WO2019233158A1

WO2019233158A1 - Traditional chinese medicine gel composition, preparation method and use thereof

Info

Publication number: WO2019233158A1
Application number: PCT/CN2019/078711
Authority: WO
Inventors: 徐丽华
Original assignee: 苏州思源天然产物研发有限公司
Priority date: 2018-06-08
Filing date: 2019-03-19
Publication date: 2019-12-12
Also published as: CN108743465A; JP2021527709A; JP7440931B2

Abstract

Provided is a gel composition comprising 30-95% by weight of a traditional Chinese medicine extract. The traditional Chinese medicine extract consists of a traditional Chinese medicine decoction extract liquid hydrosol and a clear paste made by purifying an extract liquid through a macroporous adsorption resin, 0.1-1% by weight of a surfactant, 0.5-3% by weight of a polymeric hydrogel, based on the weight of the gel composition. Also provided is a method of preparing the composition and a use thereof in preparing cosmetic products.

Description

Traditional Chinese medicine gel composition, preparation method and application thereof

(1) Technical field

The invention relates to the field of cosmetics, in particular to a traditional Chinese medicine gel composition, a preparation method thereof, and a mask prepared by using the gel composition.

(2) Background technology

In the field of cosmetics, the mask has always been a commonly used skin care product. In recent years, more and more users are accustomed to using the mask for beauty care. There are many types of disposable masks, which are usually applied before bedtime, which is more convenient and time-saving, and is popular. Among them, moisturizing and plant-based ingredients are more popular. At present, the beauty and beauty of traditional Chinese medicine is deeply rooted in people's hearts. People hope that the masks have the beauty effect of traditional Chinese medicine. However, existing masks containing traditional Chinese medicine are usually added with a small amount of extracts or original medicinal powder. The disposable cleansing mask usually has a single use amount of about 5g, and there are not many drugs or functional ingredients that can be carried. The traditional Chinese medicine mask produced in this way has a small amount of active ingredients and lacks significant effects.

Hydrogel, also known as hydrogel, is a hydrophilic network-like polymer swelling body that can swell in water, absorb and retain a large amount of water, but does not dissolve in water. It has solubility, syneresis, and permeability. Passive and sticky, it is a good drug carrier for slow release and transdermal absorption. Hydrogels are commonly used in the preparation of chemicals, and the drug loading is relatively large, up to about 5%. However, in the field of traditional Chinese medicine, due to its inaccurate preparation process and complex ingredients, there are many ingredients that can interfere with gel formation, especially a large number of acids and salts, which can cause interference with gel formation (see Research Progress in External Hydrogels, Gao Yan et al., Chinese Medicine Guide, Vol. 5, No. 11, November 2007, pages 0226-0228; the document mentioned [18] that the amount is only about 3-4%). At present, the contents of hydrogels of traditional Chinese medicines are relatively low. For example, Li Weize, et al. Research on industrial and industrial technology of Chinese medicine hydrogels and cataplasms, Chinese Journal of Herbal Medicine, Vol. 43, No. 10, October 2012, pages 1928-1933. Disclosed is a hydrogel with a bubbling agent whose content is 15%. However, the preparation is prepared as a dry powder and added with ceramic powder, a cross-linking agent, a cross-linking regulator and other ingredients. The manufacturing process requires equipment and control. Are both higher. Because it is prepared using dry powder instead of solution, the active ingredients cannot be fully dissolved and difficult to absorb; in addition, there are many powders and cross-linking agents, and the paste is opaque and sticky, which is not conducive to transdermal absorption. For another example, Li Yongxia et al., "Preparation Process of Compound Wuhuang Hydrogel", Chinese Pharmacist, Volume 14, Issue 2, 2011, pp. 192-193, and the obtained Wuhuang gel content is only 0.2%.

Therefore, in the field of cosmetics, there is still a need for a hydrogel capable of carrying a large amount of active ingredients of traditional Chinese medicine, so as to provide a more efficient, convenient, hygienic and safe traditional Chinese medicine beauty product.

(3) Content of the invention

Therefore, one aspect of the present invention provides a gel composition containing 30-98% by weight of a traditional Chinese medicine extract, wherein the traditional Chinese medicine extract is composed of a Chinese medicine decoction extract and essence The composition of the purified paste of the porous adsorption resin, and 0.1-1% by weight of a surfactant, and 0.5-3% by weight of a polymer hydrogel, based on the weight of the gel composition.

