A method for preparing plant polysaccharides and antioxidant composition thereof by high pressure microfluidization

Abstract

The present application relates to a kind of plant polysaccharide and its antioxidant composition prepared by high pressure microjet, belong to cosmetic technical field.The antioxidant composition includes 22-36 parts of red pine pine nut shell polysaccharide, 15-25 parts of resveratrol solution, 10-20 parts of anti-oxygen complex solution, 1.5-3.5 parts of ubiquinone, 10-20 parts of dextran, 1.8-3.2 parts of sodium hyaluronate and 40-60 parts of deionized water by weight.The red pine pine nut shell polysaccharide and resveratrol solution in it can form complex, the components in anti-oxygen complex solution mutually synergistic improve the antioxidant capacity of whole system, the combination of ubiquinone, dextran and sodium hyaluronate also helps to maintain skin problem, promote the transdermal absorption of other active ingredients, each component is complementary, can effectively eliminate free radical, stable, mild effect on skin, play antioxidant effect.

Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of cosmetics, and relates to a plant polysaccharide and an antioxidant composition thereof prepared by high-pressure microjet. BACKGROUND

[0002] With the improvement of living standards and the enhancement of skin care awareness, consumers' demand for cosmetics and quality requirements are continuously increasing. Skin, as a barrier directly contacting the outside world of the human body, is crucial to maintaining the body's homeostasis. However, with the increase of age and the stimulation of diverse external environment, the ability of the human body's antioxidant system gradually decreases, leading to the generation of active oxygen free radicals, which triggers skin inflammation, dryness, relaxation and other problems, and accelerates skin aging. Therefore, antioxidant products have become an important choice for consumers to pursue skin rejuvenation and health.

[0003] Traditional antioxidant cosmetics mainly improve the antioxidant effect by adding a large amount of antioxidant ingredients, but these ingredients are easily affected by conditions such as light and temperature, leading to a decrease in activity. In addition, the use of multiple antioxidant ingredients can increase the burden on the skin, limiting the skin's utilization rate. Plant polysaccharides, as a natural high-molecular compound, have rich biological activities, including antioxidant, anti-inflammatory, immune regulation, etc. However, traditional plant polysaccharide extraction methods have certain limitations, such as low extraction rate, destruction of active ingredients, etc., and repeated extraction will increase the cost of enterprises.

[0004] High-pressure microjet technology, as a new type of material processing technology, has the characteristics of high efficiency and environmental protection. It realizes the refinement, mixing and homogenization of materials by high pressure through a small channel, thereby improving the bioavailability and stability of the materials. How to apply high-pressure microjet technology to the preparation process to obtain antioxidant products with better antioxidant effect is a direction of current research. SUMMARY

[0005] The purpose of the present application is to provide a plant polysaccharide and an antioxidant composition thereof prepared by high-pressure microjet, which fully extracts the effective components inside the polysaccharide by a series of processing methods such as high-pressure microjet, and the components complement each other and synergistically enhance each other, which can effectively scavenge free radicals, stably and gently act on the skin, and play an antioxidant effect.

[0006] The purpose of the present application can be achieved by the following technical solutions:

[0007] A plant polysaccharide and an antioxidant composition thereof prepared by high-pressure microjet, the antioxidant composition comprising, by weight, 22-36 parts of red pine pine nut shell polysaccharide, 15-25 parts of white resveratrol solution, 10-20 parts of antioxidant composite solution, 1.5-3.5 parts of ubiquinone, 10-20 parts of dextran, 1.8-3.2 parts of sodium hyaluronate, and 40-60 parts of deionized water.

