CN108653133A - A kind of preparation method of the anti-oxidant gelling agent of Maize silk flavones - Google Patents

Abstract

The invention discloses the Maize silk flavones gelling agents with antioxidant activity, including following parts by weight of component：Acritamer 940, glycerine, propylene glycol, appropriate triethanolamine, main ingredient Maize silk flavones powder and salicylic acid.Maize silk flavones have effects that anti-oxidant, anti-inflammatory, whitening, restraining and sterilizing bacteria in the present invention；According to 2015 editions《Chinese Pharmacopoeia》With 2007 editions《China cosmetic hygienic practice》, comprehensive research and evaluation have been carried out to Maize silk flavones cosmetics crude drug quality, extraction process, moulding process, quality standard, release in vitro and transdermal, stability and flavones antioxidant activity；Preparation process of the present invention is simple, and property is stablized, quality controllable, and the nonirritant daily chemical products that are suitable for are develop and useedd.

Description

A kind of preparation method of corn silk flavone antioxidant gel

technical field

The invention relates to cosmetics, in particular to a preparation method of corn silk flavone antioxidant gel.

Background technique

Cosmeceuticals with natural active ingredients have the characteristics of low skin irritation, good permeability, high safety index, and high efficiency, and are increasingly favored by consumers. Therefore, cosmeceuticals with natural active ingredients have great market potential , will be the mainstream of the development of the world cosmetics industry.

Corn silk flavonoids are one of the important active ingredients in corn silk stigmas, which have the functions of antibacterial, anti-inflammatory, blood lipid lowering, and free radical scavenging. Corn silk flavonoids have anti-oxidation, anti-radiation, whitening, moisturizing and other functions on the skin; With the continuous deepening of people's research on natural cosmetics, the functions of corn silk flavonoids are more and more recognized and applied by people; in this patent, corn silk flavonoids are applied to gels to make corn silk flavonoids anti-oxidation gel Gel cosmetics, functional cosmeceutical products with anti-acne, anti-oxidation, and skin-whitening effects. It is suitable for the treatment of mild and moderate acne patients. It is safe and effective for long-term use, reduces the occurrence of skin problems, and keeps the skin healthy and moisturized.

The local effect of salicylic acid is keratolysis, which is used as a keratin softener, and its pharmacological effects vary depending on the concentration of the preparation; 1% to 3% have keratinization promoting and antipruritic effects; 5% to 10% have keratolytic effects , can also produce antifungal effect (because the cuticle is removed to inhibit fungal growth, this product can help other antifungal drugs penetrate and inhibit bacterial growth); salicylic acid acts on the hair follicle wall cells and can help remove blocked hair Hair follicles, restore the normal shedding of cells, the most effective for blackheads, it can also change the abnormal shedding of hair follicle walls, and prevent the generation of new lesions.

The body produces various free radicals during the metabolic process, such as hydroxyl free radicals, superoxide anion free radicals and lipid free radicals; the important cause of skin aging is the increase of free radicals in the skin, which damages the biofilm and also causes some hydrolytic enzymes to Released from the cells, the collagen fibers and elastic fibers in the epidermis are cross-linked, brittle, denatured and lose elasticity, making the stratum corneum of the skin thicker, and finally making the skin rough, loose and wrinkled. Corn silk flavonoids can capture and neutralize free radicals, thereby eliminating the damage caused by free radicals to the human body, delaying skin aging, maintaining skin elasticity and smoothness, and finally showing the effect of anti-oxidation.

The present invention conducts comprehensive research and evaluation on the quality, extraction process, molding process, quality standard, in vitro release and skin penetration, stability and flavonoid antioxidant activity of corn silk flavonoid antioxidant gel cosmetic raw materials.

The present invention uses corn silk flavone powder, salicylic acid, carbomer-940, glycerin, propylene glycol, and triethanolamine as raw materials, and on the basis of base materials, the production of corn silk flavone antioxidant gel is determined through orthogonal experiments technology, has anti-oxidation effect, and has bactericidal, anti-inflammatory, and whitening effects. There is no report about corn silk flavonoid anti-oxidation gel and its preparation method. This patent has certain significance for meeting the needs of the cosmetics market.

