CN112972310A

CN112972310A - Composition with antibacterial and repairing effects and preparation method thereof

Info

Publication number: CN112972310A
Application number: CN202110307121.0A
Authority: CN
Inventors: 俞超; 胡茂秀
Original assignee: Qingdao Zhibo Biotechnology Co ltd
Current assignee: Qingdao Zhibo Biotechnology Co ltd
Priority date: 2021-03-23
Filing date: 2021-03-23
Publication date: 2021-06-18

Abstract

The invention provides a combined formula with bacteriostatic and repairing effects and a preparation method thereof. The formula comprises the following components: plant essential oil with bacteriostatic action, plant source bacteriostatic substances, plant extracts with anti-inflammatory and astringent effects, sodium hyaluronate with moisturizing and repairing effects, and other auxiliary substances. The combined formula completely adopts plant-derived bacteriostatic and anti-inflammatory substances, the combination of several substances with different bacteriostatic spectrums has obvious broad-spectrum bacteriostatic effects on various skin pathogenic bacteria including propionibacterium acnes, and the compound sodium hyaluronate has the functions of repairing and moisturizing, and has the moisturizing and repairing effects on damaged skin while inhibiting bacteria. In addition, the essential oil and the fat-soluble bacteriostat in the compound are prepared into clear and transparent liquid which can be mutually dissolved with water by a nano microcapsule micro-emulsion coating technology, thereby being beneficial to the compound use of different cosmetic formulations.

Description

Composition with antibacterial and repairing effects and preparation method thereof

Technical Field

The invention belongs to the technical field of medical health care and cosmetics, and particularly relates to a composition with bacteriostatic and repairing effects and a preparation method thereof, wherein the formula comprises the following components: plant essential oil with bacteriostatic action, plant source bacteriostatic substances, plant extract with anti-inflammatory and astringent effects, sodium hyaluronate and other auxiliary substances.

Background

At present, more and more people have facial skin inflammation or skin sensitivity problems, and the factors causing the facial sensitive dermatitis are various, wherein the factors comprise acne which is better developed in adolescents and chronic inflammatory dermatosis which is developed in a pilosebaceous unit; the skin care product causes face redness, dryness and desquamation due to improper use, and the skin becomes sensitive skin after repeated attack; or severe dehydration of the skin due to seasonal changes or environmental factors may reduce the protective function of the skin, and over-washing of the face may result in loss of the protective film of the skin and the appearance of erythema and desquamation of the cheeks. The existence of skin inflammation can affect the self image, even lose self confidence, and affect the quality of work and life. At present, the acne-removing cosmetics generally use salicylic acid, azelaic acid and other active ingredients, have certain effects, but have some adverse reactions, such as local burning pain, pruritus, erythema and the like. The main reason for these adverse reactions is that these acidic substances have poor solubility and thus need to be used in excess to exert therapeutic effect, and the higher the concentration of the acidic substances, the more easily the acidic substances are used, the more easily the acidic substances irritate the skin, and the further the skin is dried. Therefore, repairing facial problems requires reasonable bacteriostasis, inflammation diminishing, water replenishing and moisture preserving, which is the most basic requirement for skin care.

Sodium hyaluronate, also known as hyaluronic acid, is a major component of natural cell matrices and widely exists in relevant tissues such as animal skin, vitreous humor and synovial fluid of eyes. The substance belongs to a natural high molecular polysaccharide, has the functions of lubrication, moisture retention, water replenishing and the like, is praised as the most natural and healthy moisture retention factor in the field of cosmetics, can be quickly dissolved in water and is prepared into water emulsion products. The macromolecular sodium hyaluronate has strong water-holding capacity, can form a layer of breathable water film on the surface of skin, has the functions of locking water and preserving water, and simultaneously blocks the invasion of external bacteria, keeps the humidity of a wound and creates a moist environment. The micromolecular sodium hyaluronate can promote water to rapidly permeate into a basal layer, and directly promote cell growth, differentiation, reconstruction, repair and the like. The unique large, medium and small molecule sodium hyaluronate combination can effectively solve the problems of skin dryness and the like. However, sodium hyaluronate is an anionic polymer, and the antibacterial effect disappears after being compounded with cationic antibacterial substances commonly used in cosmetics, such as chitosan quaternary ammonium salt, chlorhexidine, lysine and the like. Meanwhile, the application of bacteriostatic substances, especially triterpenoid acid such as ursolic acid and oleanolic acid which has a good bacteriostatic action on propionibacterium acnes, is greatly limited due to the defects of low solubility, poor compatibility, high irritation of azelaic acid, salicylic acid and the like.

