Camellia soft beads containing red camellia extract and preparation method thereof

Abstract

The present invention relates to a camellia soft bead containing red camellia extract and a preparation method thereof, comprising an external camellia soft bead essence and an internal camellia essence oil composition; the camellia soft bead essence comprises red camellia extract, a thickener, a polyol, a pH regulator, and a preservative, and the camellia essence oil comprises an oil-soluble red camellia extract and an emollient. The present invention prepares camellia soft beads containing red camellia extract by microfluidic technology, which have a transparent texture, uniform oil condensation beads, are spherical, and can pass stability tests, and can be applied to water-based essences, bringing consumers a different skin care experience.

Description

Technical Field

[0001] The invention belongs to the technical field of cosmetics, and particularly relates to camellia soft beads containing red camellia extract and a preparation method thereof. Background Art

[0002] The concept of using oil to care for the skin is gradually gaining popularity, and it is becoming more and more popular among consumers. Essential oils are generally pure oil-based systems. Although they have good skin care effects, they are prone to greasy or stuffy problems in summer or for oily skin. In order to meet the needs of more consumers, essential oil skin care products that replenish water and oil have emerged. They have both the freshness of water and the moisture of oil, and are also one of the development directions of refreshing essential oils.

[0003] The most critical component of the suspended oil essence is the soft beads, which contain the outer phase essence liquid and the inner phase essence oil composition. Through microfluidics technology, the inner phase essence oil composition can quickly form transparent oil beads of a specific particle size and evenly disperse them in the essence liquid, eventually forming nearly spherical particles with uniform particle size and crystal clearness. At present, this technology is not mature, and there are certain difficulties in the preparation of oil beads. The stability of the formed oil beads is poor, and the particle size of the beads is prone to change, the beads break or become foggy and white, which has certain limitations.

[0004] In view of the prior art, the technical problems to be solved by the present invention are specifically: to screen out an external essence liquid containing red camellia extract with a transparent appearance and certain rheological properties; to screen out an internal essence oil composition containing red camellia extract with a suitable solidification point and density ratio; to control the mass ratio of the two, and to use microfluidic technology to directly encapsulate the active essence oil therein, to obtain a suitable oil-liquid mass ratio, and the oil beads have uniform size and transparent appearance, have good stability and safety, and are used in camellia suspension oil essence with repair and anti-aging effects. Summary of the invention

[0005] The purpose of the present invention is to provide a camellia soft bead containing red camellia extract and a preparation method thereof in view of the problems existing in the prior art.

[0006] The purpose of the present invention can be achieved by the following scheme:

[0007] The present invention provides a camellia soft bead containing red camellia extract, which comprises 30-80% of an external phase and 20-70% of an internal phase by mass percentage, wherein the external phase is camellia soft bead essence liquid and the internal phase is camellia soft bead essence oil;

[0008] The camellia soft beads essence comprises the following components in percentage by weight:

[0009]

[0010]

[0011] The camellia essential oil comprises the following components in percentage by weight:

[0012] Oil-soluble red camellia extract 30-90%;

[0013] Emollients 10-70%.

[0014] As an embodiment of the present invention, the red camellia extract includes water, polyol, camellia extract, and camellia leaf extract; wherein the mass ratio of water, polyol, camellia extract, and camellia leaf extract is 50-80:3-30:1-10:1-10. The polyol is the same as the polyol in the camellia soft beads essence, including at least one of 1,3-propylene glycol, 1,2-pentanediol, 1,2-hexanediol, caprylyl glycol, etc., preferably 1,3-propylene glycol.

[0015] As an embodiment of the present invention, the thickener includes at least one of xanthan gum, carbomer, sclerotium gum, acrylic acid (esters) / C10-30 alkyl acrylate crosspolymer, hydroxyethyl cellulose, sodium alginate, polyacrylate crosspolymer-6, cellulose gum, ammonium acryloyldimethyltaurate / VP copolymer and the like.

[0016] As one embodiment of the present invention, the polyol includes at least one of 1,3-propylene glycol, 1,2-pentanediol, 1,2-hexanediol, caprylyl glycol, and the like.