[0008] Further, the preparation method of the Korean pine nut shell polysaccharide comprises the following steps:

[0009] (1) The Korean pine nut shell is dried in a 65℃ drying box, crushed and sieved through a 60-80 mesh sieve to obtain Korean pine nut shell powder;

[0010] (2) The Korean pine nut shell powder, cellulase, pepsin and deionized water are mixed in a mass ratio of 1:0.026-0.034:0.017-0.023:20-30, shaken uniformly, and then set to a water bath temperature of 60-70℃, extracted in a water bath for 4-5h, treated with high-pressure microjet 3 times, centrifuged, and the supernatant is taken, concentrated by rotary evaporation to 1 / 3 of the original volume to obtain a crude Korean pine nut shell polysaccharide extract;

[0011] (3) The crude Korean pine nut shell polysaccharide extract and 70-80% ethanol solution are mixed in a mass ratio of 1:15-25, shaken uniformly, and then placed at 4℃ for 12-24h, centrifuged, and ultrafiltered to obtain a Korean pine nut shell polysaccharide solution;

[0012] (4) The Korean pine nut shell polysaccharide solution is passed through a D101 macroporous resin, set to an elution speed of 1.5-2.5BV / h, and sequentially eluted with 3 times the volume of the resin column of deionized water, 2 times the volume of the resin column of 50-60wt% ethanol solution and 1.5 times the volume of the resin column of 30-40wt% ethanol solution, the ethanol solution is collected and dried to obtain a Korean pine nut shell polysaccharide.

[0013] Further, the parameters of the high-pressure microjet treatment in step (2) are: treatment pressure of 100-140MPa and treatment flow rate of 50-150mL / min.

[0014] Further, the centrifugation parameters in step (2) are: centrifugation temperature of 4℃, centrifugation speed of 6000-8000rmp and centrifugation time of 10-20min.

[0015] Further, the centrifugation parameters in step (3) are: centrifugation temperature of 4℃, centrifugation speed of 10000-12000rmp and centrifugation time of 10-20min.

[0016] Further, the ultrafiltration in step (3) uses an ultrafiltration membrane with a molecular weight cut-off of 6-12KD.

[0017] Further, the preparation method of the resveratrol solution is:

[0018] Mix 6-12 parts by weight of resveratrol, 10-20 parts by weight of 70-80% ethanol solution and 5-10 parts by weight of Tween-80, set the ultrasonic frequency to 300-500 W and the ultrasonic temperature to 40-50 DEG C, and ultrasonic treat for 10-30 min to obtain a resveratrol solution.

[0019] Further, the preparation method of the antioxidant composite solution is:

[0020] Mix 1.5-2.5 parts by weight of lipoic acid, 6.2-8.4 parts by weight of vitamin C, 1.8-4.2 parts by weight of vitamin E, 5-10 parts by weight of Tween-80 and 15-25 parts by weight of deionized water, dropwise add citric acid to adjust the pH to 6.2-6.8, and stir at a speed of 80-280 rpm for 20-40 min to obtain an antioxidant composite solution.

[0021] Further, the preparation method of the antioxidant composite solution is:

[0022] Set the temperature of a reaction kettle to 30-40 DEG C, mix red pine nut shell chitin and deionized water, then add the resveratrol solution, dropwise add citric acid to adjust the pH to 6-7, stir at a speed of 80-100 rpm for 20-30 min, and then sequentially add the antioxidant composite solution, ubiquinone, dextran and sodium hyaluronate, and stir at a speed of 100-300 rpm for 1-2 h to obtain an antioxidant composition.

[0023] The present application has the following advantages:

[0024] The hydroxyl groups on the red pine nut shell chitin molecules form hydrogen bonds with the phenolic hydroxyl groups of resveratrol in the resveratrol solution, the benzene ring structure of resveratrol has hydrophobicity, and the hydrophobic parts of the red pine nut shell chitin are attracted to each other through hydrophobic interaction, thereby promoting the formation of a complex of the red pine nut shell chitin and resveratrol, and the presence of the complex can reduce the oxidative damage of the red pine nut shell chitin, thereby synergistically enhancing the overall antioxidant capacity and stability.

