阅读说明：本技术 一种具有舒缓功效的皮克林乳液及其应用 (Pickering emulsion with relieving effect and application thereof ) 是由 胡喜芬 于 2021-10-08 设计创作，主要内容包括：本发明公开了一种具有舒缓功效的皮克林乳液及其应用。所述的皮克林乳液,包括如下质量百分含量的组分：淀粉辛烯基琥珀酸铝1-10%,玉米醇溶蛋白0.1-1%,油性组分1-20%,水性组分75-95%。本发明将玉米醇溶蛋白用过量乙醇溶解再旋蒸脱去乙醇,获得了小粒径的玉米醇溶蛋白,然后与大粒径的淀粉辛烯基琥珀酸铝复配,两者在油滴表面形成致密吸附层,所形成的乳液界面膜不易破裂,稳定性佳。本发明采用高压均质法处理,获得了纳米级的皮克林乳液,有利于甘草查尔酮A等活性成分的透皮吸收,生物利用度得到提高。本发明将甘草查尔酮A、植物甾醇油酸酯两者复配使用,发挥了更佳的舒缓功效。(The invention discloses a pickering emulsion with a relieving effect and application thereof. The Pickering emulsion comprises the following components in percentage by mass: 1-10% of starch aluminum octenyl succinate, 0.1-1% of zein, 1-20% of oily component and 75-95% of aqueous component. According to the invention, zein is dissolved by using excessive ethanol and then the ethanol is removed by rotary evaporation, so that zein with small particle size is obtained, and then the zein is compounded with starch octenyl aluminum succinate with large particle size, so that a compact adsorption layer is formed on the surface of oil drops, and the formed emulsion interface film is not easy to crack and has good stability. The invention adopts a high-pressure homogenization method to process, obtains the nano-scale Pickering emulsion, is beneficial to the transdermal absorption of active ingredients such as licochalcone A and the like, and improves the bioavailability. According to the invention, the licochalcone A and the phytosterol oleate are compounded for use, so that a better relieving effect is exerted.)

1. The Pickering emulsion is characterized by comprising the following components in percentage by mass: 1-10% of starch aluminum octenyl succinate, 0.1-1% of zein, 1-20% of oily component and 75-95% of aqueous component.

2. A pickering emulsion according to claim 1, wherein said oily components include licochalcone a, phytosterol oleate and fats and oils.

3. The pickering emulsion according to claim 2, wherein the oil or fat is one or a mixture of two or more of hydrocarbon oil, synthetic fatty acid ester, and animal or vegetable oil.

4. A pickering emulsion according to claim 3, wherein said oil is a mixture of glycerol tri (ethyl hexanoate) ester and corn germ oil.

5. A pickering emulsion according to claim 1, wherein said aqueous component comprises 1, 3-propanediol, hexylene glycol, water.

6. The licochalcone A-loaded Pickering emulsion with the relieving effect is characterized by comprising the following components in percentage by mass:

1-10% of starch aluminum octenyl succinate

Zein 0.1-1%

Glycerol tri (ethyl hexanoate) ester 0.4-9%

Corn germ oil 0.4-9%

Licochalcone A0.1-1%

Phytosterol oleate 0.1-1%

10-20% of 1, 3-propylene glycol

2 to 4 percent of hexanediol

The balance of water.

7. A process for the preparation of a Pickering emulsion according to any one of claims 1 to 6, comprising the steps of:

(1) dissolving zein completely with excessive ethanol, adding water-based component and aluminum starch octenyl succinate, stirring, rotary evaporating to remove ethanol, and keeping the temperature at 45-55 deg.C to obtain water phase;

(2) adding the oily component into an oil phase pan, heating to 45-55 ℃ under stirring, and completely dissolving to obtain an oil phase;

(3) pumping the water phase into an emulsifying pot, and pumping the oil phase into the emulsifying pot again under stirring; starting 30-50HZ for homogenizing, and treating for 3-5 minutes to obtain emulsion; and then treating the emulsion for 2-3 times by using a 500bar high-pressure homogenizer at 45-55 ℃ to obtain the Pickering emulsion.

Technical Field

The invention relates to the field of cosmetics, and particularly relates to a pickering emulsion with a relieving effect and application thereof.