In one embodiment of this aspect, the traditional Chinese medicine comes from wild chrysanthemum, rose, white peony, angelica, safflower, ginseng, gardenia.

In another embodiment of this aspect, the polymer hydrogel is selected from the group consisting of carbomer, hypromellose, hydroxyethyl cellulose, and xanthan gum. Preferred polymer hydrogels are selected from hydroxyethyl cellulose, carbomer, and hypromellose.

In another embodiment of this aspect, the surfactant is selected from the group consisting of Tween, sodium lauryl sulfate, and lecithin. Preferred surfactants are selected from Tween and sodium dodecylsulfonate.

In yet another embodiment of this aspect, the composition may further contain cosmetically acceptable additives and carriers, which additives and carriers may be selected from humectants, fragrances, pigments, preservatives, excipients, foaming Agent, thickener, defoamer, etc., wherein the humectant may be glycerin, preferably glycerol is present at 1-10% by weight of the composition.

In another aspect of the present invention, a method for preparing a gel composition according to the present invention is provided, which includes the steps:

a) Mix the traditional Chinese medicine extract and surfactant and stir well;

b) Add polymer gel powder and stir well;

c) Swell for 2-20 hours and stir well;

d) the pH is adjusted to 5-7; and

e) Add glycerin and mix to form a gel.

In an embodiment of this aspect, before the preparation of the composition, the method further comprises the steps of extracting the Chinese medicinal material with 10-20 times the weight of water for 1-5 hours, and distilling and condensing to prepare the Chinese medicinal material essence.

In one embodiment of this aspect, the method further comprises the step of obtaining the ointment by distilling the remaining decoction, and the ointment is prepared by the following steps:

i) filtering the decoction, and the filtrate is adsorbed through the macroporous adsorption resin;

ii) elute with 50-95% ethanol to obtain an eluate;

iii) The ethanol in the eluate is recovered, concentrated and left to stand to obtain a supernatant, ie a cream.

In one embodiment of this aspect, the macroporous resin is preferably a styrene skeleton resin. Preferably it may be LSA-7, LSA-10, LSA-33, XDA-1, etc. of Xi'an Lanxiao Technology New Materials Co., Ltd.

In another aspect of the present invention, the use of the gel composition of the present invention is disclosed for the preparation of a cosmetic product, preferably selected from a facial mask, a face cream, an emulsion, a body milk, a hand mask, a foot mask, and the like.

(4) Specific embodiments

Through careful research, the applicant has discovered an effective method for preparing a highly loaded Chinese medicine gel composition. The method is easy to operate, has few auxiliary materials, high content of traditional Chinese medicine, and the formula contains more than 90% by weight of the traditional Chinese medicine solution and more than 30% by weight of the raw medicine. Each 10g mask is equivalent to 3-9g of traditional Chinese medicine, that is, about 10g per gel. It is equivalent to using 3-9g of traditional Chinese medicine. The gel composition can be made into a cosmetic composition for external use, such as a mask. Its advantages and improvements are:

(1) Safe dosage selection Within the usual dosage range of traditional Chinese medicine, the amount of raw medicine is related to the amount of mask, which can make users feel more secure. This gel is non-irritating and non-allergenic.

(2) Convenient production: The gel has simple ingredients, simple process and easy production. No simpler gel mask formula has been retrieved.

(3) High content of traditional Chinese medicines At present, there is no gel mask that can indicate the amount of traditional Chinese medicines contained, and the crude drug content is greater than 30%, and the traditional Chinese medicine liquid accounts for more than 90% by weight. Traditional Chinese medicine mask is added with a small amount of extract, not a complete Chinese medicine extraction.

As used in this specification and claims, the words "comprising" (and any form of "including" such as containing and containing), "having" (and any form of "having" such as "having" and "having" ), "Including" (and any form of "including" such as "enclosed" and "enclosed") or "containing" (and any form of "containing" such as "included" and "including") are included Being open or open does not exclude additional elements or method steps not mentioned. It is contemplated that any embodiment discussed in this specification can be implemented with any method or composition of the invention, and vice versa. In addition, the composition of the present invention can be used to implement the method of the present invention.