[0025] The vitamin C in the antioxidant composite solution has reducing property, can directly scavenge free radicals, and can regenerate oxidized vitamin E, and the vitamin E is a fat-soluble antioxidant, can protect the cell membrane from damage by free radicals, and the addition of Tween-80 can improve the dispersibility of vitamin E in water by forming micelles to wrap the vitamin E; the lipoic acid has amphiphilicity and antioxidant property, and the conjugate base thereof has very high negative reducing potential, can be used as a stabilizer for the vitamin C and vitamin E, and synergistically enhances the overall antioxidant capacity of the system.

[0026] The ubiquinone has certain anti-inflammatory properties, the antioxidant properties of the ubiquinone and the sodium hyaluronate help the skin resist damage from free radicals, the moisturizing effect of the sodium hyaluronate and the dextran forms a protective film on the skin surface, meanwhile, the porous structure of the sodium hyaluronate and the dextran helps the transdermal absorption of other active ingredients, the three synergistically work together to help maintain skin homeostasis, relieve the stimulation of antioxidant components and the external environment on the skin, so as to achieve a mild and effective antioxidant effect.

[0027] The red pine pine nut shell polysaccharide, the resveratrol solution, the antioxidant composite solution, the ubiquinone, the dextran and the sodium hyaluronate of the present application synergistically work together, so that the antioxidant composition can stably and mildly act on the skin and jointly play an antioxidant effect. DETAILED DESCRIPTION

[0028] In order to further illustrate the technical means and effects adopted by the present application to achieve the predetermined purposes, the specific embodiments, structures, features and effects according to the present application are described in detail below in combination with examples.

[0029] Example 1

[0030] A plant polysaccharide and an antioxidant composition thereof are prepared by using high-pressure microjet, the antioxidant composition of the present example comprises 22 parts of red pine pine nut shell polysaccharide, 15 parts of resveratrol solution, 10 parts of antioxidant composite solution, 1.5 parts of ubiquinone, 10 parts of dextran, 1.8 parts of sodium hyaluronate and 40 parts of deionized water by weight.

[0031] The preparation method of the red pine pine nut shell polysaccharide of the present example comprises the following steps:

[0032] (1) The red pine pine nut shell is dried in a 65℃ drying box, crushed and then passed through a 60-mesh sieve to obtain red pine pine nut shell powder;

[0033] (2) The red pine pine nut shell powder, cellulase, pepsin and deionized water are mixed in a mass ratio of 1:0.026:0.017:20, shaken uniformly, the temperature of the water bath is set to 60℃, and then extracted by water bath for 4h, followed by high-pressure microjet treatment for 3 times, centrifugation, taking the supernatant, rotary evaporation to concentrate to 1 / 3 of the original volume, to obtain the crude extract of red pine pine nut shell polysaccharide;

[0034] (3) The crude extract of red pine pine nut shell polysaccharide and 70% ethanol solution are mixed in a mass ratio of 1:15, shaken uniformly, and then placed at 4℃ for 12h, centrifuged, ultrafiltrated to obtain the red pine pine nut shell polysaccharide solution;

[0035] (4) The Korean pine nut shell polysaccharide solution is passed into the D101 macroporous resin, the elution speed is set to 1.5 BV / h, and the macroporous resin column is eluted with 3 times the volume of deionized water, 2 times the volume of 50wt% ethanol solution and 1.5 times the volume of 30wt% ethanol solution, respectively, the ethanol solution is collected, and dried to obtain the Korean pine nut shell polysaccharide.

[0036] The parameters of the high-pressure microfluidization treatment in step (2) of the example are as follows: the treatment pressure is 100 MPa, and the treatment flow rate is 50 mL / min.

[0037] The parameters of the centrifugation in step (2) of the example are as follows: the centrifugation temperature is 4°C, the centrifugation speed is 6000 rpm, and the centrifugation time is 10 min.

[0038] The parameters of the centrifugation in step (3) of the example are as follows: the centrifugation temperature is 4°C, the centrifugation speed is 10000 rpm, and the centrifugation time is 10 min.

[0039] The ultrafiltration membrane with a molecular weight cut-off of 6KD is used in step (3) of the example.

