Preparation method of trumpet creeper extract, product and application thereof

Abstract

The present invention relates to a preparation method of a trumpet creeper extract and its products and applications. The preparation method comprises: mixing the trumpet creeper with a solution containing a deep eutectic solvent, refluxing and extracting to obtain an extract; filtering the extract to obtain a filtrate; concentrating the filtrate to obtain a concentrate; using a macroporous resin to adsorb the concentrate, eluting to obtain an eluate; concentrating and drying the eluate. The trumpet creeper extract of the present invention has significant improvements in increasing the polyphenol content in the trumpet creeper, scavenging DPPH free radicals, and promoting the secretion of PC‑1 and COL‑3. The deep eutectic solvent prepared by the present invention is a green solvent, safe and non-toxic, simple and convenient to prepare, with a wide source of raw materials, and will not cause harm to the environment and human body. The obtained trumpet creeper extract can be used as an active substance in skin care products and medical auxiliary products.

Description

Technical Field

[0001] The invention belongs to the technical field of material extraction and relates to a preparation method of a trumpet creeper extract and a product and application thereof. Background Art

[0002] Skin aging is a process in which multiple factors inside and outside the body cause degenerative changes in the appearance of the skin and the structure and function of each skin layer. The disorder of the barrier function of aging skin not only has a negative impact on the external image and mental health, but is also closely related to the occurrence of many skin diseases.

[0003] Trumpet creeper is a commonly used Chinese medicine, mainly containing phenylethanol glycosides, phenolic acids, flavonoids and anthocyanins, pentacyclic triterpenes, volatile oils and other chemical components. Modern pharmacological studies have shown that trumpet creeper has anticoagulant, anti-inflammatory, analgesic, brain protective, antioxidant, and antidepressant effects. The solvents used in the commonly used trumpet creeper extraction technology are ethanol, water, and ethyl acetate, which have the disadvantages of low efficiency and poor extraction rate. Summary of the invention

[0004] In view of the deficiencies in the prior art, the object of the present invention is to provide a method for preparing a Trumpet Creeper extract and its product and application.

[0005] In order to achieve the purpose of the invention, the present invention adopts the following technical solutions:

[0006] In a first aspect, the present invention provides a method for preparing a trumpet creeper extract, the preparation method comprising:

[0007] (1) mixing the trumpet creeper with a solution containing a deep eutectic solvent, and performing reflux extraction to obtain an extract;

[0008] (2) filtering the extract to obtain a filtrate;

[0009] (3) concentrating the filtrate to obtain a concentrated solution;

[0010] (4) using a macroporous resin to adsorb the concentrated solution and then eluting to obtain an eluate;

[0011] (5) Concentrate and dry the eluate to obtain the product.

[0012] Trumpet creeper is the flower of the climbing vine trumpet creeper of Bignoniaceae and Campsis genus. The preparation method of the trumpet creeper extract of the present invention can effectively obtain antioxidant and anti-aging components such as polyphenols, and the extractant, dust, impurities, etc. therein can be removed to ensure the safety of the obtained trumpet creeper extract. The polyphenol content in the trumpet creeper extract obtained by the preparation method of the present invention can be stably greater than 30wt.%. The trumpet creeper extract obtained by the present invention can significantly remove DPPH free radicals, and its effect is equivalent to that of vitamin C; secondly, the obtained trumpet creeper extract can significantly promote the secretion of collagen I and collagen III, wherein the secretion of collagen I can be promoted by more than 3 times, and the secretion of collagen III can be promoted by more than 2 times, and has the effects of antioxidant and anti-aging, and can be used as an active substance in skin care products and medical auxiliary products.

[0013] Preferably, the solution containing a deep eutectic solvent comprises a deep eutectic solvent and water.

[0014] Preferably, the mass percentage of the deep eutectic solvent in the solution containing the deep eutectic solvent is 10-80%, for example, 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, 80%, etc. Other specific point values ​​within the above numerical range can be selected, which will not be described here one by one.

[0015] In a solution containing a deep eutectic solvent, the mass percentage of the deep eutectic solvent is very important for increasing the polyphenol content in the extract.

[0016] Preferably, the deep eutectic solvent is obtained by reacting a hydrogen bond donor and a hydrogen bond acceptor.

