nozzle is immersed in the rotating water-soluble active substance, and the sprayed adhesive is completely coated on the water-soluble active substance particles flowing at high speed, so that the loss of the sprayed liquid is completely avoided. The hot air flowing upward penetrates the flowing layer of water-soluble active substance particles, so that the adhesive is dried in time. The particles prepared by the method are easy to adhere due to the extrusion of centrifugal force, compact and high in stacking density; meanwhile, as the adhesive is sprayed on the water-soluble active substance powder rotating at high speed, the uniformity and consistency of the shell are ensured. In addition, due to the rounding friction effect of the circular motion, the particles have no sharp acute angle and are round, so that the excellent flowability of the particles is ensured.

Further, generally, since the swelling speed of the water-soluble polymer binder is slow, the particles prepared by adding more than 5% should be relatively hard, which affects the dissolution speed; the dosage of the water-soluble polymer adhesive is too small, less than 0.1%, and the prepared particles are loose, easy to break and irregular. Therefore, when the binder is sucrose which is easily dissolved in water, the percentage of sucrose is 8.0-15.0%. When the adhesive is a high polymer material which is easy to dissolve in water, the concentration is 0.1-5.0%.

Further, the linear speed of the rotating speed of the fluidized bed is 100-2000 m/min, so that the particles are rolled firmly by the high-speed centrifugal force of the turntable of the fluidized bed, are not loosened and fall powder, and the high bulk density of the particles is ensured. When large particles (with the particle size of 1000-2000um) are needed, the rotating linear speed of the rotation of the fluidized bed is controlled to be 100-1000 m/min. When small particles (with the particle size less than 1000um) are needed, the rotating linear speed of the fluidized bed is controlled to be 1000-2000 m/min.

The water-soluble active substance is a water-soluble active substance which has the effects of moisturizing, whitening, resisting aging, resisting allergy and the like in cosmetics, and is unstable in water. Further, the water-soluble active is a water-soluble vitamin such as vitamin C, B-group vitamins (B1, B2, B5, B6, B12) niacin, folic acid, pantothenic acid and lipid derivatives of these vitamins. Among them, vitamin C is a typical active substance having very high water solubility, having whitening effect, but very unstable in water.

The water solubility of the active is defined as a 1% by mass aqueous solution of the active, which is a homogeneous clear aqueous solution at 25 ℃. Further, such water-soluble active particles are commonly used in cosmetics where the particles are packaged separately from the base, and when used, the particles are mixed into the cosmetic base, and the particles rapidly disperse and dissolve, releasing the water-soluble active. The immediate fresh use avoids the unstable problem of direct addition of active substances.

The application of the water-soluble active substance particles in cosmetics separates the water-soluble active substance particles from a base material through packaging of skin care products. When the water-soluble active substance is used, the water-soluble active substance particles are mixed into a skin care product base material, the water-soluble active substance particles can be quickly dissolved in the base material within 10-30 seconds at most within 1 minute, and fresh water-soluble active substances without oxidative deterioration can be used immediately.

Compared with the prior art, the invention has the following beneficial effects:

1. the invention is innovative in that the water-soluble active substance powder is wrapped in the instant shell to form micro-particles, thereby solving the problems that the water-soluble active substance is easy to oxidize and absorb moisture during storage, and the particles are easy to raise dust, fluffy and poor in fluidity during canning; the instant shell comprises a filling agent, a bonding agent, a disintegrating agent, a pigment and the like, which are all raw materials easily dissolved in water, and ensure that no residue is left after the granules are dissolved. Wherein the mass percentage of the water-soluble active substance powder to the instant shell is 20-99: 80 to 1.

2. The water-soluble active substance particles have high bulk density and good fluidity, are dust-free, avoid discomfort caused by inhalation of high-concentration water-soluble active substances in operation of workers, are small in volume and easy to pot, can be quickly dissolved in a water-containing cosmetic formula, usually within 10-30 seconds, at most 1min, and reduce the specific surface area of water-soluble active substance powder, so that the surface area of the water-soluble active substance powder contacting with air is reduced, and then a film shell is formed on the surface of the water-soluble active substance, so that the oxidation speed is delayed, the water-soluble active substance powder keeps higher physiological activity, and the defects of poor stability and no fluidity of the water-soluble active substance powder are overcome.