Background

The emulsion is two immiscible liquidsMultiphase systems exist stably with a short time equilibrium, in which one phase is uniformly dispersed in the other phase in the form of droplets, and thus are characterized as suspensions, which can be generally classified into oil-in-water (O/W) and water-in-oil (W/O). As a metastable system that changes thermodynamically over time, emulsions have a tendency to spontaneously stratify, and their stability needs to be enhanced by the addition of suitable exogenous agents. As early as the 20 th century, Ramsden and Pickering successively proposed that emulsions could be strengthened by the addition of solid particles in micro-or nano-scale, i.e. by adsorption of the particles at the oil-water interface, to promote their stabilization, and later this type of emulsion was named Pickering emulsion (Pickering emulsion). Because the solid particles have higher free energy, compared with the traditional emulsion with the stabilizing effect of the micromolecule surfactant, the Pickering emulsion can form a powerful physical barrier at an oil-water interface through the solid particles, avoid the coalescence of liquid drops and the austenite curing, and have better stability^[1]. In the fields of food and medicine, pickering emulsions have been widely used for the encapsulation and delivery of functional nutrients, but in the field of cosmetics, pickering emulsions have been less reported.

Under the situation that the cosmetic manufacturing industry is continuously developing, the number of types of raw materials for preparing cosmetics is continuously increased, and the number of raw materials used in the formula of the cosmetics is also continuously increased, so that the safety risk of the cosmetics is higher and higher. According to the data of the adverse reaction monitoring network of cosmetics of China Ministry of health, contact dermatitis caused by cosmetic allergy or stimulation accounts for more than 90 percent of skin diseases of cosmetics. In order to reduce the safety risk of cosmetic preparation and use as much as possible and make the product milder, various major cosmetic companies add plant extracts, active polypeptides and other skin allergy resistant active ingredients into the formula to play a role in prevention and relief.

Licochalcone a is a flavonoid, having the name of english: licochalcone a; the abbreviation is: Lico-A; CAS: 58749-22-7; the molecular formula is as follows: C21H22O 4; molecular weight: 338.4, respectively; the characteristics are as follows: the color of the general product is orange yellow, the product is powdery, and the product is insoluble in water and easy to dissolve in an organic solvent. Licorice root ChaerKetone A is the licoflavone monomer with the highest content in glycyrrhiza inflata which is the main product in Xinjiang in China, has obvious curative effects of resisting bacteria and oxidation, has activities of resisting inflammation, resisting tumors, promoting immunity, protecting nerves and the like, and has high potential economic value^[2]。

Reference documents:

[1] raney dragon, Zhoujianwei, Goode, Xuenbo, Yexing Qian, Liudong red, research progress of nano starch-based pickering emulsion [ J ]. Chinese food science, 2021,21(06): 312-.

[2] Juwei, extraction and derivatization of licochalcone A and design of extraction and separation plant [ D ]. university of Shanxi science and technology, 2018.

Disclosure of Invention

Aiming at the market demand and the defects of the prior art, the invention mainly aims to provide a Pickering emulsion with a soothing effect and loaded with active ingredients and application thereof.

In order to solve the technical problems, the invention provides the following technical scheme: the Pickering emulsion comprises the following components in percentage by mass: 1-10% of starch aluminum octenyl succinate, 0.1-1% of zein, 1-20% of oily component and 75-95% of aqueous component.

In some embodiments of the invention, the oily component comprises licochalcone a, phytosterol oleate and a lipid.

Furthermore, the oil and fat can be one or a mixture of more than two of hydrocarbon oil, synthetic fatty acid ester and animal and vegetable oil. In some of these embodiments, the oil is a mixture of glycerol tri (ethyl hexanoate) and corn germ oil.

In some embodiments of the invention, the aqueous component comprises 1, 3-propanediol, hexanediol, water.

The embodiment of the invention provides licochalcone A-loaded Pickering emulsion with a relieving effect, which comprises the following components in percentage by mass:

1-10% of starch aluminum octenyl succinate

Zein 0.1-1%

Glycerol tri (ethyl hexanoate) ester 0.4-9%

Corn germ oil 0.4-9%

Licochalcone A0.1-1%

Phytosterol oleate 0.1-1%

10-20% of 1, 3-propylene glycol

2 to 4 percent of hexanediol

The balance of water.