In order to solve the problems, bacteriostatic substances, anti-inflammatory and sedative substances and the like extracted from plants are selected to be compounded with sodium hyaluronate for experiments, and a composition formula with bacteriostatic, anti-inflammatory and moisturizing and repairing functions is sought. Meanwhile, by utilizing the nano microcapsule microemulsion technology, an acid substance with low solubility, poor compatibility and large irritation is attempted to be wrapped to prepare the microemulsion or the water-soluble inclusion compound which can be mutually dissolved with water, so that the nano microcapsule microemulsion can be applied to different formulations in the fields of cosmetics, medicine, health care and the like.

Disclosure of Invention

The invention aims to solve the technical problem of providing a composition with bacteriostatic and repairing effects aiming at the defects of the prior art. The composition with the bacteriostasis and repair effects is prepared by combining several plant-derived antibacterial substances with sodium hyaluronate, performs moisturizing and repair on skin while inhibiting bacteria, and can be safely applied to cosmetics containing animal and plant extracts and green cosmetics. The plant source extract comprises plant essential oil with antibacterial effect, including tea tree essential oil, lavender essential oil, myrrh essential oil, citronella essential oil, etc.; the plant source extract also comprises antibacterial substances such as triterpenes oleanolic acid, ursolic acid, etc., and substances with antiinflammatory and tranquillizing effects such as tea polyphenols, Sargassum extract, Hamamelis mollis extract, dipotassium glycyrrhizinate, flos Matricariae Chamomillae extract, Aloe extract, etc. According to the compatibility of different antibacterial spectra of essential oil, plant extract and fruit acid antibacterial substances, a biological antibacterial compatibility with a synergistic effect is found, a broad-spectrum universal antimicrobial system formula suitable for bacteria and fungi is prepared, and the antibacterial effect on acne propionibacterium acnes and common skin pathogenic bacteria is remarkable. The essential oil used in the invention has the functions of natural antisepsis and sterilization, skin care and skin tendering, has good bacteriostatic action on acne pathogenic bacteria, and is natural and non-irritant. The plant extract contains tannin, tea polyphenol, etc., has strong antiinflammatory effect, is helpful for treating skin inflammation such as acne and eczema, and has effect in astringing follicular orifice, so as to make skin firmer and finer. The tartaric acid substance has strong antibacterial property and good antibacterial activity on bacteria and fungi. The small-molecule sodium hyaluronate can promote water to rapidly permeate into a basal layer, directly promote cell growth, differentiation, reconstruction and repair, effectively repair pockmarks, solve the problem of dry skin and repair sensitive muscles. Therefore, the combined formula of the invention has better effects of bacteriostasis, repair and relieving skin inflammation, and can be used for different formulations in the fields of cosmetics and medical health care.

The invention also provides a method for coating essential oil, bacteriostatic substances and the like which are difficult to dissolve in water by using the nano microcapsule microemulsion technology. The plant essential oil and the plant-derived acidic bacteriostatic substance are not easy to dissolve in water, and the clear and bright essence prepared by the method is difficult. In order to overcome the problem, the invention adopts the nano microcapsule microemulsion technology to coat the essential oil and the bacteriostatic substance so as to form clear and transparent microemulsion or a water-soluble inclusion compound.

The invention also provides a preparation method of the composition essence with the bacteriostatic and repairing effects. The preparation process of the composition essence containing the antibacterial repairing effect comprises the following steps:

1) preparing plant essential oil, plant source liposoluble antibacterial substance, etc. into water-soluble microemulsion or water-soluble clathrate by nanometer microcapsule microemulsion technology, adding low molecular alcohol auxiliary substance, and mixing;

2) dissolving sodium hyaluronate with different molecular weights, adding water soluble plant extract, stirring while adding until mixing;

3) and mixing the microemulsion or the water-soluble bacteriostatic inclusion compound with the sodium hyaluronate solution, and uniformly stirring to obtain a clear and transparent solution. Then adding a proper amount of emulsion stabilizer, and uniformly stirring;

4) and (4) adding purified water to a constant volume to a theoretical amount, and continuously stirring until the solution is uniform to obtain clear and transparent essence.

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

1. the composition with the bacteriostasis and repair effects combines several plant-derived antibacterial substances with the sodium hyaluronate, performs moisturizing and repair on skin while inhibiting bacteria, and can be safely applied to cosmetics, medical appliances and medical and American industries containing plant extracts.

