A composition having an anti-glycation efficacy, and a preparation method and application thereof

Abstract

The present application relates to the cosmetic technical field, specifically to a kind of composition with anti-glycation efficacy and its preparation method and application, raw material includes cactus fruit extract, psidium guajava fruit extract, fig extract.The composition of the present application is obtained by the specific preparation process of cactus fruit extract, psidium guajava fruit extract and fig extract, and the amount of control is proportion, through the synergistic effect between plant extracts, it can effectively antioxidant and inhibit the generation of late glycosylation end product, directly and effectively and long-acting improve skin glycation, make skin present healthy luster.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of cosmetics, in particular to a composition with anti-glycation efficacy and a preparation method and application thereof. BACKGROUND

[0002] Opuntia ficus-indica, Latin name, is a new fruit, which is famous for its high concentration of polyphenols and antioxidants. According to the in vitro and biological activity data of domestic and foreign research, regular consumption of the fruit can reduce the risk of chronic diseases, and its protective effect is related to organic acids, phenolic compounds, lipid content and their synergistic effect. Ascorbic acid has been quantified in many Opuntia ficus-indica, and its content seems to be higher than other organic acids and fruits such as apples and grapes. Opuntia ficus-indica has limited application in food due to its small edible part. Current research focuses on clinical directions such as antioxidant, anti-inflammatory, and hypoglycemic effects.

[0003] Psidium guajava L., also known as guava, is a tropical fruit that is popular among consumers due to its rich nutritional content and pharmacological treatment properties. It is widely consumed in southern China. Guava is rich in various secondary metabolites in almost all parts, especially phenols, flavonoids, ascorbic acid, and polysaccharides. Polysaccharides are one of the most biologically significant chemical components of guava, and there is no comprehensive report on the systematic review of guava polysaccharides. The extraction and purification process of guava polysaccharides has been extensively studied, but there is little research on its application in personal care products.

[0004] Ficus carica Linn, also known as Aladdin, is a medicinal and edible raw material that is abundant in Xinjiang and is a rare fruit in China. Ficus carica is easily contaminated by microorganisms and mechanically damaged, and its short shelf life is one of the main reasons limiting its application. Consumers have little knowledge of the health-promoting effects of Ficus carica. Plant polysaccharides are natural high-molecular-weight polymers extracted from plants. Due to their rich biological activity, safety, and skin-friendliness, they are increasingly attracting attention. Polysaccharides are one of the main functional components of Ficus carica, accounting for 44-74.3% of the dry weight. The higher the maturity of the fruit, the higher the polysaccharide content. Ficus carica polysaccharides have been extensively studied in animal experiments, and have been shown to have effects on enhancing immunity, reducing blood sugar, anti-inflammatory, and antioxidant effects.

[0005] Prior art US08663718B2 discloses a method for producing cactus fruit extract and its use for formulating beverages, which can be used for preventing and treating venous pain. CN101491583A discloses a composition with hypoglycemic function and a preparation method thereof. The composition is prepared from bitter gourd, fresh cactus, guava leaves and chromium gluconate in a certain weight ratio, has hypoglycemic effect, and can be used for treating diabetes. However, relatively little research has been conducted on its use in personal care products, and the efficacy is relatively single, which is not conducive to market promotion and practical application. SUMMARY

[0006] To solve the problems in the prior art, the first aspect of the present application provides a composition with antioxidant efficacy, raw materials including cactus fruit extract, guava fruit extract and fig fruit extract.

[0007] In an embodiment, the mass ratio of the cactus fruit extract, guava fruit extract and fig fruit extract is (2-4):(1-3):(1-2).

[0008] In an embodiment, the mass ratio of the cactus fruit extract, guava fruit extract and fig fruit extract is 3:1:2.

[0009] In an embodiment, the mass ratio of the cactus fruit extract, guava fruit extract and fig fruit extract is 2:3:1.

[0010] In an embodiment, the mass ratio of the cactus fruit extract, guava fruit extract and fig fruit extract is 4:3:1.

[0011] In an embodiment, the mass ratio of the cactus fruit extract, guava fruit extract and fig fruit extract is 4:1:1.

[0012] The second aspect of the present application provides a preparation method of the above-mentioned composition with anti-glycation efficacy, comprising the following steps:

[0013] S1, preparation of cactus fruit extract;

[0014] S2, preparation of guava fruit extract;

[0015] S3, preparation of fig fruit extract;

[0016] S4, mixing the cactus fruit extract, guava fruit extract and fig fruit extract to obtain the composition with anti-glycation efficacy.