3. The preparation method is simple and quick, the raw materials are simple, the cost is low, regular particles with uniform sizes can be prepared by controlling the speed of the rotary table, the size of air flow and the concentration spraying speed of the adhesive, and the quality control is convenient.

4. The water-soluble active particles of the present invention are convenient to use. Since most cosmetics are aqueous, the invention is suitable for any water-soluble active, particularly for the use of water-soluble actives that are unstable in water in cosmetics. Especially has good application prospect in cosmetics which separately pack active substances and base materials. The water soluble active particles can be immediately mixed into the base material and quickly dissolved for immediate use. Avoiding the situation where water-unstable water-soluble actives are added to aqueous cosmetics that are unstable over long shelf-life.

In use, the water-soluble active substance particles are mixed with the skin care product base material only, so that the water-soluble active substance particles are quickly dissolved in the skin care product base material to form uniform liquid, the particles are quickly dissolved and completely dissolved, and the test shows that the complete dissolution speed of the particles prepared by the method is up to 60 seconds when the 10-percent water solution, namely 10 g of particles is dissolved to 90 g of pure water at room temperature by stirring, the dissolution time is usually 10-30 seconds, and the dissolution speed is basically consistent with that of water-soluble active substance powder. Has the characteristic of convenient use, enables the water-soluble active powder to retain higher physiological activity, and has good application prospect.

Drawings

Figure 1 is a schematic of the structure of a water-soluble active particle.

FIG. 2 is a schematic view of the process of the present invention.

In fig. 1, 1 is a water-soluble active material and a fast-dissolving filler, and 2 is a mixture of a binder and a disintegrant.

In FIG. 2, 3 is a raw material container (fluidized bed), 4 is a rotary turntable, and 5 is a spray-generating upward hot air.

Detailed Description

The present invention will be described in further detail with reference to examples.

Water-soluble active substance particle formula (dry weight parts)

Second, preparation method of instant vitamin C granule/instant vitamin B granule

Example 1

1) The components are proportioned according to the proportion in the example 1;

2) dissolving sodium carboxymethyl cellulose as adhesive in water to obtain 3% adhesive solution;

3) putting vitamin C powder into a tangential spraying rotary fluidized bed, rotating at 1500 rpm/min (the radius of a rotary table is about 0.2 m, the linear speed is 1884 m/min), starting a spraying device, spraying the adhesive solution prepared in the step 2) into the vitamin C powder rotating at high speed from the tangential direction, enabling the vitamin C powder to be adhered by the adhesive until the obtained particles reach the required size, stopping spraying, and drying the particles to obtain the instant vitamin C particles.

Example 2

1) The components are mixed according to the proportion in the embodiment 2;

2) dissolving a sucrose binder in water to obtain a 30% binder solution;

3) and (2) putting the vitamin C powder into a tangential spraying rotary fluidized bed, rotating at 600 rpm/min (the radius of a rotating disc is about 0.2 m, the linear speed is 750 m/min), starting a spraying device, spraying the binder solution prepared in the step (2) into the vitamin C powder rotating at high speed from the tangential direction to enable the vitamin C powder to be adhered by the binder, stopping spraying until the obtained particles reach the required size, and drying the particles to obtain the instant vitamin C particles.

Example 3

1) The components are proportioned according to the embodiment 3;

2) dissolving sodium carboxymethylcellulose adhesive in water to obtain 3% adhesive solution;

3) mixing vitamin C powder and sucrose powder in proportion, putting into a tangential spraying rotary fluidized bed, setting the speed of 750 rpm/min (the radius of a rotary table is about 0.2 m, the linear speed is 940 m/min for rotation, then starting a spraying device, spraying the adhesive solution prepared in the step 2) into the vitamin C powder rotating at high speed from the tangential direction, enabling the vitamin C powder to be adhered by the adhesive, stopping spraying until the obtained particles reach the required size, and drying the particles to obtain the instant vitamin C particles.