Contents of the invention

The purpose of the present invention is to overcome the deficiencies of the prior art, to provide a corn silk flavone antioxidant gel; the product has anti-oxidation, anti-acne functional cosmeceutical products; suitable for sensitive, dry and For damaged skin with neutral skin problems, and for the treatment of patients with mild acne, it is safe and effective for long-term use, reduces the occurrence of skin problems, and keeps the skin healthy and moisturized.

Another object of the present invention is to provide a preparation method of the above-mentioned gel.

The technical scheme adopted in the present invention:

A corn silk flavone antioxidant gel is prepared from carbomer-940, glycerin, propylene glycol L, triethanolamine, salicylic acid, corn silk flavonoid powder and deionized water; The component content is carbomer-9401~5%, glycerin 10~40%, propylene glycol 10~40%, triethanolamine amount, main drug corn silk flavonoid powder 3~6%, salicylic acid 1~4% and deionized Water 40~60%.

A kind of preparation method of above-mentioned gel:

(1) Extraction of corn silk flavonoids: Take 50 g of corn silk powder in a beaker; add 600 mL of 75% ethanol solution (corn silk: ethanol = 1:6, V/V), ultrasonicate for 30 min; The corn silk ethanol solution was vacuum filtered, and the filtrate was stored. The residue was mixed with 75% ethanol at a volume ratio of 1:5, and ultrasonicated twice for 30 min; The volume ratio of 4, ultrasonic for 30 min three times, the filtrate obtained three times combined in a rotary evaporator at 45 ° C, concentrated at a speed of 40 rpm; stop concentrating when the concentrated liquid appears wall-hanging phenomenon, and transfer the obtained concentrated liquid to Place in a beaker in a water bath at 45°C, and after 2 to 3 days, vacuum-dry to obtain the total flavonoid extract, and store in a refrigerator at 4°C to prevent deterioration. Precisely weigh 2.5 g of corn silk total flavonoids powder, add 20 mL of purified water to ultrasonically dissolve, filter, concentrate the filtrate to 1/5 volume, decolorize the filtrate with diatomaceous earth, add petroleum ether and chloroform for overnight extraction to remove alkaloids and interfere with the interference of lipids, and then use ethyl acetate to extract the obtained filtrate to obtain a relatively pure flavonoid solution, which is dried into powder;

(2) Preparation of corn silk flavonoid antioxidant gel: Weigh 10 g of glycerin, evenly sprinkle 1 g of carbomer on the surface and fully infiltrate, add 10-15 mL of purified water, stir well and place overnight to make it fully Swell, add 1.35g of triethanolamine dropwise to form a transparent gel matrix, and set aside; accurately weigh 2.5 g of purified corn silk flavonoid powder, add 20mL of purified water to dissolve it ultrasonically, and filter to obtain a corn silk preparation solution for use; take another 60 mesh sieve Add 1.5 g of salicylic acid into the mixture of propylene glycol and ethanol to dissolve the salicylic acid preparation solution, and slowly add the two medicinal solutions (corn silk preparation solution and salicylic acid preparation solution) into the gel matrix under the condition of water bath at 40 °C During the process, stir while adding, add dropwise triethanolamine to adjust the pH to 6.0-7.0, add water to a sufficient amount, and stir well. The above corn silk flavonoid antioxidant gel and its preparation method have reasonable design, simple preparation process, stable properties, controllable quality, no irritation and are suitable for the development and utilization of daily chemical products.

Detailed ways:

The present invention will be further described below in conjunction with specific examples.

