CN114796076A - An anti-allergy composition containing Scutellariae radix extract and its preparation method - Google Patents

An anti-allergy composition containing Scutellariae radix extract and its preparation method Download PDF

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CN114796076A
CN114796076A CN202210525546.3A CN202210525546A CN114796076A CN 114796076 A CN114796076 A CN 114796076A CN 202210525546 A CN202210525546 A CN 202210525546A CN 114796076 A CN114796076 A CN 114796076A
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scutellaria baicalensis
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孟悠恺
赵振
马烨
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Nanjing Yiweisen Biotechnology Co ltd
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    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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Abstract

The invention discloses an anti-allergy composition containing scutellaria baicalensis extract and a preparation method thereof. The composition comprises scutellaria baicalensis extract, oat bran extract, an antioxidant, a pH value regulator, polyhydric alcohol, deionized water and the like. The stability of the scutellaria baicalensis extract in the cosmetics is improved, the phenomena of deep color and strong smell change of the cosmetics in the storage process after the scutellaria baicalensis extract is added are improved, and the shelf life of the cosmetics product after the scutellaria baicalensis extract is added can be prolonged. Improves the anti-inflammatory and anti-allergic effects of the scutellaria baicalensis extract, and can reduce the addition amount of the scutellaria baicalensis extract in a cosmetic formula.

Description

An anti-allergy composition containing Scutellariae radix extract and its preparation method
Technical Field
The invention relates to a technology for improving stability and anti-allergic effect of a traditional Chinese medicine extract, belonging to the field of medicines and cosmetics.
Background
The traditional Chinese medicine cosmetics are cosmetics with traditional Chinese characteristics, and active ingredients extracted from Chinese herbal medicines are added into the cosmetics, so that the requirements of people on the efficacy of the cosmetics can be met, and the safety of the sources of the raw materials of the cosmetics can be improved.
The traditional Chinese medicine scutellaria is the root of a herbal plant scutellaria in the family of labiatae, is a commonly used medicine for treating skin diseases in traditional Chinese medicine, has a long medicinal history in China, is recorded in Shen nong's herbal Jing, and is mainly used for treating various fever jaundice, diarrhea, bleeding block, gangrene of skin and ulcer, and the application history can be traced back to two thousand years ago. Because of releasing lung fire and relieving muscle heat, the medicine can treat skin sores and rashes, such as acne, rosacea, psoriasis, black speck, dermatitis and the like, and achieve the effects of removing damp-heat, clearing blood toxin and moistening skin through the efficacies of releasing fire, clearing heat, drying dampness and the like (Shen Yinjun, Chinese medicine pharmacology [ M ]. Beijing: people's health publishing house, 2000.).
Baicalin (Baicalin) is one of effective components of Scutellaria baicalensis Georgi of Labiatae, is a flavonoid inducer, has remarkable biological activity including antiinflammatory, immunity regulating, antiallergic, antitumor, antibacterial, antivirus, and blood pressure lowering effects, and has especially outstanding antiinflammatory and immunity regulating effects. Baicalin shows clear anti-inflammatory and immune modulating effects in a variety of animal models of inflammation and autoimmunity, including: asthma, acute pancreatitis, acute lung injury, hepatic fibrosis, dermatitis solaris, etc. (Zhang Xingchen, extraction and purification process of baicalin in scutellaria baicalensis and antioxidation research thereof [ D ] Lanzhou university of physiology and chemistry, 2012).
In the baicalin stability study of billows, Zhanying et al, it is shown that baicalin is extremely unstable in an alkaline solution, and the stability is also reduced when the pH value is more than 3, so that the pH value of baicalin in the extraction and preparation production is controlled to be 3-4 without considering other factors. However, the pH value of the resident cosmetic is kept between 5.5 and 7.5, so that the physiological function of the skin is not affected. Therefore, the scutellaria baicalensis extract is often subjected to undesirable phenomena such as oxidative failure and the like in conventional cosmetics.
In addition, in our research, the dosage of the scutellaria baicalensis extracting solution is found to have a great influence on the stability of the emulsion. The emulsion added with the scutellaria baicalensis extracting solution has layering phenomenon after 24 hours of heat resistance and cold resistance test, and the color of the product is yellow. It is possible that the emulsion has a limited ability to tolerate ions, and when it exceeds a certain amount, it will affect the stability of the product and cause delamination (lixinen, a multi-effect study of the traditional Chinese medicine scutellaria in cosmetics and its safety evaluation [ M ]. guangdong university of medical science, 2016).