[0040] The preparation method of the resveratrol solution in the example is as follows:

[0041] 6 parts by weight of resveratrol, 10 parts by weight of 70% ethanol solution and 5 parts by weight of Tween-80 are mixed, the ultrasonic frequency is set to 300W, the ultrasonic temperature is set to 40°C, and the ultrasonic treatment is performed for 10 min to obtain the resveratrol solution.

[0042] The preparation method of the antioxidant composite solution in the example is as follows:

[0043] 1.5 parts by weight of lipoic acid, 6.2 parts by weight of vitamin C, 1.8 parts by weight of vitamin E, 5 parts by weight of Tween-80 and 15 parts by weight of deionized water are mixed, citric acid is added dropwise to adjust the pH to 6.2, and stirring is performed at a speed of 80 rpm for 20 min to obtain the antioxidant composite solution.

[0044] The preparation method of the antioxidant composition in the example is as follows:

[0045] The temperature of the reaction kettle is set to 30°C, the Korean pine nut shell polysaccharide and deionized water are mixed, the resveratrol solution is added, citric acid is added dropwise to adjust the pH to 6, stirring is performed at a speed of 80 rpm for 20 min, the antioxidant composite solution, ubiquinone, dextran and sodium hyaluronate are added in sequence, and stirring is performed at a speed of 100 rpm for 1 h to obtain the antioxidant composition.

[0046] Example 2

[0047] A kind of plant polysaccharide and its antioxidant composition prepared by high pressure microjet, the antioxidant composition of the embodiment includes 36 parts of red pine pine nut shell polysaccharide, 25 parts of resveratrol solution, 20 parts of anti-oxidation composite solution, 3.5 parts of ubiquinone, 20 parts of dextran, 3.2 parts of sodium hyaluronate and 60 parts of deionized water by weight.

[0048] The preparation method of the red pine pine nut shell polysaccharide of the embodiment includes the following steps:

[0049] (1) take red pine pine nut shell in 65 ℃ drying oven, crush and pass through 80 mesh screen to obtain red pine pine nut shell powder;

[0050] (2) mix red pine pine nut shell powder, cellulase, pepsin and deionized water according to the mass ratio of 1:0.034:0.023:30, shake uniformly, set the temperature of water bath to 70 ℃, water bath extraction for 5 h, then high pressure microjet treatment for 3 times, centrifugal, take supernatant, rotary evaporation to concentrate to 1 / 3 of the original volume, to obtain red pine pine nut shell polysaccharide crude extract;

[0051] (3) mix red pine pine nut shell polysaccharide crude extract and 80% ethanol solution according to the mass ratio of 1:25, shake uniformly, stand at 4 ℃ for 24 h, centrifugal, ultrafiltration, to obtain red pine pine nut shell polysaccharide solution;

[0052] (4) pass red pine pine nut shell polysaccharide solution into D101 macroporous resin, set the elution speed to 2.5 BV / h, sequentially use 3 times the volume of deionized water, 2 times the volume of 60 wt% ethanol solution and 1.5 times the volume of 40 wt% ethanol solution to elute the resin column, collect ethanol solution, dry to obtain red pine pine nut shell polysaccharide.

[0053] The parameters of high pressure microjet treatment in step (2) of the embodiment are: treatment pressure is 140 MPa, and treatment flow is 150 mL / min.

[0054] The centrifugal parameters in step (2) of the embodiment are: centrifugal temperature is 4 ℃, centrifugal speed is 8000 rmp, and centrifugal time is 20 min.

[0055] The centrifugal parameters in step (3) of the embodiment are: centrifugal temperature is 4 ℃, centrifugal speed is 12000 rmp, and centrifugal time is 20 min.

[0056] The ultrafiltration membrane with a molecular weight cut-off of 12 KD is used in step (3) of the embodiment.