2. The botanical extract comprises plant essential oil, plant extract and botanical bacteriostatic substances, and is compatible for use according to different antibacterial spectrums, biological bacteriostatic compatibility with synergistic effect is found, a broad-spectrum universal antimicrobial system formula suitable for bacteria and fungi is prepared, and the bacteriostatic effect on acne propionibacterium acnes and common skin pathogenic bacteria is remarkable.

3. The preparation method of the composition essence containing the bacteriostatic repair effect comprises a nano microcapsule microemulsion technology, so that essential oil, plant extracts and bacteriostatic substances which are difficult to dissolve in water can form clear and transparent essence, and a new thought and method are provided for adding and using the bacteriostatic substances which are difficult to dissolve in water-phase cosmetics.

Detailed Description

The present invention is further explained below with reference to examples, which are not intended to limit the present invention in any way.

Example 1 comparison of the antibacterial effects of different concentrations of oleanolic acid and essential oil microemulsion

Because the oleanolic acid has poor water solubility, the tea tree essential oil micro-emulsion is required to be dissolved to prepare mixed solutions with different concentrations. According to the solubility of oleanolic acid in tea tree essential oil microemulsion, two mixed solution systems of 0.2% of oleanolic acid and 0.1% of tea tree oil microemulsion and 0.3% of oleanolic acid and 0.3% of tea tree oil microemulsion are respectively prepared. Then, the two mixed solutions are subjected to a 16-day stability bacteriostasis test at 45 ℃ according to appendix C of GB15979-2002 hygienic Standard for Disposable sanitary articles, namely a product bactericidal performance, bacteriostatic performance and stability test method, wherein the acting strains are staphylococcus aureus (ATCC6538), escherichia coli (ATCC25922) and propionibacterium acnes (ATCC25922), and the acting time is 30 minutes.

Table 1: comparison table of antibacterial stability of oleanolic acid and essential oil microemulsion mixed liquor with different concentrations

The results show that: the antibacterial rate and the antibacterial stability of the 0.3% oleanolic acid and 0.3% tea tree oil microemulsion mixed solution after being placed at 45 ℃ for 16 days are obviously better than those of the 0.2% oleanolic acid and 0.1% tea tree oil microemulsion mixed solution, so that the composition with the antibacterial repairing function selects the 0.3% oleanolic acid and 0.3% tea tree oil microemulsion mixed solution.

Example 2 preparation example of tea tree essential oil essence with bacteriostasis and repair effects and stability investigation of tea tree essential oil essence

This example illustrates that the composition with bacteriostatic and repairing effects disclosed in this patent can be prepared into a clear and transparent essence by a nano microemulsion technology, but is not limited to the preparation of the essence. The preparation process of the essence with the bacteriostatic and repairing effects is described by taking tea tree essential oil as an example and comprises the following steps:

1) preparing tea tree essential oil into 2% microemulsion, adding oleanolic acid to obtain 0.3% oleanolic acid + 0.3% tea tree oil microemulsion mixed solution;

2) hyaluronic acid with molecular weights of about 180 kilodaltons, 120 kilodaltons and 8000 kilodaltons is uniformly expanded, and the final concentrations are 0.1%, 0.3% and 0.4% respectively. Mixing, sequentially adding hydroxyacetophenone with final concentration of 0.3%, hamamelis virginiana extract with final concentration of 0.1%, EDTA-2Na with final concentration of 0.05% and dipotassium glycyrrhizinate with final concentration of 0.2%, stirring while adding until mixing;

3) uniformly mixing 1, 3-butanediol and glycerol, and adding the oleanolic acid and tea tree essential oil microemulsion mixed solution prepared in the step 1); then mixing the sodium hyaluronate solution with the mixed solution of sodium hyaluronate obtained in the step 2), and uniformly stirring to obtain a clear and transparent solution;

4) then adding a high-concentration xanthan gum solution to enable the final concentration to be 0.2%, and uniformly stirring;

5) and (3) fixing the volume to a theoretical amount by using purified water, and continuously stirring until the volume is uniform to obtain clear and transparent hyaluronic acid essence containing the tea essential oil and other composite plant extracts.

In order to study the stability of the essence composition containing the antibacterial repair effect, the tea tree essential oil hyaluronic acid essence is stored for 18 days at different temperatures (4 ℃, 25 ℃, 45 ℃) and under normal-temperature illumination (illumination intensity 4000Lux), and the stability of the tea tree essential oil hyaluronic acid essence is observed. The stability detection indexes comprise color, viscosity and bacteriostatic activity. The results are shown in Table 2.