Embodiment 1: extraction, purification and assay of corn silk flavonoids

Extraction and purification of corn silk flavonoids: Take 50 g of corn silk powder in a beaker; add 600 mL of 75% ethanol solution (corn silk: ethanol = 1:6, V/V), and ultrasonically treat in an ultrasonic cleaner for 30 min; The corn silk ethanol solution after ultrasonic treatment was vacuum filtered, and the filtrate was stored. The residue was mixed with 75% ethanol at a volume ratio of 1:5, and ultrasonicated twice for 30 min; With a volume ratio of 1:4, three times of sonication for 30 min were performed, and the filtrate obtained three times was stored in a flask. The obtained extract was placed in a 45°C water bath, and after 2-3 days, vacuum-dried to obtain the total flavonoid extract, which was stored in a 4°C refrigerator to prevent deterioration. Precisely weigh 2.5 g of corn silk total flavonoids powder, add 20 mL of purified water to ultrasonically dissolve, filter, concentrate the filtrate to 1/5 volume, decolorize the filtrate with diatomaceous earth, add petroleum ether and chloroform for overnight extraction to remove alkaloids and interfere with the interference of lipids, and then use ethyl acetate to extract the obtained filtrate to obtain a relatively pure flavonoid solution, which is dried into powder.

Qualitative test of flavonoids: In this experiment, HCl-Zn powder reaction and aluminum chloride reaction are used to identify flavonoids in corn silk. Hydrochloric acid-zinc powder reaction: take 1mL of sample ethanol solution, add a little zinc powder (magnesium powder) and shake , then add a few drops of concentrated hydrochloric acid, and develop color within 1-2 minutes (heating if necessary); aluminum chloride reaction: take 1 mL of sample in ethanol solution, add 1% aluminum trichloride methanol solution, and develop color;

Determination of flavonoids content in corn silk: According to literature review, the total flavonoids have the maximum absorption value at a wavelength of 510 nm. Take the flavonoid extract, dilute 2 mL of the extract to a 10 mL colorimetric tube with 60% ethanol to the mark, then dilute 5 times. Take 4 portions of 1 mL of the diluted solution and place them in a 10 mL colorimetric tube, one of which was dilute with 60% ethanol as a reference solution. Add 0.3 mL of 5% sodium nitrite solution to each of the remaining parts, shake well, stand for 6 min, add 0.3 mL of 10% aluminum nitrate solution, shake well, stand for 6 min, add 4 mL of 1 mol sodium hydroxide solution, and then wash with 60% ethanol The solution was diluted to the mark, and after standing for 15 min, the absorbance was measured at 510 nm. Concentration data can be obtained from the standard curve regression equation (with rutin as a reference), and the average value of the three results is 0.01mg/mL. After conversion, the flavonoid content in the sample was 4~6mg/g.

Embodiment 2: the preparation of gel

Determination of gel matrix factors and levels: according to the pre-test situation, it is determined that the investigation factors are the amount of carbomer (A), the amount of glycerin (B), the amount of propylene glycol (C), and each factor arranges 3 levels for optimization. See Table 1 for the horizontal arrangement;

Table 1 Single factor level design table for gel matrix preparation factor Carbomer A (g/g) Glycerol B(g/g) Propylene Glycol C(mL/g) 1 1 5 5 2 1.5 10 10 3 2 15 15

(1) Screening of gel matrix formula: with the determined 3 factors and 3 levels, 9 samples were prepared according to the design of the L9(3^3) orthogonal table, packed in airtight plastic boxes, and stored at room temperature, 55 ℃ and - Place at 15°C for 1 day. Observe the color, clarity, spreadability, stability, viscosity, etc. of the sample, and make a comprehensive score based on it as an investigation standard. The satisfactory value of each index is 10 points (full score is 10 points), and the others range from 0 to 10 points. The results are shown in Table 2;

Table 2 Orthogonal experiment scheme and results of gel matrix Test No. A B C room temperature 55°C -15°C total score 1 1 1 1 5 4 4 13.5 2 1 2 2 8.5 8 7 2.5 3 1 3 3 6 4 4 4 4 2 1 2 7 8 9 twenty four 5 2 2 3 4 4 4 12 6 2 3 1 4 4 3 11 7 3 1 3 5 4 3.5 12.5 8 3 2 1 8 7 6 twenty one 9 3 3 2 4 4 3.5 11.5 K1 50.5 49.5 45 K2 47 56.5 58.5 K3 15 12.2 12.5 R 1.8 3.4 7

From the results in Table 2, it can be seen that factor C has the most significant influence on the matrix formulation, followed by factor B, and factor A again (Rc > Rb > Ra). The optimal matrix condition determined by the average value of K is A ₃ B ₃ C ₂ , namely Carbomer 1 g, glycerin 10 g, propylene glycol 10 mL;