[0057] The preparation method of the resveratrol solution of the embodiment is:

[0058] Mix 12 parts by weight of resveratrol, 20 parts by weight of 80% ethanol solution and 10 parts by weight of Tween-80, set the ultrasonic frequency to 500W and the ultrasonic temperature to 50℃, and ultrasonically treat for 30min to obtain a resveratrol solution.

[0059] The preparation method of the antioxidant composite solution of the present embodiment is as follows:

[0060] Mix 2.5 parts by weight of lipoic acid, 8.4 parts by weight of vitamin C, 4.2 parts by weight of vitamin E, 10 parts by weight of Tween-80 and 25 parts by weight of deionized water, dropwise add citric acid to adjust the pH to 6.8, and stir at a speed of 280rmp for 40min to obtain an antioxidant composite solution.

[0061] The preparation method of the antioxidant composite solution of the present embodiment is as follows:

[0062] Set the temperature of the reaction kettle to 40℃, mix the Korean pine nut shell polysaccharide and deionized water, then add the resveratrol solution, dropwise add citric acid to adjust the pH to 7, stir at a speed of 100rmp for 30min, then sequentially add the antioxidant composite solution, ubiquinone, dextran and sodium hyaluronate, and stir at a speed of 300rmp for 2h to obtain an antioxidant composition.

[0063] Example 3

[0064] An antioxidant composition prepared from a plant polysaccharide by high-pressure microjet, the antioxidant composition of the present embodiment includes, by weight, 29 parts of Korean pine nut shell polysaccharide, 20 parts of resveratrol solution, 15 parts of antioxidant composite solution, 2.5 parts of ubiquinone, 15 parts of dextran, 2.5 parts of sodium hyaluronate and 50 parts of deionized water.

[0065] The preparation method of the Korean pine nut shell polysaccharide of the present embodiment includes the following steps:

[0066] (1) Dry the Korean pine nut shell in a 65℃ drying oven, crush and pass through a 70-mesh sieve to obtain Korean pine nut shell powder;

[0067] (2) Mix the Korean pine nut shell powder, cellulase, pepsin and deionized water in a mass ratio of 1:0.03:0.02:25, shake uniformly, set the temperature of the water bath to 65℃, water-bath extract for 4.5h, then perform high-pressure microjet treatment for 3 times, centrifuge, take the supernatant, and rotary-evaporate to concentrate to 1 / 3 of the original volume to obtain a crude Korean pine nut shell polysaccharide extract;

[0068] (3) Mix the crude Korean pine nut shell polysaccharide extract and 75% ethanol solution in a mass ratio of 1:20, shake uniformly, stand at 4℃ for 18h, centrifuge, and ultrafilter to obtain a Korean pine nut shell polysaccharide solution;

[0069] (4) The Pinus koraiensis seed shell chitan solution is passed into the D101 macroporous resin, the elution speed is set as 2BV / h, and the macroporous resin column is eluted with 3 times the resin column volume of deionized water, 2 times the resin column volume of 55wt% ethanol solution and 1.5 times the resin column volume of 35wt% ethanol solution in sequence, the ethanol solution is collected, and dried to obtain the Pinus koraiensis seed shell chitan.

[0070] The high-pressure microfluidization treatment in step (2) of the example has the following parameters: the treatment pressure is 120MPa, and the treatment flow rate is 100mL / min.

[0071] The centrifugation in step (2) of the example has the following parameters: the centrifugation temperature is 4℃, the centrifugation speed is 7000rmp, and the centrifugation time is 15min.

[0072] The centrifugation in step (3) of the example has the following parameters: the centrifugation temperature is 4℃, the centrifugation speed is 11000rmp, and the centrifugation time is 15min.

[0073] The ultrafiltration in step (3) of the example uses an ultrafiltration membrane with a molecular weight cut-off of 9KD.

[0074] The preparation method of the resveratrol solution in the example is as follows:

[0075] 9 parts by weight of resveratrol, 15 parts by weight of 75% ethanol solution and 7.5 parts by weight of Tween-80 are mixed, the ultrasonic frequency is set as 400W, the ultrasonic temperature is set as 45℃, and the mixture is ultrasonically treated for 20min to obtain the resveratrol solution.