Table 2: result of examining stability of essence with acne removing effect

The results show that: after the combined formula with bacteriostasis and restoration and the essence prepared by the combined formula are stored for 18 days under different temperature and illumination conditions, various performance indexes and bacteriostasis effects are stable, and the quality is in a composite standard.

Example 3 preparation of lavender essential oil essence with bacteriostatic repair effect and evaluation of bacteriostatic effect

This example illustrates that the composition with bacteriostatic and repairing effects disclosed in this patent can be prepared into a clear and transparent essence through a nanocapsule inclusion process, but is not limited to the preparation of the essence. The preparation process of the essence with the bacteriostatic and repairing effects by taking the lavender essential oil as an example is as follows:

1) wrapping azelaic acid with beta-cyclodextrin to obtain high-concentration inclusion compound, adding lavender essential oil microemulsion with final concentration of 0.1%, mixing uniformly to obtain azelaic acid final concentrations of 0.25% and 0.5%, and using non-wrapped azelaic acid with final concentration of 0.25% as control;

2) 3 kinds of hyaluronic acid with different molecular weights are dissolved uniformly, and the final concentrations are 0.1%, 0.3% and 0.2% respectively. Mixing, sequentially adding flos Matricariae Chamomillae extract with final concentration of 0.1% and dipotassium glycyrrhizinate with final concentration of 0.2%, stirring while adding until mixing;

3) mixing 1, 3-butanediol and glycerol, and adding the microemulsion mixture of azelaic acid/azelaic acid clathrate and lavender essential oil; then mixing the mixture with the sodium hyaluronate mixed solution, and uniformly stirring the mixture to obtain a clear and transparent solution;

4) adding high-concentration xanthan gum solution to make the final concentration be 0.2%, uniformly stirring;

5) adding purified water to a desired volume, and stirring to obtain clear and transparent hyaluronic acid essence containing lavender essential oil and other composite plant extracts.

The three essences are subjected to bacteriostatic tests according to appendix C of GB15979-2002 hygienic Standard for Disposable sanitary articles, namely a product bactericidal performance, bacteriostatic performance and stability test method, wherein the acting strains are staphylococcus aureus (ATCC6538) and escherichia coli (ATCC25922), and the acting time is 1 hour and 5 hours. The results are shown in Table 3, where samples 1 and 2 are lavender essential oil essence containing azelaic acid inclusion compound, and the final concentration of azelaic acid corresponds to 0.25% and 0.5%, respectively; the control was a lavender essential oil serum containing 0.25% non-azelaic acid inclusion.

Table 3: comparison table of bacteriostatic effects of different concentrations of inclusion azelaic acid and essential oil microemulsion mixed solution

The results show that: the non-included azelaic acid in the control sample has 100% of bacteriostatic activity on escherichia coli and staphylococcus aureus within 1h, but the azelaic acid inclusion compound with different concentrations has 61% and 90.6% of bacteriostatic activity on staphylococcus aureus within 1h, and the azelaic acid inclusion compound with different concentrations is sensitive to escherichia coli, and the bacteriostatic activity of the azelaic acid inclusion compound with the concentration of 0.25% is only 94.3%; after 5 hours of action, the antibacterial activity of the azelaic acid inclusion compound with different concentrations reaches 100 percent. This result indicates that the inclusion azelaic acid has a significant slow release effect, which has a good effect of reducing the irritation of azelaic acid to skin. In the embodiment, the solubility of the water-insoluble raw material substances such as azelaic acid and the like in the water-soluble preparation is improved through the nano-encapsulation technology, more importantly, the irritation is reduced through the slow-release effect, and a solution strategy is provided for the application of the azelaic acid and other raw materials with irritation to the skin in the fields of cosmetics, medical care and the like.

Example 4 evaluation of skin feel of tea tree essential oil hyaluronic acid essence

In the embodiment, the tea essential oil hyaluronic acid essence is taken as an example for skin feel evaluation, and 10 persons in the age range of 16-50 years old are selected as male and female for evaluation, and the evaluation persons use the essence once in the morning and at night. The evaluation items include foamability, absorbency, sticky feeling, soft feeling, and presence or absence of odor, and the evaluation rules are as follows: the lathering, absorbency, stickiness and softness are given as scores, the score of 10 points is full, the lower the lathering and stickiness scores are, the better the skin feel is, and the higher the absorbency, moisturization and softness scores are, the better the skin feel is. The skin feel of different skin materials on different evaluation items and the use effect of the skin materials after being smeared for 28d are recorded. The results are shown in Table 4.