[0017] In an embodiment, the preparation of the cactus fruit extract in the S1 step comprises:

[0018] a. The fresh cactus fruit is washed and cut into pieces, and then placed in the dark at room temperature after being irradiated by a UV lamp. Then the cactus fruit is put into a mixed solution containing enzyme preparation and broken wall extraction is performed using a magnetic stirrer. After the stirring is completed, the enzyme is inactivated by heating, and then the extraction is performed at a temperature of 65-75℃ and a speed of 1500-2000 rpm for 1-2 hours to obtain an extract liquid;

[0019] b. The extract liquid is filtered, and the filtrate is centrifuged to obtain supernatant. The supernatant is heated and concentrated, and then high-pressure steam sterilization is performed to obtain a cactus fruit extract.

[0020] In an embodiment, the UV irradiation time in the a step is 10-20 min.

[0021] In an embodiment, the cutting treatment in the a step is cutting into 4 pieces.

[0022] In an embodiment, the enzyme preparation contains one or both of pectinase and cellulase.

[0023] In an embodiment, the enzyme preparation contains pectinase and cellulase.

[0024] In an embodiment, the mixed solution contains butanediol.

[0025] In an embodiment, the mass ratio of the pectinase, cellulase, cactus fruit and butanediol is (3-5) : (30-50) : 1000 : 4000.

[0026] In an embodiment, the mass ratio of the pectinase, cellulase, cactus fruit and butanediol is 4:40:1000:4000.

[0027] In an embodiment, the enzyme activity of the pectinase is 10-30 thousand u / g, and the enzyme activity of the cellulase is 10 thousand u / g.

[0028] In an embodiment, the enzyme activity of the pectinase is 20 thousand u / g.

[0029] In an embodiment, the breaking wall extraction condition in the a step is a temperature of 40-45℃ and a centrifugal force of 1500-2000 rpm.

[0030] In an embodiment, the breaking wall extraction condition in the a step is a temperature of 42℃ and a centrifugal force of 1700 rpm.

[0031] In an embodiment, the stirring time in the a step is 1h, and the inactivation condition of the enzyme is a temperature of 70-80℃ and a stirring time of 10-20 min.

[0032] In an embodiment, the a step of heat denaturing the enzyme is performed at a temperature of 75°C for 15 minutes.

[0033] In an embodiment, the b step of filtering the extract is performed using whatman 4 filter paper or 500 mesh filter cloth.

[0034] In an embodiment, the b step of centrifuging is performed at a centrifugal force of 5000-6000 rpm for 10-20 minutes.

[0035] In an embodiment, the b step of centrifuging is performed at a centrifugal force of 5500 rpm for 15 minutes.

[0036] In an embodiment, the b step of autoclaving is performed at 121°C for 10 minutes.

[0037] In an embodiment, the S2 step of preparing the guava fruit extract comprises:

[0038] The fresh guava fruit is washed and sliced, dried in an oven at 60°C, and then the dried fruit is ground and filtered. Deionized water is added and the mixture is stirred using a magnetic stirrer for 1 hour. The mixture is filtered using a sieve, and the residue is subjected to a second extraction using the above steps. The two extracts are filtered, centrifuged, and the supernatant is heated and concentrated. The mixture is filtered using a micropore filter to remove bacteria, and the guava fruit extract is obtained.

[0039] In an embodiment, the drying time is until the weight of the dried fruit is 12-18% of the weight of the fresh fruit.

[0040] In an embodiment, the drying time is until the weight of the dried fruit is 15% of the weight of the fresh fruit.

[0041] In an embodiment, the mass ratio of the dried guava fruit to deionized water is 1: (45-55).

[0042] In an embodiment, the mass ratio of the dried guava fruit to deionized water is 1:50.

[0043] In an embodiment, the first extraction is performed at a temperature of 65-70°C and a centrifugal force of 1000-2000 rpm.

[0044] In an embodiment, the first extraction is performed at a temperature of 67°C and a centrifugal force of 1500 rpm.

[0045] In an embodiment, the mesh size of the sieve is 300 mesh.

[0046] In an embodiment, the centrifugal force in the S2 step is 5000-6000 rpm for 10-20 min.

[0047] In an embodiment, the centrifugal force in the S2 step is 5500 rpm for 150 min.

[0048] In an embodiment, the pore size of the microfiltration membrane is 0.22 μm.