[0076] The preparation method of the antioxidant composite solution in the example is as follows:

[0077] 2 parts by weight of lipoic acid, 7.3 parts by weight of vitamin C, 3 parts by weight of vitamin E, 7.5 parts by weight of Tween-80 and 20 parts by weight of deionized water are mixed, citric acid is added dropwise to adjust the pH to 6.5, and the mixture is stirred at a speed of 180rmp for 30min to obtain the antioxidant composite solution.

[0078] The preparation method of the antioxidant composition in the example is as follows:

[0079] The temperature of the reaction kettle is set as 35℃, the Pinus koraiensis seed shell chitan and deionized water are mixed, the resveratrol solution is added, citric acid is added dropwise to adjust the pH to 6.5, the mixture is stirred at a speed of 90rmp for 25min, the antioxidant composite solution, ubiquinone, dextran and sodium hyaluronate are added in sequence, and the mixture is stirred at a speed of 200rmp for 1.5h to obtain the antioxidant composition.

[0080] Comparative Example 1

[0081] On the basis of example 3, the cellulase in the preparation process of the Pinus koraiensis Sieb. et Zucc. seed shell polysaccharide is removed, and an equal weight of protease is used instead, and other conditions are consistent with example 3.

[0082] Comparative example 2

[0083] On the basis of example 3, the protease in the preparation process of the Pinus koraiensis Sieb. et Zucc. seed shell polysaccharide is removed, and an equal weight of cellulase is used instead, and other conditions are consistent with example 3.

[0084] Comparative example 3

[0085] On the basis of example 3, the high-pressure microfluidization treatment step in the preparation process of the Pinus koraiensis Sieb. et Zucc. seed shell polysaccharide is removed, and other conditions are consistent with example 3.

[0086] Comparative example 4

[0087] On the basis of example 3, the treatment pressure of the high-pressure microfluidization treatment in the preparation process of the Pinus koraiensis Sieb. et Zucc. seed shell polysaccharide is changed to 80 MPa, and other conditions are consistent with example 3.

[0088] Comparative example 5

[0089] On the basis of example 3, the treatment pressure of the high-pressure microfluidization treatment in the preparation process of the Pinus koraiensis Sieb. et Zucc. seed shell polysaccharide is changed to 160 MPa, and other conditions are consistent with example 3.

[0090] Comparative example 6

[0091] On the basis of example 3, the macroporous resin elution step in the preparation process of the Pinus koraiensis Sieb. et Zucc. seed shell polysaccharide is removed, and other conditions are consistent with example 3.

[0092] Comparative example 7

[0093] On the basis of example 3, the elution method of the macroporous resin elution step in the preparation process of the Pinus koraiensis Sieb. et Zucc. seed shell polysaccharide is changed to sequentially using 3 times the resin column volume of deionized water, 2 times the resin column volume of 70 wt% ethanol solution, and 1.5 times the resin column volume of 50 wt% ethanol solution for elution, and other conditions are consistent with example 3.

[0094] Comparative example 8

[0095] On the basis of example 3, the ultrasonic treatment step in the preparation process of the resveratrol solution is removed, and other conditions are consistent with example 3.

[0096] Comparative example 9

[0097] On the basis of example 3, the Tween-80 in the preparation process of the resveratrol solution is removed, and an equal weight of 75% ethanol solution is used instead, and other conditions are consistent with example 3.

[0098] Comparative example 10

[0099] On the basis of Example 3, lipoic acid was removed in the preparation process of the antioxidant composite solution, and an equal weight of vitamin E was used instead, and other conditions were consistent with Example 3.

[0100] Comparative Example 11

[0101] On the basis of Example 3, vitamin E was removed in the preparation process of the antioxidant composite solution, and an equal weight of vitamin C was used instead, and other conditions were consistent with Example 3.