Disclosure of Invention
The invention aims to solve the problems that the stability of the effective component baicalin in the scutellaria baicalensis extract in a cosmetic system is poor, and the product quality is influenced; the scutellaria baicalensis extract with too high conductivity can damage an emulsion system of the emulsion, and the stability of the product is influenced and the phenomenon of emulsion breaking and layering occurs if the conductivity exceeds a certain amount; the application range of the scutellaria baicalensis in the field of cosmetics is expanded, and the efficacy value of components such as baicalin is guaranteed.
In order to solve the problems, the invention adopts the following scheme: an anti-allergy composition containing a scutellaria baicalensis extract is characterized by comprising 2.0-10.0% of a scutellaria baicalensis ethanol extract, 1.0-3.0% of an antioxidant, 20.0-30.0% of deionized water, 2.0-10.0% of an oat bran ethanol extract and 50.0-70.0% of a polyhydric alcohol.
A method for preparing an anti-allergy composition containing a scutellaria baicalensis extract is characterized by comprising the following steps:
(1) cleaning Scutellariae radix, drying, and pulverizing to obtain Scutellariae radix micropowder;
(2) mixing the scutellaria baicalensis superfine powder with an ethanol water solution with the ethanol concentration of 40-60% according to the mass ratio of 1:10, and performing ultrasonic extraction for 40-60 minutes to obtain a scutellaria baicalensis extracting solution;
(3) purifying the Scutellariae radix extractive solution with AB-8 macroporous resin column, concentrating, and drying to obtain Scutellariae radix extract;
(3) mixing Scutellariae radix extract, antioxidant and deionized water at a mass ratio of 5:1:20, and heating in a water bath to dissolve;
(4) dissolving oat bran ethanol extract with the same mass as that of the scutellaria baicalensis extract in 10 times of polyol with the mass of the oat bran ethanol extract at the temperature of 55 ℃;
(5) heating the solution in (3) to 55 deg.C, slowly stirring, and dissolving in (4) to obtain Scutellariae radix extract composition, i.e. antiallergic composition; and then adding a pH value regulator to regulate the pH value of the scutellaria baicalensis extract composition to be 5.5-6.5.
Further, the preparation method of the anti-allergy composition containing the scutellaria baicalensis extract is characterized in that the antioxidant is one or more of sodium metabisulfite, carnosine, ascorbic acid, BHA, BHT and propyl gallate, and the addition amount of the antioxidant is 1.0-5.0% of the total mass of the scutellaria baicalensis extract composition.
Further, the preparation method of the anti-allergy composition containing the scutellaria baicalensis extract is characterized in that the pH value regulator comprises one or more of citric acid, ascorbic acid, triethanolamine and sodium hydroxide.
Further, the preparation method of the anti-allergy composition containing the scutellaria baicalensis extract is characterized in that the polyalcohol is 1, 3-butanediol.
An anti-allergy composition containing Scutellariae radix extract is used in preparing cosmetic.
The invention has the following technical effects: after the scutellaria baicalensis extract is purified by an AB-8 macroporous resin column, the conductivity of the scutellaria baicalensis extract solution is reduced, and the influence of the scutellaria baicalensis extract solution on the stability of the emulsion is reduced. After the baicalin is combined with the antioxidant, the oat bran extract, the polyalcohol and the pH value regulator, the stability of the baicalin in the solution can be obviously improved, the baicalin content does not change greatly after the baicalin is stored for one year at room temperature in a dark place, and the baicalin is easy to store and transport. After the scutellaria baicalensis extract and the oat bran extract are combined, the synergistic effect is realized on the aspects of anti-inflammation and anti-allergy, and the soothing and anti-allergy capability is improved while the dosage is reduced.
Drawings
FIG. 1 shows the results of hyaluronidase inhibition in vitro.
FIG. 2 initial allergic reaction in the arm of the volunteer.
FIG. 3 comparative picture after 2h of applying 3% composition emulsion to volunteers (right side at the place where the emulsion is applied).