[0049] In an embodiment, the preparation of the fig extract in the S3 step comprises:

[0050] Fresh figs are washed, sliced, dried in an oven at 60°C, then the dried figs are ground and filtered, then added to deionized water, and the extract is extracted by ultrasonic extraction for 1-1.5 h, then the extract is filtered, centrifuged, and the supernatant is heated and concentrated, then filtered through a microfiltration membrane to remove bacteria, to obtain the fig extract.

[0051] In an embodiment, the drying time in the S3 step is 12%-18% of the weight of the fresh fruit.

[0052] In an embodiment, the mass ratio of the dried figs to deionized water is 1:(50-60).

[0053] In an embodiment, the mass ratio of the dried figs to deionized water is 1:55.

[0054] In an embodiment, the ultrasonic conditions in the S3 step are 300 W, 35-45 kHz, and 75-85°C.

[0055] In an embodiment, the centrifugal force in the S3 step is 7000-8000 rpm for 10-20 min.

[0056] In an embodiment, the centrifugal force in the S3 step is 7500 rpm for 15 min.

[0057] The third aspect of the present application provides the use of the composition in cosmetics.

[0058] Advantages

[0059] 1. The composition prepared by the present application has anti-glycation effect, uses natural plant extracts, does not contain any harmful substances, and has no risk to skin health.

[0060] 2、The extraction method of the present application involves ultrasonic, hot water extraction, secondary extraction, low cost, simple and safe operation, no pollution of reagents, less interfering substances, high extraction yield, low energy consumption, without changing the structure of active substances.

[0061] 3、The composition has no irritation by the chicken embryo chorioallantoic membrane irritation test, and can be used by people with sensitive skin barrier.

[0062] 4、The composition of the present application is obtained by a specific preparation process, and the use amount of the cactus fruit extract, guava fruit extract and fig fruit extract is controlled, and the synergistic effect between the plant extracts can effectively resist oxidation and inhibit the generation of AGEs, directly and effectively and long-acting improve skin glycation, and make the skin present healthy luster.

[0063] 5、The composition prepared by the present application has anti-glycation effect and can be applied to cosmetics, increasing the commercial value of cactus fruit, guava fruit and fig. BRIEF DESCRIPTION OF DRAWINGS

[0064] Figure 1 The figure is the in-vitro test of the anti-oxidation effect of the samples prepared in Examples 1-6, Comparative Examples 1-3 and the control group.

[0065] Figure 2 The figure is the in-vitro test of the anti-irritation effect of the samples prepared in Examples 1-6, Comparative Examples 1-3 and the control group.

[0066] Figure 3 The figure is the in-vitro test of the anti-glycation effect of the samples prepared in Examples 1-6, Comparative Examples 1-3 and the control group.

[0067] Figure 4 The figure is the clinical test of the anti-glycation effect of the gel product containing the composition prepared in Example 3.

[0068] Figure 5 The figure is the clinical test of the skin color improvement effect of the gel product containing the composition prepared in Example 3. DETAILED DESCRIPTION

[0069] In order to make the purpose, technical scheme and advantages of the present application more clear, the present application is further described in detail below in combination with examples. It should be understood that the specific examples described herein are only used to explain the present application, and are not used to limit the present application. The experimental methods not specified in the examples are carried out according to the conventional conditions or the conditions recommended by the manufacturer. The reagents or instruments used are not specified by the manufacturer, and are conventional products that can be purchased on the market.

[0070] Example 1

[0071] The first aspect of the embodiment provides a composition with anti-glycation efficacy, raw materials including cactus fruit extract, psidium fruit extract and fig extract.

[0072] The mass ratio of the cactus fruit extract, psidium fruit extract and fig extract is 1:1:1.

[0073] The second aspect of the embodiment provides a preparation method of a composition with anti-glycation efficacy, including the following steps:

[0074] S1. Preparation of cactus fruit extract:

[0075] Fresh cactus fruit is washed and cut into four pieces, and then irradiated by a UVB-313 ultraviolet lamp for 15 min, and then placed in the dark at room temperature for 24 h.

[0076] Then pectinase, cellulase, cactus fruit and butanediol are put into a beaker according to a mass ratio of 4:40:1000:4000. Wall breaking extraction is carried out at a temperature of 42℃ and a speed of 1700 rpm for 1 h, and then the temperature is increased to 75℃ for 15 min to inactivate the enzyme. Then extraction is carried out at a temperature of 70℃ and a speed of 1700 rpm for 1.5 h.