[0102] Comparative Example 12

[0103] On the basis of Example 3, vitamin C was removed in the preparation process of the antioxidant composite solution, and an equal weight of lipoic acid was used instead, and other conditions were consistent with Example 3.

[0104] Comparative Example 13

[0105] On the basis of Example 3, Tween-80 was removed in the preparation process of the antioxidant composite solution, and an equal weight of deionized water was used instead, and other conditions were consistent with Example 3.

[0106] Comparative Example 14

[0107] On the basis of Example 3, dextran was removed, and an equal weight of ubiquinone was used instead, and other conditions were consistent with Example 3.

[0108] Comparative Example 15

[0109] On the basis of Example 3, sodium hyaluronate was removed, and an equal weight of dextran was used instead, and other conditions were consistent with Example 3.

[0110] Comparative Example 16

[0111] On the basis of Example 3, ubiquinone was removed, and an equal weight of sodium hyaluronate was used instead, and other conditions were consistent with Example 3.

[0112] 1. DPPH free radical scavenging test

[0113] The antioxidant compositions prepared in Examples 1-3 and Comparative Examples 1-16 were used as samples, and 4 mL of DPPH solution with a concentration of 6 x 10 5 mol / L was added to an equal volume of 19 groups of samples, and mixed uniformly to obtain the corresponding mixed samples.

[0114] The absorbance value Ac of the DPPH solution, the initial absorbance value Ai of the mixed sample, and the absorbance value Aj after 30 min of room temperature light shielding were tested at 518 nm, and the DPPH free radical scavenging rate was calculated according to the following formula: scavenging rate (%) = [1-(Ai-Aj) / Ac] x 100%, and the test results are shown in Table 1.

[0115] Table 1 DPPH radical scavenging rate

[0116]

[0117]

[0118] As can be seen from Table 1, after the steps of crushing, enzymatic hydrolysis, ultrafiltration, high-pressure microjet treatment, and macroporous resin elution, the internal active ingredients of polysaccharides are fully extracted, and the components are compatible and complementary to each other, and synergistic. The DPPH radical scavenging rate of the antioxidant composition prepared in Examples 1-3 is obviously higher, and the DPPH radical scavenging rate measured finally will be affected due to the change of components or preparation method, etc. of Comparative Examples 1-16, thereby affecting the overall use feeling.

[0119] 2. Skin irritation test

[0120] Twenty healthy skin volunteers, half male and half female, aged 20-40 years old, all of whom had no history of skin disease, no known allergy to test materials, and no use of any drugs or cosmetics that could affect skin response within at least 2 weeks before the test.

[0121] The antioxidant compositions prepared in Examples 1-3 and Comparative Examples 1-16 were used as samples, and the degree of skin irritation of the samples was tested using a patch test. Twenty test points were selected on the back of the subject, with a 2 cm interval between adjacent test points, avoiding the spine and ribs.

[0122] After cleaning the test area, 19 patch testers with 0.05 g of the sample added and one empty patch tester were attached to the back of the subject with a low-sensitization tape, and the skin was evenly coated with the sample by lightly pressing with the fingers for 48 hours. After removing the patch tester 30 min later, the skin reaction of the test site was observed, and the evaluation criteria were divided into 0-4 levels, 0 level was no redness and irritation, and 4 level was severe redness and irritation. The test results are shown in Table 2.

[0123] Table 2 Skin redness and irritation degree

[0124]

[0125]

[0126] As can be seen from Table 2, the antioxidant composition in the present application has better compatibility between components, less skin irritation, and can gently act on the skin, and jointly exert beneficial effects.

[0127] The above merely describes the preferred embodiments of the present application, and is not intended to limit the present application in any form. Although the present application has been disclosed with the preferred embodiments as above, it is not intended to limit the present application. Any person skilled in the art can make some changes or modifications to the above disclosed technical content to obtain equivalent embodiments with equivalent changes, as long as the changes or modifications do not deviate from the technical solution of the present application. Any modification, change, equivalent change and modification of the above embodiments made according to the technical essence of the present application still belong to the scope of the technical solution of the present application.