[0017] As an embodiment of the present invention, the pH adjuster includes at least one of arginine, tromethamine, sodium hydroxide, etc. The pH adjuster of the present invention is used when the pH value needs to be adjusted (maintained at 5.0-7.0).

[0018] As one embodiment of the present invention, the preservative includes at least one of p-hydroxyacetophenone, phenoxyethanol, chlorphenesin and the like.

[0019] As an embodiment of the present invention, the oil-soluble red camellia extract comprises camellia seed oil, camellia extract and camellia leaf extract, wherein the mass ratio of camellia seed oil, camellia extract and camellia leaf extract is 90-94:3-5:3-5.

[0020] As an embodiment of the present invention, the emollient includes at least one of tri(ethylhexanoin)glyceryl, caprylic / capric triglyceride, coconut oil alcohol-caprylate / caprate, isononyl isononanoate, cetyl ethylhexanoate, etc., preferably one or more of tri(ethylhexanoin)glyceryl, caprylic / capric triglyceride.

[0021] As an embodiment of the present invention, the camellia essential oil does not contain higher fatty alcohol.

[0022] The present invention also provides a method for preparing the camellia soft beads, comprising the following steps:

[0023] S1. Preparation of Camellia Soft Bead Essence

[0024] The thickener is dispersed in part of the red camellia extract, and then heated and stirred to homogenize, and then a pH adjuster is added and stirred to form a hydrogel essence; then a preservative and a polyol are added, and after cooling, the remaining red camellia extract is added, stirred, and filtered to obtain a transparent aqueous phase, i.e., the camellia soft bead external phase essence liquid;

[0025] S2. Preparation of camellia essential oil

[0026] Mixing and stirring the oil-soluble red camellia extract and the emollient, filtering, and obtaining a transparent oil phase, namely, camellia essential oil;

[0027] S3. Preparation of Camellia Soft Beads

[0028] The obtained water phase and oil phase are heated and passed through a valve to form an oil bead mixture, namely Camellia Soft Beads.

[0029] As an embodiment of the present invention, in step S1, the red camellia extract includes water, polyol, camellia extract, and camellia leaf extract; wherein the mass ratio of water, polyol, camellia extract, and camellia leaf extract is 50-80:3-30:1-10:1-10. The preparation process of the red camellia extract and the camellia leaf extract includes but is not limited to water extraction or alcohol extraction process. Part of the red camellia extract refers to 60-85% of the total mass of the red camellia extract.

[0030] As an embodiment of the present invention, in step S1, the heating temperature is 8585°C; and the cooling temperature is 4085°C.

[0031] As an embodiment of the present invention, in step S1, the viscosity of the obtained external phase essence is controlled at 1000-6000 CP (measured by BROOKFIELD DV2T viscometer), and the yield value is maintained at about 10-500 Pa (measured by rheometer).

[0032] As an embodiment of the present invention, in step S2, the oil-soluble red camellia extract comprises camellia seed oil, camellia extract, and camellia leaf extract, wherein the mass ratio of camellia seed oil, camellia extract, and camellia leaf extract is 85-95:3-10:3-10. The preparation process of the oil-soluble red camellia extract includes but is not limited to pressing or supercritical carbon dioxide process.

[0033] As an embodiment of the present invention, in step S3, the heating temperature is 80-100° C. The present invention does not add any additional packaging ingredients.

[0034] As an embodiment of the present invention, in step S3, the obtained oil droplet size is between 0.01-5.0 mm and the particle size is uniform. According to the required soft bead size and the content of encapsulated oil, the required flow rates of the outer phase and the inner phase are adjusted.