The embodiment of the invention also discloses a preparation method of the pickering emulsion, which comprises the following steps:

(1) dissolving zein completely with excessive ethanol, adding water-based component and aluminum starch octenyl succinate, stirring, rotary evaporating to remove ethanol, and keeping the temperature at 45-55 deg.C to obtain water phase;

(2) adding the oily component into an oil phase pan, heating to 45-55 ℃ under stirring, and completely dissolving to obtain an oil phase;

(3) pumping the water phase into an emulsifying pot, and pumping the oil phase into the emulsifying pot again under stirring; starting 30-50HZ for homogenizing, and treating for 3-5 minutes to obtain emulsion; and then treating the emulsion for 2-3 times by using a 500bar high-pressure homogenizer at 45-55 ℃ to obtain the Pickering emulsion.

The technical scheme provided by the embodiment of the invention has the following beneficial effects:

(1) according to the invention, zein is dissolved by using excessive ethanol and then is subjected to rotary evaporation to remove the ethanol, so that zein with small particle size is obtained, and then is compounded with starch octenyl aluminum succinate with large particle size, so that a compact adsorption layer is formed on the surface of oil drops, and the prepared emulsion interface film is not easy to crack and has good stability;

(2) the invention adopts a high-pressure homogenization method for treatment, obtains the nanoscale Pickering emulsion, is beneficial to the transdermal absorption of active ingredients such as licochalcone A and the like, and improves the bioavailability;

(3) according to the invention, the licochalcone A and the phytosterol oleate are compounded for use, so that a better relieving effect is exerted.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art are briefly introduced below.

FIG. 1 volunteer TEWL improvement;

FIG. 2 change in mean of VISIA skin Red zone feature counts before and after volunteer use; "x" indicates significant differences in comparison of data at different time points (p < 0.05);

FIG. 3 improvement of skin problems in volunteers.

Detailed Description

The invention discloses a Pickering emulsion. Those skilled in the art can modify the process parameters appropriately to achieve the desired results with reference to the disclosure herein. It is expressly intended that all such similar substitutes and modifications which would be obvious to one skilled in the art are deemed to be included in the invention. While the methods and applications of this invention have been described in terms of preferred embodiments, it will be apparent to those of ordinary skill in the art that variations and modifications in the methods and applications described herein, as well as appropriate variations and combinations, may be made to implement and use the techniques of this invention without departing from the spirit and scope of the invention.

The raw materials and reagents used in the pickering emulsion provided by the invention can be purchased from the market.

The invention is further illustrated by the following examples:

example 1

The Pickering emulsion comprises the following components in percentage by mass:

starch aluminum octenyl succinate 1%

Zein 1%

Glycerol tris (ethylhexanoate) 9%

Corn germ oil 0.4%

1, 3-propanediol 20%

2 percent of hexanediol

The balance of water.

The preparation method of the pickering emulsion comprises the following steps:

(1) completely dissolving zein with excessive ethanol, adding the aqueous component and aluminum starch octenyl succinate, stirring, rotary evaporating to remove ethanol, and keeping the temperature at 45 deg.C to obtain water phase;

(2) adding the oily components into an oil phase pot, heating to 55 ℃ under stirring, and completely dissolving to obtain an oil phase;

(3) pumping the water phase into an emulsifying pot, and pumping the oil phase into the emulsifying pot again under stirring; starting 30HZ for homogenizing, and treating for 5 minutes to obtain emulsion; and then treating the emulsion for 3 times at 45 ℃ by using a 500bar high-pressure homogenizer to obtain the Pickering emulsion.

Example 2

The Pickering emulsion comprises the following components in percentage by mass:

aluminum starch octenyl succinate 10%

Zein 0.1%

Glycerol tri (ethyl hexanoate) 0.4%

Corn germ oil 9%

1, 3-propanediol 10%

Hexanediol 4%

The balance of water.