(2) Determination of the dosage of penetration enhancer: due to corn silk flavonoids as the main ingredient, according to the different concentrations of menthol, multiple groups of formulas are designed

recipe one

Corn silk flavonoids 2.5g; salicylic acid 1.5g; carbomer 1g; glycerin 10g; propylene glycol 10mL; ethanol 10mL; menthol 0.75g; triethanolamine 1.35g;

recipe two

Corn silk flavonoids 2.5g; salicylic acid 1.5g; carbomer 1g; glycerin 10g; propylene glycol 10mL; ethanol 10mL; menthol 1.0g; triethanolamine 1.35g;

Recipe three

Corn silk flavonoids 2.5g; salicylic acid 1.5g; carbomer 1g; glycerin 10g; propylene glycol 10mL; ethanol 10mL; menthol 1.25g; triethanolamine 1.35g;

Preparation of Corn Silk Flavone Antioxidant Gel

Weigh glycerin, sprinkle carbomer evenly on the surface and fully infiltrate it, add appropriate amount of purified water, stir well and leave overnight to make it fully swell, add triethanolamine dropwise to form a transparent gel matrix, and set aside. Accurately weigh the purified corn silk flavonoid powder, add appropriate amount of purified water to dissolve it ultrasonically, and filter to obtain the corn silk preparation solution for later use; add salicylic acid passed through a 60-mesh sieve into a mixture of propylene glycol and ethanol for dissolution to obtain salicylic acid Acid preparation solution; slowly add two kinds of medicinal solutions (corn silk preparation solution and salicylic acid preparation solution) into the gel matrix under the condition of 40 ℃ water bath, stir while adding, adjust the pH to 6.0-7.0, add water to a sufficient amount , Stir well to get the finished product.

Embodiment 3: the quality control of main raw material of corn silk flavone antioxidant gel

Physical and chemical identification of salicylic acid: FeCl ₃ chromogenic method: take the dilute solution of the test product, add 1 drop of ferric chloride test solution, and it will appear purple;

Content determination: determine that the maximum absorption wavelength of salicylic acid is 298 nm, accurately weigh 100 mg of salicylic acid reference substance placed in a desiccator for 24 h, put it in a 100 mL volumetric flask, dissolve with an appropriate amount of ethanol, add purified water to the mark, Shake well. Accurately draw 0.3, 0.6, 0.9, 1.2, 1.5, 1.8, 2.1, 2.4, 2.7 mL of the above solutions respectively, put them in a 100 mL volumetric flask, add purified water to the mark in sequence, and shake well. Using purified water as a blank, measure the absorbance at 298nm, and perform linear regression on the concentration C with the absorbance A to obtain the linear regression equation of salicylic acid: Y=0.2537C+0.024, r = 0.9999 (n= 9), the result It shows that in the range of 3-21mg/L salicylic acid, the absorbance A has a good linear relationship with the concentration C;

Flavonoid identification and containing test are the same as [0016], [0017];

pH check: Take three samples from the three batches of corn silk flavonoid antioxidant gel finished product for testing, take about 1.0 g gel for each sample, put a small amount of distilled water in a 10 mL beaker, stir and transfer to a 10 mL capacity In the bottle, add an appropriate amount of distilled water, sonicate for 20 minutes, let it cool down, make up to volume, centrifuge and filter, take the filtrate to measure the pH value, the pH value of the three batches of small test samples is in the range of 6.75~6.97, so the pH value of this product is tentatively determined 6.8±0.2;

Microbiological limit inspection: Take about 1.0 g of the finished samples of three batches of corn silk flavonoid antioxidant gel, and check according to the method under the microbial limit inspection item of "China Hygienic Standards for Cosmetics" 2007 edition. See Table 3, and the results are all in compliance with the regulations;

Table 3 Microbial inspection project index protein type normal type baked type The total number of colonies, each/g ≤30000 ≤1000 ≤1000 Coliform bacteria, individual/100g ≤90 ≤40 ≤40 Pathogenic bacteria, individual/g ≤50 pathogenic bacteria Not allowed to check out