The "traditional Chinese medicine" described herein refers to any literature or record or a traditional Chinese medicine with cosmetic effects known from the prior art, which is derived from roses, wild chrysanthemums, gardenia, angelica, angelica, safflower, ginseng and the like. Those skilled in the art can understand that other Chinese medicinal materials can also be made into essences and creams by the methods described herein, and added to the gel composition, based on the contents of the present disclosure, especially the specific embodiments. For beauty products, Chinese herbal essential oils have the effect of moisturizing the skin, and at the same time need to retain effective ingredients to improve the texture of the skin. Therefore, combining ointments with essential oils as the active ingredients of traditional Chinese medicine in gel compositions, There are special benefits to making the most of it.

Wherein, the essence refers to an oil-water mixture collected by a steam distillation condenser, and the temperature range thereof may be 70-100 ° C; and the pressure range may be -0.01 to 0.01 MPa.

The ointment was purified and collected by filtration through a macroporous resin. The macroporous resin can be polar or non-polar. For example, LSA-7 can also use other conventional macroporous resins with a styrene skeleton, such as LSA-33, D101, LS-300, and the like. The washing of the macroporous resin removes organic acids, salts, and macromolecular impurities in the raw materials of traditional Chinese medicine, thereby enhancing gel stability and the ability to contain active ingredients therein.

For the safety of the user, the ingredients of all the compositions of the present invention are food additive grade.

The polymer hydrogel described herein is selected from carbomer, hypromellose, hydroxyethyl cellulose, xanthan gum, and the like. A "polymeric hydrogel" as used herein refers to a hydrogel polymer having a molecular weight greater than 10,000. Those skilled in the art will understand that other types of hydrogels with similar properties can also be used.

The surfactants described herein are conventional surfactants used in the field of cosmetics, such as Tween, sodium lauryl sulfate, lecithin, and the like. The content of surfactant is between 0.1-1%, so that as little surfactant as possible can form drug-containing micelles.

Additional cosmetically acceptable additives such as humectants, fragrances, colorants, preservatives, and the like can be added to the gel compositions described herein.

The gel composition described herein can be made into a facial mask, but also can be made into a cream, lotion, body product, and the like. Those skilled in the art will understand that the product can be made into various forms of facial mask components, such as paper facial masks, directly applied facial masks, disposable facial masks, and the like.

As a mask product, the mask of the present invention has the following characteristics:

(1) Good effect Because the traditional Chinese medicine is purified, the mask is transparent and moisturized, has a good feel and good appearance, can be enjoyed by users, and is easy to use, avoiding the rough sense of the traditional Chinese medicine mask.

(2) The formula is simple and scientific. It makes full use of the effects of traditional Chinese medicine ingredients. The essential oil penetrates and nourishes, and the water-soluble essence is locally recuperated. No artificially synthesized effective ingredients such as hormones and vitamins are added. In addition, because no bacterial nutritional ingredients are added, and the traditional Chinese medicine ingredients have natural antibacterial properties, no bacteriostatic and preservatives are added to the formula.

(3) Easy to use and apply directly after cleansing, no primer required. A single dose of about 5g, about 5 minutes to dry naturally, disposable. There is no need to use skin care products anymore. Essential oils and glycerin moisturize the gel. Take out with a small spoon and it will not pollute.

The invention is further described in the following examples, which do not limit the scope of the invention described in the claims.

Example 1: Formulation of a gel composition:

1. Source of raw materials

Glycerin (Malaysian Coconut Brand, Food Grade)

Wild chrysanthemum, white peony, rose (Luzhou Lijian Pharmaceutical Co., Ltd., complies with Pharmacopoeia standards)

Macroporous resins LSA-7, LSA-33, XDA-1 (Xi'an Lanxiao Technology New Materials Co., Ltd., food grade)

Carbomer (Qingdao Yiweikang Biotechnology Co., Ltd., pharmaceutical grade)

Tween 80 (Jiangsu Sixin Interface Agent Technology Co., Ltd., food grade)

Hydroxyethyl cellulose (Shenzhen Shenghai Biological Engineering Co., Ltd., food grade)

Hypromellose (Shenzhen Shenghai Biological Engineering Co., Ltd., food grade)

2. Formula:

(1) 100 parts of the essence of wild chrysanthemum (essence + clear cream) (medicine content 0.3g crude drug / ml), 1 part of carbomer powder, 0.6 part of Tween, 4 parts of glycerin (food additive).