The preparation method of the pickering emulsion comprises the following steps:

(1) completely dissolving zein with excessive ethanol, adding the aqueous component and aluminum starch octenyl succinate, stirring, rotary evaporating to remove ethanol, and keeping the temperature at 55 deg.C to obtain water phase;

(2) adding the oily components into an oil phase pot, heating to 45 ℃ under stirring, and completely dissolving to obtain an oil phase;

(3) pumping the water phase into an emulsifying pot, and pumping the oil phase into the emulsifying pot again under stirring; starting 50HZ for homogenizing, and treating for 3 minutes to obtain emulsion; and then treating the emulsion for 2 times by using a 500bar high-pressure homogenizer at 55 ℃ to obtain the Pickering emulsion.

Example 3

The Pickering emulsion comprises the following components in percentage by mass:

starch aluminum octenyl succinate 5%

Zein 0.5%

Glycerol tris (ethylhexanoate) 5%

Corn germ oil 4%

1, 3-propanediol 15%

Hexanediol 3%

The balance of water.

The preparation method of the pickering emulsion comprises the following steps:

(1) completely dissolving zein with excessive ethanol, adding the aqueous component and aluminum starch octenyl succinate, stirring, rotary evaporating to remove ethanol, and keeping the temperature at 50 deg.C to obtain water phase;

(2) adding the oily components into an oil phase pan, heating to 50 ℃ under stirring, and completely dissolving to obtain an oil phase;

(3) pumping the water phase into an emulsifying pot, and pumping the oil phase into the emulsifying pot again under stirring; starting 40HZ homogenization, and treating for 4 minutes to obtain emulsion; and then treating the emulsion for 2 times by using a 500bar high-pressure homogenizer at 50 ℃ to obtain the Pickering emulsion.

Comparative example 1

The Pickering emulsion comprises the following components in percentage by mass:

starch aluminum octenyl succinate 5%

Glycerol tris (ethylhexanoate) 5%

Corn germ oil 4%

1, 3-propanediol 15%

Hexanediol 3%

The balance of water.

The preparation method of the pickering emulsion comprises the following steps:

(1) completely dissolving zein with excessive ethanol, adding the aqueous component and aluminum starch octenyl succinate, stirring, rotary evaporating to remove ethanol, and keeping the temperature at 50 deg.C to obtain water phase;

(2) adding the oily components into an oil phase pan, heating to 50 ℃ under stirring, and completely dissolving to obtain an oil phase;

(3) pumping the water phase into an emulsifying pot, and pumping the oil phase into the emulsifying pot again under stirring; starting 40HZ homogenization, and treating for 4 minutes to obtain emulsion; and then treating the emulsion for 2 times by using a 500bar high-pressure homogenizer at 50 ℃ to obtain the Pickering emulsion.

Comparative example 2

The Pickering emulsion comprises the following components in percentage by mass:

zein 0.5%

Glycerol tris (ethylhexanoate) 5%

Corn germ oil 4%

1, 3-propanediol 15%

Hexanediol 3%

The balance of water.

The preparation method of the pickering emulsion comprises the following steps:

(1) completely dissolving zein with excessive ethanol, adding the aqueous component and aluminum starch octenyl succinate, stirring, rotary evaporating to remove ethanol, and keeping the temperature at 50 deg.C to obtain water phase;

(2) adding the oily components into an oil phase pan, heating to 50 ℃ under stirring, and completely dissolving to obtain an oil phase;

(3) pumping the water phase into an emulsifying pot, and pumping the oil phase into the emulsifying pot again under stirring; starting 40HZ homogenization, and treating for 4 minutes to obtain emulsion; and then treating the emulsion for 2 times by using a 500bar high-pressure homogenizer at 50 ℃ to obtain the Pickering emulsion.

Test 1 laser particle size Analyzer measurement

The pickering emulsions prepared in examples 1 to 3 and comparative examples 1 to 2 were measured with a laser particle size analyzer using water as a dispersion medium at a temperature of 25 ℃. According to the reference (Liuwei, von Neng-Neng. transdermal administration nanotechnology [ M ]. Beijing: Chinese pharmaceutical science and technology Press, 2020: 11.), PDI less than 0.3 indicates that the nano-carrier is well dispersed and less in adhesion and aggregation. The specific test results are shown in table 1 below.

TABLE 1 particle diameter and particle diameter distribution measurement results

As can be seen from Table 1, the Pickering emulsions prepared in examples 1-3 all had average particle sizes of less than 100nm and PDI values of < 0.3, showing better stability and smaller particle sizes than those of comparative examples 1-2.