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
Example 1
1 preparation of Scutellaria baicalensis Georgi extract
The scutellaria baicalensis is cleaned, dried and crushed to prepare the scutellaria baicalensis submicron powder. Mixing the scutellaria baicalensis ultra-fine powder with an ethanol water solution with the ethanol concentration of 40% -60% according to the mass ratio of 1:10, and carrying out ultrasonic extraction for 40-60 minutes to obtain a scutellaria baicalensis extracting solution. Recovering ethanol from Scutellariae radix extractive solution, purifying with AB-8 macroporous resin column, desalting, concentrating, and drying to obtain Scutellariae radix extract.
2 preparation of the composition
Dissolving Scutellariae radix extract five parts in deionized water twenty parts, and adding antioxidant one part. Five parts of oat bran extract were dissolved in fifty parts of polyol at 55 ℃. Mixing the two solutions, and adjusting the pH value to be 5.5-6.5. Wherein the antioxidant is selected from sodium pyrosulfite, ascorbic acid and carnosine, the polyalcohol is selected from 1, 3-butanediol, and the pH value regulator is selected from ascorbic acid and triethanolamine.
3 composition stability study method and results
30mL of the analyte was added to each of the clean and dry centrifuge tubes 4. Respectively placing into a freezing chamber of a refrigerator at minus 15 ℃, a thermostat at 40 ℃ and a direct sunlight place, and keeping out of the sun at room temperature. Taking out every 7 days, 14 days, 21 days and 28 days, and observing whether the phenomena of layering, precipitation, color deepening, odor change, pH value change and the like occur after the sample is recovered to the normal temperature.
First, stability of a single extract of scutellaria baicalensis was tested in a solution, and the extract of scutellaria baicalensis was formulated into a 0.05g/mL solution and subjected to a stability test. Table 1 shows the stability test results of a single scutellaria baicalensis extract, which may be caused by the oxidation of baicalin in the scutellaria baicalensis extract in the solution.
In order to improve the stability of the scutellaria baicalensis extract, an antioxidant is required to prevent the oxidation of the baicalin. Table 2 shows the stability test results of 0.1% sodium metabisulfite added to 0.05g/mL of the Scutellariae radix extract solution, and the test results show that the stability of the Scutellariae radix extract solution is improved by adding sodium metabisulfite. Baicalin is not easily oxidized under acidic condition, and in order to prevent baicalin from being oxidized in the preparation process of the composition, antioxidant ascorbic acid is added to reduce the pH value and further prevent baicalin from being oxidized. Table 3 shows the stability test results after 0.1% of each of sodium metabisulfite and ascorbic acid was added to 0.05g/mL of the Scutellariae radix extract solution, and the test results show that the stability is further improved.
Carnosine has good antioxidant effect, and can be synergistically acted with sodium metabisulfite to enhance the antioxidant effect. Table 4 shows the results of stability tests after 0.1% of each of sodium metabisulfite, ascorbic acid and carnosine was added to 0.05g/mL of the Scutellariae radix extract solution.
The results show that the sodium pyrosulfite, the ascorbic acid and the carnosine can synergistically enhance the stability of the scutellaria baicalensis extract, and the cold and hot stability of the composition does not obviously change in four-week experiments.
Table 1, stability test record of scutellaria baicalensis extract.
Storage conditions Whether it is stable for 7 days Whether it is stable for 14 days Whether it is stable for 21 days Whether it is stable for 28 days
Minus 15 deg.C Is that Is that Whether or not Whether or not
40℃ Whether or not Whether or not Whether or not Whether or not
Illumination of light Whether or not Whether or not Whether or not Whether or not
At normal temperature Whether or not Whether or not Whether or not Whether or not
Table 2. stability test record of combination of scutellaria baicalensis extract and sodium metabisulfite.
Storage conditions Whether it is stable for 7 days Whether it is stable for 14 days Whether it is stable for 21 days Whether it is stable for 28 days
Minus 15 deg.C Is that Is that Is that Is that
40℃ Is that Is that Whether or not Whether or not
Illumination of light Is that Whether or not Whether or not Whether or not
At normal temperature Is that Is that Is that Is that
Table 3, scutellaria baicalensis extract, sodium metabisulfite, ascorbic acid, combination stability test record.
Storage conditions Whether it is stable for 7 days Whether it is stable for 14 days Whether it is stable for 21 days Whether or not it is stable for 28 days
Minus 15 deg.C Is that Is that Is that Is that
40℃ Is that Is that Is that Whether or not
Illumination of light Is that Is that Whether or not Whether or not
At normal temperature Is that Is that Is that Is that
Table 4, scutellaria baicalensis extract, sodium metabisulfite, ascorbic acid, carnosine combination stability test record.