The content of traditional Chinese medicine accounts for 32% by weight of the gel, that is, 3.2g of wild chrysanthemum ingredients are contained per 10g of the gel, and the essence accounts for 94% of the weight of the gel.

(2) 100 parts of rose essence (essence + clear cream) (medicine content 1.0g crude drug / ml), 1.5 parts of hypromellose powder, 0.2 parts of Tween and 2 parts of glycerin.

The content of traditional Chinese medicine accounts for 96% by weight of the gel, that is, 9.6g per 10g of the gel contains the rose component, and the essence accounts for 96% by weight of the gel.

(3) 100 parts of the essence of white peony (essence + clear cream) (medicine content 0.7g crude drug / ml), 2 parts of hydroxyethyl cellulose, 1 part of sodium lauryl sulfate, 6 parts of glycerin.

The content of traditional Chinese medicine accounts for 64% by weight of the gel, that is, 6.4g of paeony is contained per 10g of the gel, and the essence accounts for 92% of the weight of the gel.

3. Gel preparation process:

(1) Fry 60kg wild chrysanthemums in a multifunctional extraction tank, add 16 times the amount of water for 3 hours, and collect 120L of essence. The decoction extract is purified with a macroporous adsorption resin LSA-33 column, and concentrated to obtain a clear paste 60L. . Take 100 parts of the essence of Chinese medicine (fine dew + ointment, medicinal content 0.3 crude drug / ml), add 0.6 parts of Tween and mix well for 30 minutes, then add 1 part of carbomer powder, stir well, swell for 3 hours, stir to adjust the pH The value is 6, add 4 parts of glycerin, mix for 10 minutes to form a uniform gel, and aliquot it to obtain Example 1.

(2) 60 kg of roses are decoctioned in a multifunctional extraction tank for 3 hours, 14 times the amount of water is added, and 30 L of essence is collected. The decoction extract is purified with a macroporous resin XDA-10 column and concentrated to obtain 30 L of cream. Take 100 parts of the essence of Chinese medicine (fine dew + ointment, medicinal content 1.0 crude drug / ml), add 0.2 parts of Tween and mix well for 25 minutes, then add 2 parts of hypromellose powder, stir well, swell for 20 hours, stir Adjust the pH to 5, add 2 parts of glycerin, mix for 30 minutes to form a homogeneous gel, and dispense to obtain Example 2.

(3) 60 kg of white scallion was boiled and extracted in a multifunctional extraction tank for 3 hours, 12 times the amount of water was added, 30 L of essence was collected, and the decoction extract was purified with a macroporous adsorption resin LSA-7 column, and concentrated to obtain 60 L of cream. Take 100 parts of the essence of Chinese medicine (fine dew + ointment, medicinal content 0.7 crude drugs / ml), add 1 part of sodium lauryl sulfate and mix well for 20 minutes, then add 2 parts of hydroxyethyl cellulose powder, stir well and swell For 20 hours, stir to adjust the pH to 7, add 6 parts of glycerin, mix for 60 minutes to form a uniform gel, and distribute it to obtain Example 3.

4. Active ingredient detection

The pharmacopoeia law or national standard testing standards determined the active ingredients of the three formulas, and the results are as follows:

Determination of the effect of the gel composition of Example 2:

The preparation and use effects of the three samples of Examples 1, 2, and 3 were observed, and the results are as follows:

(1) Security

①Experiment of skin irritation in rabbits:

For the skin irritation test, 6 rabbits were selected, male and female, and the hair removal treatment was performed on the administration area 24 hours before the test, one on each side, and the hair removal range was 3cm × 3cm. The damaged skin group was marked with a "well" with a sterile syringe needle at the medication site, with the degree of bleeding as the degree. Apply 0.5ml of medicine on the left hair removal site, and apply the same amount of excipients on the right. The mask is applied to the skin for 14 consecutive days, and the volume is 0.5 g / piece. Carefully observe whether there is erythema and edema at the application site and 1 h after each application, and score it. Observe it continuously for 3 days after the last application . The test results found that the gel compositions of the three examples were all non-irritating.