Viscosity check: Take 10.0 g to 50 mL of corn silk flavonoids antioxidant gel into a measuring bottle, add water to dissolve, shake well, add water to the mark, ultrasonic degassing, use a Ping's viscometer with a capillary inner diameter of 1.0 mm, according to " Chinese Pharmacopoeia 2015 Edition Appendix VIG Method 1 was used to determine the kinematic viscosity of 3 batches at 20 °C. The results are shown in Table 4. According to the test results of the 3 batches and the general requirements of the gel, the kinematic viscosity of this product should be 10-100 mm ² /s;

Table 4 Viscosity check batch number 20140510 20140511 20140512 Viscosity (mm ² /s) 39.8 40.1 40.3

Centrifugal experiment: Take 1.0 g of corn silk flavone antioxidant gel and put it in a centrifuge tube, and centrifuge at 4000 r/min for 15 min. As a result, all the samples were uniform and delicate, and no delamination was observed. Prove that the prepared corn silk flavone antioxidant gel is stable;

Stability test: According to the test results, the gel produced according to the screened prescription and process is tested under strong light irradiation test, high temperature, high humidity and low temperature test under the conditions of commercially available packaging, and the properties, content, and related parameters of the gel are determined. The substances had no significant change, and the related substances of the gel in the high temperature test increased slightly, suggesting that the gel should be stored under high temperature conditions. The above test results show that the prescription, production process and packaging material selection of this gel are reasonable, and the gel is packaged above market requirements, and the product is stable.

Transdermal test

Preparation of isolated mouse skin

The mice (20±5) g were divided into 6 groups, with 4 mice in each group. The abdominal skin of the mice was depilated with a depilatory agent, sacrificed, peeled off the abdominal skin, removed the subcutaneous fat, washed repeatedly with purified water, and refrigerated in normal saline for later use;

Transdermal test method

Using a rotating membrane diffusion device, the Pharmacopoeia dissolution cup is used as the receiving chamber, the supply chamber is connected to the rotating rod, and the diffusion port is at the bottom of the supply chamber; 1 g of corn silk flavonoid antioxidant gel is evenly coated in the rotating basket, and the in vitro The mouse skin is fixed at the lower end of the rotating basket, and the cuticle is in close contact with the test solution facing the supply chamber, and penetrates 3.15 cm2. The receiving tank was filled with 50 mL of normal saline, containing 10% PEG 400 and 2 d drops of oleic acid, and stirred at a constant temperature of (37±1)°C and 100 r·min-1. At intervals of 1, 3, 5, 7, and 9 hours, take 2 mL of the receiving solution (while supplementing 2 mL of the medium solution), add 6 mL of absolute ethanol, shake well, and measure the absorbance value at 284 nm; operate in the same way as the blank reference substance , the results obtained were blank-corrected, and the cumulative infiltration Q and the infiltration multiple Er were calculated with formula 1; the results are shown in Table 5;

Q=[2×∑Ci+V×Cn] /SEr=K/K0 Formula 1

Q: Cumulative infiltration amount; S: Infiltration area; V: Receiving tank volume; Er: Infiltration multiple; K: Infiltration rate after infiltration; K0: Infiltration rate without infiltration; Ci: From the first time to the last sampling Accept the drug concentration in the pool; Cn: accept the drug concentration in the pool when sampling this time;

Table 5 Effects of corn silk flavonoids compound salicylic acid gel containing different concentrations on transdermal cumulative penetration ( mg··cm- 2, n = 3) flavonoid content 1 hour 3 hours 5h 7h 9h Er 0.0% 0.0501 0.7106 0.4302 1.0763 1.2795 1.5% 0.0254 1.1623 1.4877 1.9320 2.0832 1.63 2.0% 0.1198 1.1419 1.6136 2.3937 2.1593 1.69 2.5% 0.2278 1.4859 2.0789 2.7650 3.1123 2.43

According to the statistical test, corn silk flavonoids antioxidant gels containing different concentrations of corn silk flavonoids all have a strong penetration-promoting effect ( P < 0.05), and 2.5% corn silk flavonoids has a significant difference on salicylic acid ( P < 0.01).