[0035] Compared with the prior art, the present invention has the following beneficial effects:

[0036] Adding visualized microparticles, especially oil beads, to cosmetics, evenly suspending them in the essence, can increase the fun of consumers' use, and is also an innovation in new product formulations. However, the current technology is still immature, and the preparation and stability of oil beads are limited. The present invention uses microfluidic technology to prepare camellia soft beads containing red camellia extract, which are transparent in texture, uniform in oil beads, and spherical in shape. They can pass stability tests and can be applied to water-based essences, giving consumers a different skin care experience. DETAILED DESCRIPTION

[0037] The present invention is described in detail below in conjunction with specific embodiments. The following examples are implemented under the premise of the technical solution of the present invention, and provide detailed implementation methods and specific operation processes, which will help those skilled in the art to further understand the present invention. It should be pointed out that the protection scope of the present invention is not limited to the following embodiments, and several adjustments and improvements made under the premise of the concept of the present invention all belong to the protection scope of the present invention.

[0038] Example 1

[0039] The purpose of the present invention can be achieved by the following scheme:

[0040] The present invention provides camellia soft beads containing red camellia extract, which include camellia soft beads external essence liquid and camellia essential oil composition by mass percentage, and the specific component contents are shown in Table 1.

[0041] The red camellia extract used includes water, 1,3-propylene glycol, camellia extract and camellia leaf extract in a mass ratio of 69:25:3:3; the preparation processes of the red camellia extract and camellia leaf extract are as follows: crush equal amounts of camellia and camellia leaf powder respectively, add water 20 times of their mass, perform ultrasonic extraction for 30 minutes, then heat up to 60°C, stir and extract for 2 hours, then cool down to 40°C and filter to obtain a camellia leaf extract solution; heat the extract solution to 65°C, then add 2% of its mass of activated carbon to the extract solution and stir for 30 minutes, then filter, and then concentrate the filtrate to one tenth of its mass to obtain a camellia extract and a camellia leaf extract, and finally the components are blended and filtered to obtain.

[0042] The oil-soluble red camellia extract used includes camellia seed oil, camellia extract and camellia leaf extract in a mass ratio of 92:4:4. The preparation process of the oil-soluble red camellia extract is as follows: first, the camellia seeds are crushed and passed through a 40-mesh sieve to obtain camellia seed powder, then the camellia seed powder is loaded into a supercritical carbon dioxide extraction column, the pressure is set to 25 MPa, the temperature is 50°C, and the extraction is performed for 2 hours to obtain camellia seed oil; equal amounts of camellia and camellia leaves are crushed respectively, passed through a 40-mesh sieve to obtain camellia leaf powder, then the camellia leaf powder is loaded into a supercritical carbon dioxide extraction column, the pressure is set to 20 MPa, the temperature is 45°C, and the extraction is performed for 3 hours to obtain red camellia leaf extract, and the camellia seed oil and the camellia leaf extract are mixed and filtered to obtain the extract.

[0043] The preparation method of the camellia soft beads comprises the following steps:

[0044] S1. Preparation of Camellia Soft Beads Essence:

[0045] a. Add 0.6% of the thickener carbomer to 80% of the total mass of the red camellia extract and disperse, then heat to 85°C and stir to form a uniform aqueous phase;

[0046] b. Add 0.5% tromethamine as a pH adjuster and stir to form a hydrogel essence with a certain viscosity;

[0047] c. Add 0.4% p-hydroxyacetophenone and 0.5% polyol 1,2-hexanediol as preservatives, and stir to disperse evenly;

[0048] d. Cool down and stir the remaining red camellia extract, filter it evenly to form a transparent water phase (Camellia Soft Bead Essence, viscosity is 4500CP, yield value is 300Pa).

[0049] S2. Preparation method of camellia essential oil:

[0050] a. Mix the oil-soluble red camellia extract and the emollient in a mass ratio of 50:50;

[0051] b. Filter the mixed camellia essential oil composition to form a transparent oil phase (camellia essential oil).

[0052] S3. Preparation method of camellia soft beads:

[0053] The water phase and the oil phase are heated to 95°C according to the oil / liquid mass ratio (25:75), and a transparent oil condensate mixture with a certain oil droplet size is formed through a valve with a 2mm aperture. The oil droplet size is between 2mm and the particle size is uniform.

[0054] Among them, the thickener used is carbomer, the pH adjuster is tromethamine, the preservative is p-hydroxyacetophenone, the polyol is 1,2-hexanediol, and the emollient is camellia sinensis extract and triethylhexanoin.