Example 4

1) The components are proportioned according to the proportion in the example 4;

2) dissolving hydroxyethyl cellulose binder in water to obtain 3% binder solution;

3) mixing vitamin B1, B5 and B6 powders, mannitol powder and sodium carboxymethyl starch. Proportionally mixing, putting into a tangential spraying rotary fluidized bed, setting the speed of the rotary table to be 1500 rpm/min (the radius of the rotary table is about 0.2 m, the linear speed is about 1900 m/min for rotation, then starting a spraying device, spraying the adhesive solution prepared in the step 2) into the mixed powder rotating at high speed from the tangential direction, enabling the vitamin B powder to be adhered by the adhesive, stopping spraying until the obtained particles reach the required size, and drying the particles to obtain the instant vitamin B particles.

Example 5

1) The components are mixed according to the proportion of 5;

2) dissolving povidone adhesive in water to obtain 5% adhesive solution;

3) mixing vitamin B5 powder, xylitol and mannitol powder in proportion, putting into a tangential spraying rotary fluidized bed, setting the speed of the rotary table to be about 0.2 m/min (the linear speed is 1100 m/min, rotating, then starting a spraying device, spraying the adhesive solution prepared in the step 2) into vitamin B5 powder rotating at high speed from the tangential direction, enabling the mixed powder to be adhered by the adhesive, stopping spraying until the obtained particles reach the required size, and drying the particles to obtain the instant vitamin B5 particles.

From the above table, the water-soluble active substance particles prepared by the invention have high bulk density, good fluidity and small volume, are easy to pot, can be quickly dissolved in a water-containing cosmetic formula, usually within 10-30 seconds, keep higher physiological activity of the vitamin particles, and ensure that the vitamin particles can be stably stored in a skin care product for 2-3 years according to the shelf life.

Application of instant vitamin C granules

3.1, the instant vitamin C/B granules prepared in the examples 1 to 5 are used in a facial mask.

When packaging, the facial mask bag is divided into 3 small bags (3 chambers), and the 3 chambers are respectively filled with film cloth, essence and VC/VB particles. When in use, the VC/VB particles are poured into the essence liquid, are quickly dissolved, and then the essence liquid containing VC/VB is added into the membrane cloth, is soaked in the membrane cloth, and is immediately applied to the face.

3.2 use of instant vitamin C particles in cosmetics.

1) The instant vitamin C granules prepared in the examples 1-3/6-8 are used in essence

The package contains two cavities at two room vacuum package, and in the big cavity of water-based essence packing's theme, the VC granule dress is in inside less cavity, unscrews dress VC granule cavity switch when using for the first time, and the VC granule mixes in the essence, shakes and dissolves the VC granule, then uses the essence that has mixed VC

2) The instant vitamin C particles prepared in the examples 1-6 are used in whitening cream

The VC particles are separately packaged by aluminum foil light-resistant plastic bags, poured into the whitening cream base material before use, stirred, dissolved and mixed uniformly. And then used.

3.3 use of the instant vitamin B mixture granules prepared in examples 4-5 in an anti-aging sleep mask

The packaging bottle of the facial mask comprises two parts, wherein the inside of the bottle is filled with emulsion, and the inside of the cover is provided with a cavity (filled with mixed vitamin B instant particles, the particles are poured into the emulsion for uniform mixing when the facial mask is used for the first time, and after the particles are added, the product needs to be used within 30 days, so that the activity of active substances is ensured.

Fourthly, the principle and method of the water-soluble active substance granules based on the embodiments 1 to 8, wherein the water-soluble active substance adopts vitamin B group (B1, B2, B5, B6, B12) nicotinic acid, folic acid, pantothenic acid or lipid derivatives of these vitamins, all of which can achieve the purpose of the present invention, and are not exhaustive herein.