Embodiment 5: skin irritation/corrosion test of corn silk flavone antioxidant gel

Acute skin irritation test procedure

About 24 hours before the test, the hair on both sides of the back and spine of the experimental animals was cut off without damaging the epidermis. Take about 0.5 mL (g) of the test substance and apply it directly on the skin, then cover it with two layers of gauze (2.5 cm × 2.5 cm) and a layer of cellophane or similar, and then fix it with non-irritating adhesive tape and bandage. The skin on the other side served as a control. The closed test was adopted, and the application time was 4 h. For cosmetic products, the application time can be extended or shortened according to the actual use of the person and the type of product. For cosmetic products that are rinsed off after use, only the 2-hour application test is used. After the test, remove the residual test substance with warm water or non-irritating solvent. If it is suspected that the test substance may cause severe irritation or corrosion, a segmented test can be adopted, and three gauze pieces coated with the test substance are applied to the skin of a rabbit's back hair removal area at the same time or successively. After 3 minutes, 60 minutes and 4 hours, remove a piece of gauze, and the test can be stopped if corrosion occurs at any time point on the skin application site. Observe the skin reaction at the application site at 1, 24, 48 and 72 hours after the test substance is removed, score the skin reaction according to Table 6, and conduct a comprehensive evaluation based on the average value of the points of the tested animals. According to Table 3, determine the intensity of skin irritation according to the highest integral mean value of time. The determination of the observation time should be sufficient to observe the whole process of reversible or irreversible stimulation, generally not exceeding 14 days;

Multiple skin irritation test procedure

Before the test, the hair on both sides of the back and spine of the experimental animals was cut off. The range of hair removal was 3 cm×3 cm, and the smear area was 2.5 cm×2.5 cm. Take about 0.5 mL (g) of the test substance and smear it on one side of the skin. When the test substance is prepared with a non-irritating solvent, apply the solvent on the other side as a control, and apply it once a day for 14 consecutive days. From the next day, the hair should be clipped before each application, and the residual test substance should be removed with water or non-irritating solvent. Observe the result one hour later, score according to Table 6, and treat the control area and the test area in the same way

Calculate the average score of each animal per day according to the following formula, and use Table 7 to determine the intensity of skin irritation

Average score per animal per day = erythema and edema score / number of animals tested / 14

Table 6 Irritation score skin reaction integral Erythema and eschar formation no erythema 0 Slight erythema (barely visible) 1 obvious erythema 2 moderate to severe erythema 3 Severe erythema (purple) to mild eschar formation 4 Edema formation no edema 0 Slight edema (barely visible) 1 Mild edema (well-defined skin bumps) 2 Moderate edema (skin swelling about 1mm) 3 Severe edema (skin bulge of more than 1mm, expanding in scope) 4

Table 7 Irritation levels integral mean strength 0~＜0.5 non-irritating 0.5~＜2.0 Mild irritation 2.0~＜6.0 Moderate irritation 6.0～8.0 strong stimulus

Table 8 Stimulus levels animal number 1h 24h 48 hours 72h erythema edema total score erythema edema total score erythema edema total score erythema edema 1 0 0 0 0.5 0.1 0.6 0.5 0 0.5 0.3 0 2 0 0 0 0.5 0.1 0.6 0.5 0 0.5 0.3 0 3 0 0 0 0.5 0 0.5 0.5 0.1 0.6 0.2 0.1 4 0.5 0.5 1 0.5 0.1 0.6 0.5 0.1 0.6 0.1 0.1

Total score mean 0.11

Stimulus intensity classification Non-irritating

Corn silk flavonoids anti-oxidant gel is a gel type cosmetic, using carbomer-940 as the base of the gel, with corn silk flavonoids and salicylic acid as the main components, with anti-oxidation and anti-acne functions Cosmeceutical products. It is suitable for the treatment of mild and moderate acne patients. It is safe and effective for long-term use, reduces the occurrence of skin problems, and keeps the skin healthy and moisturized.

Embodiment 4: in vitro antioxidant activity test of corn silk flavone antioxidant gel

Sample pretreatment: Precisely weigh corn silk flavone antioxidant gels of different qualities, dissolve them in methanol and dilute to different concentrations, mix them with ultrasonic waves, centrifuge, and take the supernatant to obtain sample solutions.