[0055] Embodiment 2-8

[0056] The composition and preparation method are basically the same as those in Example 1, and the specific examples are shown in Table 1:

[0057] Table 1

[0058]

[0059]

[0060] The stability of Camellia Soft Beads was examined under seven accelerated stability test conditions (room temperature, 40°C, 48°C, 3°C, -10°C, -18°C and light), and passed the preservation challenge test. The safety of Camellia Soft Beads was verified by human testing using a 1% sodium dodecyl sulfate 24h occluded patch stimulation model and the chick embryo chorioallantoic membrane eye irritation test method.

[0061] The results of product stability test are shown in Table 2: Examples 2, 3, 4, and 8 have better effects, and Examples 1, 5-7 are used for comparison.

[0062] Table 2

[0063]

[0064] Camellia Soft Beads Antiseptic Challenge Test

[0065] The test method and judgment standard of the antiseptic challenge experiment were formulated with reference to the United States Pharmacopoeia USP51, the European Pharmacopoeia EP7.0 and the CTFA method. A mixed inoculation method was adopted, inoculated on the 0th day, and inoculated in two groups: one group of bacteria was mixed, and the actual concentration inoculated into the sample was 10 6 cfu / ml(g). The fungi were mixed with mold and yeast and the actual concentration of the sample was 10 5 The results were tested 7, 14, 21 and 28 days after inoculation.

[0066] The inoculated strains are shown in Table 3:

[0067] Table 3

[0068]

[0069] The results are shown in Table 4:

[0070] Table 4

[0071]

[0072] The results of the Camellia Soft Beads antiseptic challenge test are shown in Figure 5, and all of them passed the antiseptic challenge test.

[0073] Table 5

[0074]

[0075]

[0076] Camellia Soft Beads Safety Test

[0077] 1. Human patch test

[0078] The camellia beads prepared in all the above examples were subjected to human skin occlusive patch test, and the test method was based on the human skin patch test in the "Technical Specifications for Safety of Cosmetics" (2015 edition). The method of the skin occlusive patch test is as follows: 30 subjects aged 18-60 years old were selected, and the area of ​​​​the patch was not more than 50mm 2 , a qualified spot test device with a depth of about 1mm, take 20μL of the essence oil prepared in the above examples and comparative examples and put it into the small chamber of the spot tester, the negative control well is a blank control (no substance is placed), apply the spot tester to the inner side of the forearm of the subject, and gently press it with the palm to evenly apply it on the skin for 24 hours. Observe the skin reaction according to the standards in Table 6 30 minutes (after the indentation disappears), 24 hours and 48 hours after removing the spot tester, and record the observation results. The patch test results are shown in Table 7.

[0079] The experimental results showed that there were no adverse reactions in the 30 subjects treated with Examples 1-8.

[0080] Table 6 Skin reaction grading standards for skin occlusive patch test

[0081]

[0082] Table 7 Human safety test results

[0083]

[0084] 2. Chicken embryo chorioallantoic membrane test

[0085] Camellia japonica soft beads prepared by all the above-mentioned embodiments are subjected to the chicken embryo chorioallantoic membrane test, and the test method is the chicken embryo chorioallantoic membrane test of eye irritation / corrosiveness of cosmetics with reference to SN / T 2329-2009. This is a kind of eye irritation in vitro evaluation method adopted earlier, and chorioallantoic membrane (CAM) is a respiratory membrane, surrounded by chicken embryo. This test utilizes the complete, clear and transparent characteristics of the chorioallantoic membrane vascular system of the chicken embryo incubation period, and a certain amount of test substance is directly contacted with the chicken embryo chorioallantoic membrane, and the change of the chorioallantoic membrane toxic effect index (such as: hemorrhage, coagulation and vascular melting) is observed after acting for a period of time, and these indexes reflect the morphological structure, color and permeability of blood vessels and vascular network, and reflect the phenomenon such as chorioallantoic membrane protein denaturation and its degree of damage, and then combine to obtain a score, which is used to evaluate the eye irritation of the test substance. The scoring standard is as shown in Table 8. Experimental result Table 9 shows that the chicken embryo test of embodiment 1-8 has no irritation reaction.