TABLE 4 evaluation of skin feel of tea tree essential oil hyaluronic acid essence

The results show that the subjects have high evaluation on the absorptivity, the moistening degree and the soft feeling of the tea tree essential oil hyaluronic acid essence prepared by the bacteriostatic repair combination formula, and no obvious uncomfortable feeling and sticky feeling exist in the wiping and coating process, so that the essence prepared by the combination formula is suitable for different skin types (except 1 female with serious red blood filaments and thin skin lipid layer) of different sexes, and is safe and non-irritant. The tea tree essential oil has no peculiar smell, which indicates that the auxiliary substances in the formula do not change the taste of the essential oil. After the essence is continuously used for 28 days, the acne quantity and the acne mark color of 1 teenager acne muscle are obviously improved, and the tea tree essential oil hyaluronic acid essence is proved to have obvious bacteriostatic acne-removing effect. The essential oil hyaluronic acid essence prepared by the antibacterial formula has good antibacterial repair effect and use experience, and is related to the fact that the combined formula contains hyaluronic acid with the functions of moisturizing and repairing, and substances such as witch hazel extract, dimethyl glycyrrhizinate and the like which have the functions of resisting inflammation, relieving the stress and regulating the oil balance, and meanwhile, the nano microcapsule emulsion wraps essential oil and oleanolic acid which possibly have irritation, so that the product is antibacterial and safe.

The above-described embodiments of the present invention do not limit the scope of the present invention. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the scope of the claims of the present invention.

Claims

1. A composition with bacteriostasis and repair functions is characterized by comprising plant essential oil with bacteriostasis, plant extracts, plant source bacteriostasis substances, sodium hyaluronate and other auxiliary substances.

2. The composition with bacteriostatic and repairing effects as claimed in claim 1, wherein the plant essential oil with bacteriostatic effect comprises one or more of tea tree essential oil, lavender essential oil, myrrh essential oil, lemongrass essential oil, permanent flower essential oil, clove essential oil, mint essential oil, etc., and the essential oil exists in the form of nano microcapsule emulsion and constitutes the microemulsion of essential oil, and the concentration of the essential oil is 0.1% -1%.

3. The composition with bacteriostasis and repair effects according to claim 1, wherein the plant-derived bacteriostasis substance is one or more of triterpenes, oleanolic acid, ursolic acid and other fruit acids, ferulic acid and azelaic acid, and is encapsulated by using a nano microemulsion microencapsulation technology to form a microemulsion or an inclusion compound, wherein the optimal concentration range is 0.1-1%.

4. The composition with antibacterial and repairing effects as claimed in claim 1, wherein the plant extract is a substance with antiinflammatory, sedative and/or astringent repairing effects, such as one or more of tea polyphenols, seaweed extract, hamamelis virginiana extract, centella asiatica extract, dipotassium glycyrrhizinate, chamomile extract, aloe extract, etc., and is used in an amount of 1% -10%.

5. The composition with bacteriostatic and repairing effects as claimed in claim 1, wherein the sodium hyaluronate comprises sodium hyaluronate with different molecular weights, the sodium hyaluronate is a mixture with a high molecular weight of more than 180 ten thousand daltons, a medium molecular weight of 100-.

6. The composition with bacteriostatic and repairing effects as claimed in claim 1, wherein the other auxiliary substances comprise low molecular alcohols, and are one or more of isopropanol, propylene glycol, glycerol, butanediol or pentanediol.

7. The composition with bacteriostatic and repairing effects as claimed in claim 1, wherein the other auxiliary substances further comprise an emulsion stabilizer which is one or more of carbomer, potassium alginate or xanthan gum.

8. The composition with bacteriostasis and repair effects as claimed in claim 2, wherein the essential oil micro emulsion comprises one or more of Tween series, span series, hydrogenated castor oil series and butanol polyether series as surface active substances.

9. A method for preparing essence from the composition with bacteriostatic and repairing effects according to any one of claims 1 to 8, which is characterized by comprising the following steps:

2) swelling sodium hyaluronate with different molecular weights uniformly, adding water-soluble plant extract while stirring until uniformly mixing;

3) mixing the microemulsion or the water-soluble inclusion compound prepared in the step 1) and the sodium hyaluronate solution prepared in the step 2), and uniformly stirring to obtain a clear and transparent solution. Then adding a proper amount of emulsion stabilizer, and uniformly stirring;

10. The composition with bacteriostatic and repairing effects as claimed in claims 1 to 8, which can be used for different cosmetic purposes, including but not limited to bacteriostatic, acne removing, speckle fading, anti-aging and the like; can be used in cosmetic preparations including but not limited to essence, facial mask liquid, toner, lotion and cream; can be used in the fields of medical care, medical and beauty and cosmetics.