Example 4

The Pickering emulsion with the relieving effect comprises the following components in percentage by mass:

starch aluminum octenyl succinate 5%

Zein 0.5%

Glycerol tris (ethylhexanoate) 5%

Corn germ oil 4%

Licochalcone A0.1%

Phytosterol oleate 1%

1, 3-propanediol 15%

Hexanediol 3%

The balance of water.

The preparation method of the pickering emulsion comprises the following steps:

(1) completely dissolving zein with excessive ethanol, adding the aqueous component and aluminum starch octenyl succinate, stirring, rotary evaporating to remove ethanol, and keeping the temperature at 50 deg.C to obtain water phase;

(2) adding the oily components into an oil phase pan, heating to 50 ℃ under stirring, and completely dissolving to obtain an oil phase;

(3) pumping the water phase into an emulsifying pot, and pumping the oil phase into the emulsifying pot again under stirring; starting 40HZ homogenization, and treating for 4 minutes to obtain emulsion; and then treating the emulsion for 2 times by using a 500bar high-pressure homogenizer at 50 ℃ to obtain the Pickering emulsion.

Example 5

The Pickering emulsion with the relieving effect comprises the following components in percentage by mass:

starch aluminum octenyl succinate 5%

Zein 0.5%

Glycerol tris (ethylhexanoate) 5%

Corn germ oil 4%

Licochalcone A1%

Phytosterol oleate 0.1%

1, 3-propanediol 15%

Hexanediol 3%

The balance of water.

The preparation method of the pickering emulsion comprises the following steps:

(1) completely dissolving zein with excessive ethanol, adding the aqueous component and aluminum starch octenyl succinate, stirring, rotary evaporating to remove ethanol, and keeping the temperature at 50 deg.C to obtain water phase;

(2) adding the oily components into an oil phase pan, heating to 50 ℃ under stirring, and completely dissolving to obtain an oil phase;

(3) pumping the water phase into an emulsifying pot, and pumping the oil phase into the emulsifying pot again under stirring; starting 40HZ homogenization, and treating for 4 minutes to obtain emulsion; and then treating the emulsion for 2 times by using a 500bar high-pressure homogenizer at 50 ℃ to obtain the Pickering emulsion.

Example 6

The Pickering emulsion with the relieving effect comprises the following components in percentage by mass:

starch aluminum octenyl succinate 5%

Zein 0.5%

Glycerol tris (ethylhexanoate) 5%

Corn germ oil 4%

Licochalcone A0.5%

Phytosterol oleate 0.5%

1, 3-propanediol 15%

Hexanediol 3%

The balance of water.

The preparation method of the pickering emulsion comprises the following steps:

(1) completely dissolving zein with excessive ethanol, adding the aqueous component and aluminum starch octenyl succinate, stirring, rotary evaporating to remove ethanol, and keeping the temperature at 50 deg.C to obtain water phase;

(2) adding the oily components into an oil phase pan, heating to 50 ℃ under stirring, and completely dissolving to obtain an oil phase;

(3) pumping the water phase into an emulsifying pot, and pumping the oil phase into the emulsifying pot again under stirring; starting 40HZ homogenization, and treating for 4 minutes to obtain emulsion; and then treating the emulsion for 2 times by using a 500bar high-pressure homogenizer at 50 ℃ to obtain the Pickering emulsion.

Comparative example 3

The Pickering emulsion with the relieving effect comprises the following components in percentage by mass:

starch aluminum octenyl succinate 5%

Zein 0.5%

Glycerol tris (ethylhexanoate) 5%

Corn germ oil 4%

Phytosterol oleate 1%

1, 3-propanediol 15%

Hexanediol 3%

The balance of water.

The preparation method of the pickering emulsion comprises the following steps:

(1) completely dissolving zein with excessive ethanol, adding the aqueous component and aluminum starch octenyl succinate, stirring, rotary evaporating to remove ethanol, and keeping the temperature at 50 deg.C to obtain water phase;

(2) adding the oily components into an oil phase pan, heating to 50 ℃ under stirring, and completely dissolving to obtain an oil phase;

(3) pumping the water phase into an emulsifying pot, and pumping the oil phase into the emulsifying pot again under stirring; starting 40HZ homogenization, and treating for 4 minutes to obtain emulsion; and then treating the emulsion for 2 times by using a 500bar high-pressure homogenizer at 50 ℃ to obtain the Pickering emulsion.