Total reducing power method: Take 2.5 mL of phosphate buffer solution (pH6.6 0.2 mol/L) in a test tube, add 0.3 mL of sample solutions of different concentrations (0.07, 0.14, 0.21, 0.28, 0.35 mg/mL) and mix well Then add 1ml of potassium ferricyanide, put it in a water bath at 50°C for 20 minutes, add 1 mL of 10% trichloroacetic acid after cooling, and mix well. Take 2.5 mL of supernatant, add 2.5 mL of distilled water and 0.5 mL of 0.1% ferric chloride, and measure the absorbance at 700 nm after reacting for 5 min. VC was used as a control.

DPPH free radical removal method:

Take 2ml of sample solutions with different mass concentrations of 0.5mg/ml, 1.0mg/ml, 1.5mg/ml, 2.0mg/ml, and 2.5mg/ml, and add an equal volume of DPPH solution with a concentration of 0.1mmol/l (with anhydrous prepared with ethanol), mixed well and reacted in the dark at room temperature for 30 min. Absorbance Ai was measured at 517nm, and 4ml of absolute ethanol and distilled water (2ml of both) were used as blank for zero adjustment. The blank control group is 2ml of sample solution plus 2ml of absolute ethanol, and its absorbance value at 517nm is Aj. The purpose of setting the blank control group is to remove the absorbance value of the flavonoid sample itself. The model control group was 2ml DPPH solution plus 2ml absolute ethanol, and its absorbance value at 517nm was Ao. Take the average value of 3 parallel determinations, and calculate the clearance rate according to the formula: clearance rate (%)=[1-(Ai-Aj)/Ao]×100%.

Eliminate ABTS free radical method:

Mix equal volumes of 7 mmol/L ABTS and 2.45 mmol/L K2S2O8 solution, and place in the dark at room temperature for 12 h to obtain the ABTS stock solution. Dilute with absolute ethanol so that the absorbance range is 2.000±0.100 to obtain ABTS+ detection solution. Take 11 colorimetric tubes and divide them into groups to be tested: 3.00 mL ABTS+ detection solution and samples with different mass concentrations of 0.05mg/ml, 0.10mg/ml, 0.25mg/ml, 0.5mg/ml and 1mg/ml Control group: use 95% ethanol instead of ABTS+ detection solution, blank group: use 95% ethanol instead of corn silk flavonoids test solution, mix each group, let stand at room temperature for 6 minutes, use absolute ethanol to zero, and quickly The absorbance was measured 3 times in parallel at a wavelength of 734 nm, and the average value was taken. Calculate according to the following formula: clearance rate=[1-(A to be tested-A control)/A blank]×100%.

Results: As shown in Figures 1, 2, and 3 of the specification, the corn silk flavone antioxidant gel has the ability to reduce iron ions, and can inhibit free radicals from transferring electrons, so that free radicals can be transformed into relatively stable products to terminate the series of free radical reactions , and its reducing ability increases with the increase of concentration. At the same concentration, the absorbance value of corn silk flavone antioxidant gel was slightly lower than VC, and the results showed that corn silk flavonoid antioxidant gel had strong antioxidant capacity, but lower than VC.

Description of the drawings: Figure 1 The reducing ability of corn silk flavonoids antioxidant gel to Fe3+, Figure 2 The scavenging ability of corn silk flavonoids antioxidant gel to DPPH free radicals, Figure 3 The corn silk flavonoids antioxidant gel to ABTS Free radical scavenging ability.

Claims (5)