[0077] The extract liquid is filtered by using 500 mesh filter cloth, and the filtrate is centrifuged at 5500 rpm for 15 min by using a centrifuge. The supernatant is obtained, heated and concentrated, and then sterilized by using 121℃ high pressure steam for 10 min to obtain the cactus fruit extract.

[0078] The enzyme activity of the pectinase is 20,000 u / g, and the enzyme activity of the cellulase is 10,000 u / g.

[0079] S2. Preparation of psidium fruit extract:

[0080] Fresh psidium fruit is washed and sliced, and then dried in an oven at 60℃ to a weight of 15% of the fresh fruit. Then the dried fruit is crushed and sieved through a 50 mesh sieve. Then the dried psidium fruit and deionized water are put into a beaker according to a mass ratio of 1:50, and extraction is carried out by using a magnetic stirrer at a temperature of 67℃ and a speed of 1500 rpm for 1 h. After the first extraction, the filtrate is filtered by using a 300 mesh screen, and the filter residue is repeated for the second extraction. After the second extraction, the extract liquids of the two times are filtered by using whatman 4 filter paper, and the filtrate is centrifuged at 5500 rpm for 15 min by using a centrifuge. The supernatant is obtained, heated and concentrated, and then filtered by using a 0.22μm microporous filter membrane to remove bacteria to obtain the psidium fruit extract.

[0081] S3. Preparation of fig extract:

[0082] Fresh figs were washed and sliced, dried in an oven at 60℃ to 15% of the weight of fresh figs, then the dried figs were crushed and sieved through a 50 mesh sieve, then the dried figs and deionized water were put into a beaker at a mass ratio of 1:55, and ultrasonic extraction was carried out at 300 W, 40 kHz, and 80℃ for 1 h.

[0083] After ultrasonic extraction, the extract liquid was filtered through a 500 mesh filter cloth, and the filtrate was centrifuged at 7500 rpm for 15 min, and the supernatant was obtained, concentrated, filtered through a 0.22 μm microporous filter membrane, and sterilized to obtain the fig extract.

[0084] S4, the cactus fruit extract, psidium fruit extract and fig extract were mixed to obtain a composition having an anti-glycation effect.

[0085] The third aspect of the embodiment provides an application of the composition having an anti-glycation effect in cosmetics.

[0086] Examples 2-6, Comparative Examples 1-3

[0087] The specific embodiments of Examples 2-6, Comparative Examples 1-3 are the same as those of Example 1, except that the mass ratio of the cactus fruit extract, psidium fruit extract and fig extract is different, as shown in Table 1:

[0088] Table 1

[0089]

[0090]

[0091] Performance test

[0092] 1. Antioxidant effect test (in vitro experiment)

[0093] Test samples: samples prepared in Examples 1-6 and Comparative Examples 1-3, and a control group.

[0094] Test method: prepare a DPPH solution at 80 μg / mL, and test samples at a concentration of 2.5 (% v / v), and 0.1% VC as a control group sample. The antioxidant effect of the test sample is determined by testing the DPPH free radical scavenging ability of the test sample.

[0095] Test results: see Figure 1 The antioxidant capacity is: Example 3 > Example 2 > Example 4 > Example 5 > Example 6 > Example 1 > Comparative Example 2 > Comparative Example 1 > Comparative Example 3 > control group. The composition of the present application is obviously superior to the comparative examples in terms of antioxidant performance, indicating that the composition of the present application can have a synergistic effect.

[0096] 2. Anti-stimulation efficacy test (in vitro experiment)

[0097] Test samples: Samples prepared in Examples 1-6, Comparative Examples 1-3, and the control group.

[0098] Test method: Dilute the sample with normal saline to 95%. Using the chick embryo chorioallantoic membrane model, with sodium dodecyl sulfate (SDS) as the stimulant, mix the sample with SDS and then add it to the chick embryo chorioallantoic membrane. Score by observing the changes in the toxicity effect indexes (bleeding, vascular lysis, coagulation) of the chick embryo chorioallantoic membrane. Evaluate the inhibitory effect of the sample on mucosal irritation caused by the stimulant.

[0099] In the control group, use the chick embryo chorioallantoic membrane model, add sodium dodecyl sulfate (SDS) as the stimulant to the chick embryo chorioallantoic membrane, score by observing the changes in the toxicity effect indexes (bleeding, vascular lysis, coagulation) of the chick embryo chorioallantoic membrane, and evaluate the inhibitory effect of the sample on mucosal irritation caused by the stimulant. Result determination: ES ≤ 12, no / mild irritation; 12 < ES < 16, moderate irritation; ES ≥ 16, strong irritation.