Comparative example 4

The Pickering emulsion with the relieving effect comprises the following components in percentage by mass:

starch aluminum octenyl succinate 5%

Zein 0.5%

Glycerol tris (ethylhexanoate) 5%

Corn germ oil 4%

Licochalcone A1%

1, 3-propanediol 15%

Hexanediol 3%

The balance of water.

The preparation method of the pickering emulsion comprises the following steps:

(1) completely dissolving zein with excessive ethanol, adding the aqueous component and aluminum starch octenyl succinate, stirring, rotary evaporating to remove ethanol, and keeping the temperature at 50 deg.C to obtain water phase;

(2) adding the oily components into an oil phase pan, heating to 50 ℃ under stirring, and completely dissolving to obtain an oil phase;

(3) pumping the water phase into an emulsifying pot, and pumping the oil phase into the emulsifying pot again under stirring; starting 40HZ homogenization, and treating for 4 minutes to obtain emulsion; and then treating the emulsion for 2 times by using a 500bar high-pressure homogenizer at 50 ℃ to obtain the Pickering emulsion.

Experiment 3 skin irritation repair experiment

The pickering lotion prepared in examples 4 to 6 and comparative examples 3 to 4 was subjected to skin irritation recovery test, and example 3 in which no active ingredient was added was used as a control group.

Selection of volunteers: volunteers 32 of 25-60 years old who meet the requirements of the test were selected as subjects. The following cases cannot be selected as subjects: those who use antihistamines for nearly one week or immunosuppressants for nearly one month; in the last two months, any anti-inflammatory drug is applied to the tested part; the subject has a clinically unvulcanized inflammatory skin condition; insulin-dependent diabetic patients; patients suffering from asthma or other chronic respiratory diseases undergoing therapy; those receiving anti-cancer chemotherapy within approximately 6 months; patients with immunodeficiency or autoimmune disease; lactating or pregnant women; bilateral mastectomy and bilateral underarm lymph node resection; the judgment of the test result is influenced by scars, pigments, atrophy, port wine stains or other flaws on the skin to be tested; participation in other clinical trial investigators; non-volunteer participants or those who cannot complete the prescribed content as required by the trial.

The evaluation method comprises the following steps: in many previous studies, SLS patch test was used to evaluate whether patients are prone to irritant dermatitis, which is a means of evaluating skin barrier function. Referring to the reference (Cao Ming, Fii, Yangying, application study of Tremella polysaccharide WSK in strengthening skin barrier [ J ]. contemporary chemical research, 2020(14): 106-. TEWL change (%) = (before use-after use)/100% before use.

As can be seen from FIG. 1, the Pickering emulsions prepared in examples 4-6 of the present invention have a stronger ability to repair skin barrier damage than comparative examples 3-4.

Test 4 trial test on population

11 volunteers from Guangzhou, 8 women, 3 men, aged 28-52 years, with marked abnormal conditions of redness, itching, desquamation, etc. were collected during 3-6 months in 2021 at the cooperative beauty parlor. The volunteers used the Pickering lotion prepared in example 6 of the present invention 1 time each day, and applied a proper amount of the sample to the affected part, and the sample was applied gently and uniformly. After 1 week of continuous use, pictures of the face were taken using VISIA 7 and reviewed on day 7 to inquire the volunteers about abnormal conditions such as redness, itching, desquamation, etc. The record of significant improvement in abnormal conditions such as redness, itching, desquamation, etc. was significant, the record of some improvement in abnormal conditions was significant, and the record of other cases was invalid. The specific test results are shown in fig. 2 and fig. 3.

As can be seen from fig. 2, the volunteer's red zone characteristic count values decreased significantly after use of the product; as can be seen from FIG. 3, after the product is used, the abnormal conditions of redness, pruritus, desquamation and the like of most volunteers are relieved. Therefore, the pickering emulsion prepared by the embodiment of the invention shows good relieving effect.

The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.