1. A corn silk flavonoid antioxidant gel, by weight percentage, the raw materials are composed of: the gel matrix prescription is carbomer-940 1 ~ 4%, glycerol 10 ~ 40%, propylene glycol by orthogonal test screening 10~40%, appropriate amount of triethanolamine; purified corn silk flavonoids powder 3~6%, salicylic acid 1~4%; The preparation method comprises the following steps: (1) Extraction, decolorization and purification of corn silk flavonoids: Take 50 g of corn silk powder in a beaker; add 600 mL of 75% ethanol solution (corn silk: ethanol = 1:6, V/V), and ultrasonicate for 30 min; Vacuum filter the corn silk ethanol solution after sonication, store the filtrate, and mix the residue with 75% ethanol at a volume ratio of 1:5, sonicate twice for 30 min; vacuum filter, combine the filtrate, and mix the residue with 75% ethanol The solution was ultrasonicated three times for 30 min at a volume ratio of 1:4, and the filtrates obtained three times were combined in a rotary evaporator at 45°C and concentrated at a speed of 40 rpm; when the concentrated solution appeared to hang on the wall, it stopped, and the obtained concentrated The solution was transferred to an evaporating dish, placed in a water bath at 45 °C, and after 2 to 3 days, vacuum-dried to obtain the total flavonoids extract, which was stored in a refrigerator at 4 °C to prevent deterioration; 2.5 g of corn silk total flavonoids powder was precisely weighed, Add 20mL of purified water for ultrasonic dissolution, filter, concentrate the filtrate to 1/5 volume, decolorize the filtrate with diatomaceous earth, add petroleum ether and chloroform for overnight extraction to remove the interference of alkaloids and interfering lipids, and then use acetic acid Ethyl ester extracts the filtrate obtained above to obtain a relatively pure flavonoid solution, which is dried to powder; (2) Preparation of corn silk flavonoid antioxidant gel: Weigh 10 g of glycerin, evenly sprinkle 1 g of carbomer on the surface to fully infiltrate, add 10-15 mL of appropriate amount of purified water, stir well and leave overnight to make it fully Swell, add 1.35g of triethanolamine dropwise to form a transparent gel matrix, and set aside; accurately weigh the purified corn silk flavonoid powder, add an appropriate amount of purified water to ultrasonically dissolve, filter to obtain a corn silk preparation, and set aside; Another 1.5 g of salicylic acid passed through a 60-mesh sieve was added to a mixture of propylene glycol and ethanol to dissolve to obtain a salicylic acid preparation solution, and the two medicinal solutions (corn silk preparation solution and salicylic acid preparation solution) were mixed in a water bath at 40 °C. ) into the gel matrix slowly, stirring while adding, dropwise adding triethanolamine to adjust the pH to 6.0-7.0, adding water to a sufficient amount, and stirring well. 2. the preparation, decolouring and purification of corn silk flavonoids according to claim 1: corn silk adopts the ultrasonic extraction method to select 75% ethanol solution respectively according to corn silk: ethanol=1:6,1:5,1:4 Ratio of solid to liquid: Ultrasonic treatment in an ultrasonic cleaner three times for 30 minutes each time; store the filtrate obtained three times in a flask to obtain an extract at 45 °C and concentrate in a rotary evaporator at a speed of 40 rpm until the concentrated solution appears to hang on the wall After the phenomenon occurs, stop the concentration, transfer the obtained concentrated solution into a beaker, place it in a water bath at 45°C, and after 2~3 days, vacuum-dry it to obtain the total flavonoid extract, and store it in a refrigerator at 4°C to prevent deterioration; weigh it accurately Total flavonoids powder of corn silk, add purified water to ultrasonically dissolve, filter, the volume of the filtrate is concentrated to 1/5 volume, the filtrate is decolorized with diatomaceous earth, and petroleum ether and chloroform are added for overnight extraction to remove the interference of alkaloids and interfering lipids function, and then extract the filtrate obtained above with ethyl acetate to obtain a relatively pure flavonoid solution, which is dried to powder. 3. the corn silk flavonoids antioxidant gel according to claim 1, is characterized in that this product is every 100 g salicylic acid range 1 ~ 4g, the corn silk flavone after purification 3 ~ 6g; Generally speaking, 1 g cal About 1.35 g of triethanolamine is needed for carbomer, and the final mass fraction of carbomer should be controlled to be ≤0.8% when blended with skin care products. 4. The corn silk flavone antioxidant gel according to claim 1, characterized in that the pH value of this product is 6-8, the kinematic viscosity of this product should be 10-100 mm2/s, and the total integral mean value of skin irritation level 0.11. 5. The corn silk flavone antioxidant gel according to claim 1, the preparation has high antioxidant biological activity, good spreadability, simple preparation process, stable properties, controllable quality, and meets the characteristics and requirements of the gel .