[0100] Test results: See Figure 2 , anti-stimulation ability: Example 4 > Example 2 = Example 3 > Example 5 > Example 6 > Example 1 > Comparative Example 2 = Comparative Example 1 > Comparative Example 3 > control group.

[0101] 3. Anti-glycation efficacy test (in vitro experiment)

[0102] Test samples: Samples prepared in Examples 1-6, Comparative Examples 1-3, and the control group. <000022​​​​​​​​​

[0106] 4. Anti-glycation and skin tone improvement test (clinical trial)

[0107] Test subject: Gel products containing the composition prepared in Example 3. The formulation of the gel products is shown in Table 2 below. The formulation uses ingredients that do not affect the tested efficacy. The preparation method is conventional mixing and stirring.

[0108] Test method: Thirty subjects were selected and applied the gel product morning and evening for four consecutive weeks. AGEs Reader was used at weeks 0, 2, and 4. TM The CM-700D spectrophotometer was used to test the AGEs content and skin brightness in the skin to determine the efficacy of the sample in anti-glycation and skin tone improvement.

[0109] Test results: see Figure 4 and Figure 5 , Figure 4 and Figure 5 In the figure, 0W represents 0 weeks, 2W represents 2 weeks, and 4W represents 4 weeks. * indicates a significant difference compared to before use; * represents 0.01 ≤ p < 0.05; ** represents 0.001 ≤ p < 0.01; *** represents p < 0.001.

[0110] The composition of this invention, when applied to gel products, has long-lasting anti-glycation and skin-improving effects.

[0111] Table 2

[0112] Gel components Content (%) Water 91.87 Calcium chloride 0.03 Glycerol 5 Xanthan gum 0.6 Sodium benzoate 0.5 Example 3 composition 2

Claims

1. A composition with anti-glycation effects, characterized in that, The ingredients include cactus fruit extract, guava fruit extract, and fig extract; The mass ratio of the cactus fruit extract, guava fruit extract, and fig extract is (2~4):(1~3):(1~2). The preparation of the cactus fruit extract includes: a. Wash and cut fresh cactus fruit into pieces, irradiate with ultraviolet light, and place at room temperature in the dark. Then, add butanediol containing enzyme preparation and use a magnetic stirrer to break the cell wall and extract. After stirring, heat to inactivate the enzyme, and then extract at 65~75℃ and 1500~2000rpm for 1~2 hours to obtain the extract. b. Filter the extract, centrifuge the filtrate to obtain the supernatant, heat and concentrate it, and then sterilize it by high pressure steam to obtain the cactus fruit extract. The enzyme preparation is a combination of pectinase and cellulase; The preparation of the guava fruit extract includes: Fresh guava fruits were washed, sliced, and dried in an oven at 60°C. The dried guava fruits were then crushed and filtered, and then added to deionized water. The first extraction was performed using a magnetic stirrer and stirred for 1 hour. The mixture was then filtered through a sieve, and the residue was collected and the above steps were repeated for a second extraction. After the second extraction, the extracts from both extractions were filtered, the filtrate was centrifuged, the supernatant was collected, heated and concentrated, and then filtered through a microporous membrane to remove bacteria, thus obtaining guava fruit extract. The preparation of the fig extract includes: Fresh figs were washed, sliced, and dried in an oven at 60°C. The dried figs were then crushed and filtered, and then added to deionized water. The mixture was extracted using ultrasound for 1-1.5 hours. The extract was then filtered, the filtrate was centrifuged, the supernatant was collected, heated and concentrated, and then filtered through a microporous membrane to remove bacteria, thus obtaining the fig extract.

2. A method for preparing a composition with anti-glycation effect according to claim 1, characterized in that, Includes the following steps: S1. Preparation of cactus fruit extract; S2, Preparation of guava fruit extract; S3. Preparation of fig extract; S4. A combination with anti-glycation effects is obtained by mixing cactus fruit extract, guava fruit extract and fig extract.

3. The method for preparing the composition with anti-glycation effect according to claim 2, characterized in that, The mass ratio of pectinase, cellulase, cactus fruit and butanediol is (3~5):(30~50):1000:4000.

4. The use of the composition with anti-glycation effect according to claim 1 in the preparation of cosmetics.

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