The above description is only exemplary of the present invention and should not be taken as limiting, and any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims

A water-soluble active particle, wherein a water-soluble active powder is encapsulated in a fast dissolving shell to form a fine particle; wherein the mass percentage of the water-soluble active substance powder to the instant shell is 20-99: 80-1; the instant shell includes a binder, an instant filler, and a disintegrant.
The water-soluble active particle of claim 1, wherein the instant shell further comprises a pigment in an amount of 0-1% by weight of the water-soluble active particle.
The water-soluble active substance particle according to claim 1 or 2, wherein the water-soluble active substance is a water-soluble active substance having moisturizing, whitening, anti-aging, or anti-allergic effects in cosmetics.
The water-soluble active substance particles according to claim 1 or 2, wherein the binder is sucrose or a high molecular material which is easily soluble in water.
The water-soluble active substance granulate according to claim 1 or 2, wherein the fast dissolving filler is an edible dissolvable material comprising sucrose, glucose, mannitol, sorbitol, fructose or lactose powder.
The water-fast soluble active substance granule according to claim 1 or 2, wherein the disintegrant is a water-highly swellable material comprising sodium carboxymethyl cellulose, sodium carboxymethyl starch, acrylic starch or agar.
The water-soluble active substance particles according to claim 1 or 2, wherein the bulk density of the water-soluble active substance particles is 0.4 to 1.2 g/ml.
The water-soluble active substance particles according to claim 1 or 2, wherein the particle size of the water-soluble active substance particles is 100 to 2000 μm.
The water-soluble active substance granules according to claim 1 or 2, characterized in that the weight percentage composition thereof is: 0.1-15% of adhesive, 1-80% of instant filler, 0.1-5% of disintegrating agent and the balance of water-soluble active matter.
The water-soluble active substance particle according to claim 3, wherein the water-soluble active substance is a water-soluble active substance which has moisturizing, whitening, anti-aging, anti-allergy, etc. effects in cosmetics but is unstable in water.
The water-soluble active substance granulate of claim 3, wherein the water-soluble active substance is a water-soluble vitamin comprising vitamin C, the B-group of vitamins (B1, B2, B5, B6 or B12) niacin, folic acid, pantothenic acid and lipid derivatives of these vitamins.
The water-soluble active substance particle according to claim 4, wherein the polymer material comprises one or more water-soluble polymer materials selected from the group consisting of carboxymethyl cellulose, hydroxypropyl methyl cellulose, hydroxyethyl cellulose, methyl cellulose, cross-linked poly-vitamin one, polyvinyl alcohol, sodium alginate, xanthan gum, carrageenan and agar.
The water-soluble active substance particles according to claim 7, wherein the bulk density of the water-soluble active substance particles is 0.6 to 1.0 g/ml.
A method of preparing water-soluble active particles, comprising the steps of:

1) compounding the components according to any one of claims 1 to 2;

2) dissolving a binder and a disintegrant in water to obtain a binder solution;

3) putting the mixture of the water-soluble active substance powder and the filler powder into a tangential spraying rotary fluidized bed and rotating at a high speed, then starting a spraying device, spraying the adhesive solution prepared in the step 2) into the high-speed rotating mixed powder of the water-soluble active substance powder and the instant filler from the tangential direction, enabling the mixed powder to be adhered by the adhesive to form granules, and drying to obtain the water-soluble active substance granules.
The method of preparing water-soluble active particles of claim 14, wherein the concentration of the binder solution is 0.1-15.0%.
The method for preparing water-soluble active substance particles according to claim 14, wherein the rotational linear velocity of the fluidized bed is 100-2000 m/min.
The method of claim 14, wherein the binder and sucrose, which is readily soluble in water, are present in the granule in an amount of 8.0 to 15.0%.
The method of claim 14, wherein the binder is a polymeric material that is readily soluble in water, and the percentage of the binder in the granules is 0.1-5.0%.
The method as claimed in claim 16, wherein the rotational linear velocity of the fluidized bed is medium or low 100-1000 m/min, and the particle size is 1000-2000 um.
The method as claimed in claim 16, wherein the rotational linear velocity of the fluidized bed is higher than 1000-2000 m/min, and the particle size of the obtained particles is less than 1000 um.