[0086] Table 8 Endpoint scoring method results evaluation

[0087] End point scoring Irritation classification ES=0 Non-irritating 0<ES≤4 Mild irritation 4<ES<5.3 Moderate irritation 5.3≤ES Strong irritant / corrosive

[0088] Table 9 Irritation ratings of the examples

[0089]

[0090]

[0091] The above describes the specific embodiments of the present invention. It should be understood that the present invention is not limited to the above specific embodiments, and those skilled in the art may make various modifications or variations within the scope of the claims, which do not affect the essence of the present invention.

Claims

1. A camellia soft bead containing red camellia extract, characterized in that: Calculated by mass percentage, it includes 30-80% of the outer phase and 20-70% of the inner phase, the outer phase is camellia soft bead essence liquid, and the inner phase is camellia soft bead essence oil; The camellia soft beads essence comprises the following components in percentage by weight: Red Camellia Extract 60-99%; Thickener 0.01-15%; Polyol 0.01-10%; pH adjuster 0-5%; Preservatives 0.01-10%; The camellia soft bead essence oil comprises the following components in percentage by weight: Oil-soluble red camellia extract 30 -90%; Emollients 10-70%; The red camellia extract comprises water, polyol, camellia extract and camellia leaf extract; wherein the mass ratio of water, polyol, camellia extract and camellia leaf extract is 50-80:3-30:1-10:1-10; The oil-soluble red camellia extract comprises camellia seed oil, camellia extract and camellia leaf extract, wherein the mass ratio of camellia seed oil, camellia extract and camellia leaf extract is 90-94:3-5:3-5; The emollient is at least one of tri(ethylhexanoin)glyceryl, caprylic / capric triglyceride, coconut oil alcohol-caprylate / caprate, isononyl isononanoate, and cetyl ethylhexanoate; The camellia soft beads containing red camellia extract are prepared by microfluidic technology, and the steps are as follows: S1. Preparation of Camellia Soft Bead Essence The thickener is dispersed in part of the red camellia extract, and then heated and stirred to homogenize, and then a pH adjuster is added and stirred to form a hydrogel essence; then a preservative and a polyol are added, and after cooling, the remaining red camellia extract is added, stirred, and filtered to obtain a transparent aqueous phase, i.e., the camellia soft bead essence; S2. Preparation of Camellia Soft Beads Essence Oil Mix the oil-soluble red camellia extract and the emollient, stir, and filter to obtain a transparent oil phase, namely, the camellia soft bead essence oil; S3. Preparation of Camellia Soft Beads The obtained camellia soft bead essence liquid and camellia soft bead essence oil are heated and formed into an oil gel bead mixture, namely camellia soft beads, through a valve.

2. The camellia soft beads according to claim 1, characterized in that: The thickener includes at least one of xanthan gum, carbomer, sclerotium gum, acrylic acid (esters) / C10-30 alkyl acrylate cross-linked polymer, hydroxyethyl cellulose, sodium alginate, polyacrylate cross-linked polymer-6, cellulose gum, and ammonium acryloyldimethyltaurate / VP copolymer; the polyol includes at least one of 1,3-propylene glycol, 1,2-pentanediol, 1,2-hexanediol, and caprylyl glycol; the pH adjuster includes at least one of arginine, tromethamine, and sodium hydroxide; and the preservative includes at least one of p-hydroxyacetophenone, phenoxyethanol, and chlorphenesin.

3. The camellia soft beads according to claim 1, characterized in that: In step S1, the heating temperature is 85±5°C; the cooling temperature is 40±5°C.

4. The camellia soft beads according to claim 1, characterized in that: In step S1, the viscosity of the obtained external phase essence liquid is 1000-6000CP, and the yield value is 10-500 Pa.

5. The camellia soft beads according to claim 1, characterized in that: In step S3, the heating temperature is 80-100°C.

6. The camellia soft beads according to claim 1, characterized in that: In step S3, the particle size of the obtained oil condensate beads is 0.01-5.0 mm.

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