Multiple sexual stimulation tests on rabbits

The experimental results show that the mean value of the irritant response score to rabbits is zero.

② Guinea pig skin irritation experiment:

Fifty guinea pigs were selected. The guinea pigs were randomly divided into 5 groups. The auxiliary control group was given a blank preparation, the test group was given a mask, and the positive control group was given 2-mercaptobenzothiazole. Each group had 10 animals. The skin and hair on both sides of the back of the guinea pig are shaved 24 hours before the administration. The area of the hair removal area is about 3cm × 3cm. During the sensitization period, the test article or reference substance is evenly applied to the left hair removal site. The test article is then removed with water; when the test phase is administered, the test article or reference substance is evenly applied to the right shaving site, and it is fixed by a suitable method. After 6 hours of application, the test article is removed with water. Animals in each group were sensitized and administered 3 times, with administration every 7 days or so. Dosed once during the challenge phase. The method of administration is skin application, and the dosage is 0.2 g / animal. Generally, skin erythema, edema and other abnormal reactions are observed at 1h and 24h after sensitization and at 24h and 48h after challenge. Erythema and edema are scored according to the corresponding standards, and the sensitization effect of the test substance and blank is judged according to the scoring standards. The test results showed that all the gel compositions of the three examples showed no allergies.

Guinea pig skin allergy test erythema integral value and incidence of allergic reactions

Experimental results prove that these gel compositions are also non-irritating to guinea pigs.

(2) Microbiological test results:

Bacterial testing was performed in accordance with the Standard Test Method for Cosmetic Microorganisms (GB7918.1-5). The products of the three examples were all sterile.

Microbiological indicators and test results

(3) Trial effect of gel composition

Each of the three example formulas was tried by 20 people (female, average age 30 years), and applied after cleansing at night, once every 2 days, a total of 5 results are as follows:

Example effect

In summary, the gel composition prepared by the method and composition of the present invention has a high load of active ingredients of traditional Chinese medicine, is safe and hygienic, and has a good user experience.

The above disclosure is provided to illustrate rather than limit the scope of the invention. Variations of the invention will be apparent to those of ordinary skill in the art and are included in the appended claims. All publications, databases, web resources, patents, patent applications, and registration numbers cited herein are incorporated by reference for all purposes.

Claims

A gel composition, characterized in that the gel composition contains 30-95% by weight of a Chinese medicine extract, and the Chinese medicine extract is purified from a Chinese medicine decoction extract essence and an extract solution through a macroporous adsorption resin The composition of the ointment, 0.1-1% by weight of a surfactant, and 0.5-3% by weight of a polymer hydrogel, based on the weight of the gel composition.
The gel composition according to claim 1, wherein the traditional Chinese medicine is selected from the group consisting of wild chrysanthemum, rose, gardenia, white peony, angelica, safflower, and ginseng.
The gel composition according to claim 1, wherein the polymer hydrogel is selected from the group consisting of carbomer, hypromellose, hydroxyethyl cellulose, and xanthan gum.
The gel composition according to claim 1, wherein the surfactant is selected from the group consisting of Tween, sodium lauryl sulfate, and lecithin.
The gel composition of claim 1, further comprising a cosmetically acceptable additive and a carrier.
A method for preparing a gel composition according to claim 1, comprising the steps of:

a) Mix the traditional Chinese medicine extract and surfactant and stir well;

b) Add polymer gel powder and stir well;

c) Swell for 2-20 hours and stir well;

d) the pH is adjusted to 5-7;

e) Add glycerin and mix to form a gel.
The method according to claim 6, further comprising the steps of extracting the Chinese medicinal material with 10-20 times the weight of water for 1-5 hours, and distilling and condensing to prepare the Chinese medicinal material essence before preparing the composition.
The method according to claim 7, further comprising the step of obtaining an ointment by distilling the remaining decoction, said ointment being prepared by the following steps:

i) filtering the decoction, and the filtrate is adsorbed through the macroporous adsorption resin;

ii) elute with 50-95% ethanol to obtain an eluate;

iii) The ethanol in the eluate is recovered, concentrated and left to stand to obtain a supernatant, ie a cream.
The method according to claim 6, wherein the macroporous resin is a styrene skeleton resin.
The use of the gel composition according to claim 1, wherein the gel composition is used for preparing a cosmetic product.