[0017] Preferably, the reaction temperature is 40-70°C and the reaction time is 1-2h.

[0018] The reaction temperature can be selected from 40°C, 45°C, 50°C, 55°C, 60°C, 65°C, 70°C, etc., and the reaction time can be selected from 1.1h, 1.2h, 1.3h, 1.4h, 1.5h, 1.6h, 1.7h, 1.8h, 1.9h, 2h, etc. Other specific point values ​​within the above numerical range can be selected, and they will not be described one by one here.

[0019] Preferably, the hydrogen bond donor comprises citric acid and / or urea.

[0020] Preferably, the hydrogen bond acceptor comprises any one of choline chloride, L-proline or betaine, or a combination of at least two thereof.

[0021] Preferably, the molar ratio of the hydrogen bond donor to the hydrogen bond acceptor is (1-6):1, wherein the specific point values ​​in (1-6) can be selected from 1, 1.5, 2, 2.5, 3, 3.5, 4, 4.5, 5, 5.5, 6, etc., and other specific point values ​​within the above numerical range can be selected, which will not be repeated here.

[0022] Preferably, the ratio of the trumpet creeper to the solution containing the deep eutectic solvent is 1 g:(5-20) mL, wherein the specific point values ​​in (5-20) can be selected from 5, 5.5, 6, 6.5, 7, 7.5, 8, 8.5, 9, 9.5, 10, 10.5, 11, 11.5, 12, 12.5, 13, 13.5, 14, 14.5, 15, 15.5, 16, 16.5, 17, 17.5, 18, 18.5, 19, 19.5, 20, etc. Other specific point values ​​within the above numerical range can be selected, and they will not be repeated here.

[0023] Preferably, the reflux extraction is carried out at a temperature of 60-100°C and for a time of 1-3 hours.

[0024] The temperature can be selected from 60°C, 65°C, 70°C, 75°C, 80°C, 85°C, 90°C, 95°C, 100°C, etc., and the time can be selected from 1h, 1.2h, 1.5h, 1.8h, 2h, 2.2h, 2.5h, 2.8h, 3h, etc. Other specific point values ​​within the above numerical range can be selected, and they will not be elaborated here.

[0025] Preferably, the number of reflux extractions is 1-3 times, for example, 1 time, 2 times, 3 times, etc. Other specific point values ​​within the above numerical range can be selected and will not be described one by one here.

[0026] Preferably, the filtration pressure is 50-150 mbar, for example, 50 mbar, 60 mbar, 70 mbar, 80 mbar, 90 mbar, 100 mbar, 110 mbar, 120 mbar, 130 mbar, 140 mbar, 150 mbar, etc. Other specific point values ​​within the above numerical range can be selected, which will not be described here one by one.

[0027] Preferably, the volume ratio of the filtrate to the concentrate is (3-10):1, wherein the specific point values ​​in (3-10) can be selected from 3, 3.5, 4, 4.5, 5, 5.5, 6, 6.5, 7, 7.5, 8, 8.5, 9, 9.5, 10, etc. Other specific point values ​​within the above numerical range can be selected and will not be described one by one here.

[0028] Preferably, the macroporous resin comprises AB-8 or D101.

[0029] Preferably, the mass ratio of the filtrate to the macroporous resin is 1:(30-50), wherein the specific point values ​​in (30-50) can be selected from 30, 32, 34, 36, 38, 40, 42, 44, 46, 48, 50, etc. Other specific point values ​​within the above numerical range can be selected, and they will not be described one by one here.

[0030] Preferably, the adsorption time is 6-18h, for example 6h, 7h, 8h, 9h, 10h, 11h, 12h, 13h, 14h, 15h, 16h, 17h, 18h, etc. Other specific point values ​​within the above numerical range can be selected, which will not be described here one by one.

[0031] Preferably, the elution comprises eluting with water, 10-25% ethanol aqueous solution, and 40-80% ethanol aqueous solution in sequence.

[0032] The mass percentage of ethanol in the 10-25% ethanol aqueous solution can be selected from 10%, 12%, 14%, 16%, 18%, 20%, 22%, 24%, 25% and the like; the mass percentage of ethanol in the 40-80% ethanol aqueous solution can be selected from 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, 80% and the like; other specific point values ​​within the above numerical range can be selected, which will not be described one by one here.