Claims

1. An antioxidant composition, characterized in that, The antioxidant composition comprises, by weight, 22-36 parts of red pine nut shell polysaccharide, 15-25 parts of resveratrol solution, 10-20 parts of antioxidant complex solution, 1.5-3.5 parts of ubiquinone, 10-20 parts of dextran, 1.8-3.2 parts of sodium hyaluronate and 40-60 parts of deionized water; The preparation method of the red pine nut shell polysaccharide includes the following steps: (1) Dry the pine nuts of red pine in a drying oven at 65℃, pulverize them and pass them through a 60-80 mesh sieve to obtain red pine nut shell powder; (2) Mix red pine nut shell powder, cellulase, pepsin and deionized water at a mass ratio of 1:0.026~0.034:0.017~0.023:20~30, shake evenly, set the water bath temperature to 60~70℃, extract in water bath for 4~5h, then perform high pressure micro-jet treatment 3 times, centrifuge, take the supernatant, and concentrate it to 1 / 3 of the original volume by rotary evaporation to obtain crude extract of red pine nut shell polysaccharide; (3) Mix the crude extract of red pine nut shell polysaccharide and 70-80% ethanol solution at a mass ratio of 1:15-25, shake evenly, let stand at 4℃ for 12-24h, centrifuge, and ultrafilter to obtain red pine nut shell polysaccharide solution. (4) The red pine nut shell polysaccharide solution was passed into D101 macroporous resin and the elution rate was set to 1.5-2.5 BV / h. The solution was eluted sequentially with 3 times the resin column volume of deionized water, 2 times the resin column volume of 50-60 wt% ethanol solution, and 1.5 times the resin column volume of 30-40 wt% ethanol solution. The ethanol solution was collected and dried to obtain red pine nut shell polysaccharide. The resveratrol solution is prepared as follows: Mix 6-12 parts by weight of resveratrol, 10-20 parts by weight of 70-80% ethanol solution, and 5-10 parts by weight of Tween-80, and then set the ultrasonic frequency to 300-500W and the ultrasonic temperature to 40-50℃, and ultrasonically treat for 10-30 minutes to obtain a resveratrol solution. The preparation method of the antioxidant composite solution is as follows: Mix 1.5–2.5 parts by weight of lipoic acid, 6.2–8.4 parts by weight of vitamin C, 1.8–4.2 parts by weight of vitamin E, 5–10 parts by weight of Tween-80 and 15–25 parts by weight of deionized water, add citric acid dropwise to adjust the pH to 6.2–6.8, and stir at 80–280 rpm for 20–40 min to obtain an antioxidant complex solution; The parameters for the high-pressure microjet treatment in step (2) are: treatment pressure of 100-140 MPa and treatment flow rate of 50-150 mL / min.

2. The antioxidant composition according to claim 1, characterized in that, The centrifugation parameters in step (2) are: centrifugation temperature of 4℃, centrifugation speed of 6000~8000rpm, and centrifugation time of 10~20min.

3. The antioxidant composition according to claim 1, characterized in that, The centrifugation parameters in step (3) are: centrifugation temperature of 4℃, centrifugation speed of 10000~12000rpm, and centrifugation time of 10~20min.

4. The antioxidant composition according to claim 1, characterized in that, The ultrafiltration in step (3) uses an ultrafiltration membrane with a molecular weight cutoff of 6 to 12 kDa.

5. An antioxidant composition according to any one of claims 1 to 4, characterized in that, The method for preparing the antioxidant composition is as follows: Set the reactor temperature to 30–40°C, add red pine nut shell polysaccharide and deionized water, mix well, then add resveratrol solution, add citric acid dropwise to adjust the pH to 6–7, stir at 80–100 rpm for 20–30 min, then add antioxidant complex solution, ubiquinone, dextran and sodium hyaluronate in sequence, stir at 100–300 rpm for 1–2 h to obtain antioxidant composition.

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