Storage conditions Whether or not it is stable for 7 days Whether or not it is stable for 14 days Whether it is stable for 21 days Whether it is stable for 28 days
Minus 15 deg.C Is that Is that Is that Is that
40℃ Is that Is that Is that Is that
Illumination of light Is that Is that Whether or not Whether or not
At normal temperature Is that Is that Is that Is that
4 composition inhibition of Hyaluronidase Activity
Taking 0.1mL of CaCl2 solution (0.25mmol/L) and 0.5mL of hyaluronidase solution (100U/mL) to perform water bath constant temperature culture at 37 ℃ for 20 min; adding 0.5mL of sample solution to be tested, and keeping the temperature for 20 min; adding 0.5mL sodium hyaluronate solution (0.5mg/mL), culturing in water bath at 37 deg.C for 30min, taking out, and standing at room temperature for 5 min; adding 0.1mL of NaOH solution (0.4mol/L) and 0.5mL of acetylacetone solution (3.5mL of acetylacetone dissolved in 50mL of 1.0mol/L sodium carbonate solution), heating in a boiling water bath for 15min, and immediately transferring to an ice water bath to cool for 5 min; 1.0mL of an Ellisib reagent (0.8g p-dimethylaminobenzaldehyde dissolved in 15mL concentrated hydrochloric acid and 15mL absolute ethanol) was added dropwise and diluted with 3.0mL absolute ethanol, and the mixture was left at room temperature for 20min for color development and measured for absorbance at a wavelength of 540nm with a spectrophotometer. The calculation formula of the sample for measuring the hyaluronidase inhibition rate is as follows:
hyaluronidase inhibition rate ═ [ (a-B) - (C-D) ]%/(a-B).
Wherein A is the absorbance value of the control solution (the sample solution is replaced by acetic acid buffer solution); b-control blank solution absorbance value (the sample solution and enzyme solution are replaced by acetic acid buffer solution); c is the absorbance value of the sample solution; d-absorbance value of sample blank solution (replacing enzyme solution with acetic acid buffer solution).
The scutellaria baicalensis extract, the oat bran extract, the scutellaria baicalensis extract and the oat bran extract 1:1 are respectively prepared into solutions with different concentrations of 0.1% -1.0%, and the solutions are used as sample solutions to carry out hyaluronidase in-vitro inhibition rate test determination.
FIG. 1 shows the results of hyaluronidase inhibition in vitro. The experimental result shows that the hyaluronidase inhibition rate is improved along with the increase of concentration, when the concentration of the scutellaria baicalensis extract is 1%, the inhibition rate can reach 78.4%, and the half inhibition concentration is 0.567%; when the concentration of the oat bran extract is 1%, the inhibition rate can reach 77.8%, and the half inhibition concentration is 0.483%; when the concentration of the composition is 1%, the inhibition rate can reach 84.5%, and the half inhibition concentration is 0.308%. The experimental result can show that when the oat bran extract and the scutellaria baicalensis extract are combined in a ratio of 1:1, the hyaluronidase inhibition rate is obviously improved, and the median inhibition concentration is obviously reduced. The combination of the scutellaria extract and the oat bran extract has the advantages of improved anti-allergic effect and reduced dosage.
5 the composition is formulated into cream and has antihistaminic effect
The compositions were formulated into creams, table 5 for the test cream formulations, and the creams were prepared according to the following formulations for the antihistaminic sensitization test.
Table 5 test cream formulations
Figure BDA0003642374310000061
Figure BDA0003642374310000071
Find 10 well-conditioned volunteers, numbered from 1 to 10. Cleaning the inner side of the arm, smearing 1% histamine solution after 15 minutes, and waiting for the occurrence of positive reaction, (-) represents negative, shows no reaction, (+ -) represents suspicious positive, shows only mild erythema, (+) represents weak positive, shows erythema and infiltration, can have a small amount of papules, (++) represents medium positive, shows erythema, infiltration, papules, blisters and (+ ++) represents strong positive, and shows erythema, infiltration, papules and bulla. Then, the right half of the medial side of the arm was smeared with cream, and the skin conditions at 0.5h, 1h, 1.5h, 2h, 2.5h, 3h, 3.5h, and 4h were observed and recorded.
TABLE 6 record of the experiment with 3% composition addition
Numbering Number 1 Number 2 No. 3 Number 4 Number 5 Number 6 No. 7 Number 8 Number 9 Number 10
Initiation of (++) (++) (++) (++) (++) (++) (++) (++) (++) (++)
0.5h (++) (++) (++) (++) (++) (++) (++) (++) (++) (++)
1h (+) (++) (+) (+) (+) (+) (+) (++) (+) (+)
1.5h (+) (+) (+) (+) (+) (+) (+) (+) (±) (+)
2h (±) (±) (±) (±) (±) (±) (±) (±) (±) (+)
2.5h (±) (±) (±) (±) (±) (±) (±) (±) (±) (±)
3h (-) (±) (-) (-) (±) (-) (±) (±) (-) (±)
3.5h (-) (-) (-) (-) (-) (-) (-) (-) (-) (±)
4h (-) (-) (-) (-) (-) (-) (-) (-) (-) (-)
As can be seen from the data in Table 6, when the addition amount of the composition is 3%, the effect of the composition on the skin of a volunteer can be obviously red-removing and relieving effect, and the composition can rapidly remove red and relieve itching within 0.5-2 h. Fig. 2 is the initial allergic reaction of arm of volunteer, and fig. 3 is the comparative picture of volunteer after applying 3% composition emulsion for 2h (right side is the place where cream is applied).

Claims (6)

1. An anti-allergy composition containing a scutellaria baicalensis extract is characterized by comprising 2.0-10.0% of a scutellaria baicalensis ethanol extract, 1.0-3.0% of an antioxidant, 20.0-30.0% of deionized water, 2.0-10.0% of an oat bran ethanol extract and 50.0-70.0% of a polyhydric alcohol.
2. A method for preparing an anti-allergy composition containing a scutellaria baicalensis extract is characterized by comprising the following steps:
(1) cleaning Scutellariae radix, drying, and pulverizing to obtain Scutellariae radix micropowder;
(2) mixing the scutellaria baicalensis superfine powder with an ethanol water solution with the ethanol concentration of 40-60% according to the mass ratio of 1:10, and performing ultrasonic extraction for 40-60 minutes to obtain a scutellaria baicalensis extracting solution;
(3) purifying the Scutellariae radix extractive solution with AB-8 macroporous resin column, concentrating, and drying to obtain Scutellariae radix extract;
(3) mixing the scutellaria baicalensis extract, the antioxidant and deionized water according to the mass ratio of 5:1:20, and heating and dissolving in a water bath kettle;
(4) dissolving oat bran ethanol extract with the same mass as that of the scutellaria baicalensis extract in 10 times of polyol with the mass of the oat bran ethanol extract at the temperature of 55 ℃;
(5) heating the solution in (3) to 55 deg.C, slowly stirring, and dissolving in (4) to obtain Scutellariae radix extract composition, i.e. antiallergic composition; and then adding a pH value regulator to regulate the pH value of the scutellaria baicalensis extract composition to be 5.5-6.5.
3. The method of claim 2, wherein the antioxidant is one or more of sodium metabisulfite, carnosine, ascorbic acid, BHA, BHT, and propyl gallate, and is added in an amount of 1.0-5.0% of the total weight of the Scutellariae radix extract composition.
4. The method of claim 2, wherein the pH regulator comprises one or more of citric acid, ascorbic acid, triethanolamine, and sodium hydroxide.
5. The method of claim 2, wherein the polyhydric alcohol is 1, 3-butylene glycol.
6. An anti-allergy composition comprising the extract of scutellaria baicalensis as claimed in claim 1, for use in the preparation of cosmetics.
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CN110200830A (en) * 2019-05-23 2019-09-06 广州科斯曼生物科技有限公司 A kind of anti-inflammatory Shu Min remediation composition and its preparation method and application
CN113143833A (en) * 2021-04-30 2021-07-23 中国医学科学院北京协和医院 Skin care product and preparation method thereof
CN113616801A (en) * 2021-08-10 2021-11-09 南京益唯森生物科技有限公司 Preparation method and application of antiseptic and antibacterial preparation containing Scutellariae radix extract
CN114469828A (en) * 2022-02-17 2022-05-13 广州合众无纺化妆品集团有限公司 Amber congee and preparation method thereof

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