[0033] Preferably, the volume ratios of water, 10-25% ethanol aqueous solution, 40-80% ethanol aqueous solution and macroporous resin are independently (8-15):1, wherein the specific point values ​​in (8-15) can be selected from 8, 8.5, 9, 9.5, 10, 10.5, 11, 11.5, 12, 12.5, 13, 13.5, 14, 14.5, 15, etc. Other specific point values ​​within the above numerical range can be selected, and they will not be repeated here.

[0034] Preferably, the concentration pressure in step (5) is 50-150 mbar and the temperature is 40-60°C.

[0035] The pressure can be selected from 50mbar, 60mbar, 70mbar, 80mbar, 90mbar, 100mbar, 110mbar, 120mbar, 130mbar, 140mbar, 150mbar, etc., and the temperature can be selected from 40°C, 42°C, 44°C, 46°C, 48°C, 50°C, 52°C, 54°C, 56°C, 58°C, 60°C, etc. Other specific point values ​​within the above numerical range can be selected, and they will not be elaborated here one by one.

[0036] Preferably, the drying temperature is -80 to -50°C and the drying time is 48 to 72 hours.

[0037] The drying temperature can be selected from -80℃, -78℃, -75℃, -72℃, -70℃, -68℃, -65℃, -62℃, -60℃, -58℃, -55℃, -52℃, -50℃, etc., and the time can be selected from 48h, 52h, 56h, 60h, 64h, 68h, 72h, etc. Other specific point values ​​within the above numerical range can be selected, so they will not be described one by one here.

[0038] In a second aspect, the present invention provides a Trumpet Creeper extract prepared according to the preparation method of the Trumpet Creeper extract described in the first aspect.

[0039] In a third aspect, the present invention provides a use of the Trumpet Creeper extract according to the second aspect in the preparation of an anti-aging product.

[0040] The trumpet creeper extract of the present invention can significantly promote the secretion of collagen I and collagen III, and can promote the secretion of collagen I by more than 3 times, and promote the secretion of collagen III by more than 2 times.

[0041] In a fourth aspect, the present invention provides a use of the Trumpet Creeper extract according to the second aspect in the preparation of an antioxidant product.

[0042] Preferably, the product comprises a cosmetic or a health product.

[0043] Preferably, the mass percentage of the trumpet creeper extract in the product is 0.005-0.02%, for example, 0.005%, 0.006%, 0.007%, 0.008%, 0.009%, 0.01%, 0.011%, 0.012%, 0.013%, 0.014%, 0.015%, 0.016%, 0.017%, 0.018%, 0.019%, 0.02%, etc. Other specific point values ​​within the above numerical range can be selected, which will not be described here one by one.

[0044] Compared with the prior art, the present invention has the following beneficial effects:

[0045] (1) The present invention adopts the deep eutectic extraction method for the first time to obtain the trumpet creeper extract;

[0046] (2) The preparation method of the trumpet creeper extract of the present invention can effectively obtain antioxidant and anti-aging components such as polyphenols, and can remove the extractant, dust, impurities, etc. therein to ensure the safety of the obtained trumpet creeper extract;

[0047] (3) The polyphenol content in the trumpet creeper extract obtained by the preparation method of the present invention can be stably greater than 30 wt.%, which can ensure the reliability of its quality and facilitate commercialization;

[0048] (4) The trumpet creeper extract obtained by the preparation method of the present invention can significantly scavenge DPPH free radicals, and its effect is equivalent to that of vitamin C. Secondly, the trumpet creeper extract can significantly promote the secretion of collagen I and collagen III, wherein the secretion of collagen I can be promoted by more than 3 times, and the secretion of collagen III can be promoted by more than 2 times. It has antioxidant and anti-aging effects, and can be used as an active substance in skin care products and medical auxiliary products. BRIEF DESCRIPTION OF THE DRAWINGS

[0049] Figure 1 The present invention is a flow chart of the preparation method of the trumpet creeper extract. DETAILED DESCRIPTION

[0050] The technical solution of the present invention is further described below by specific implementation methods. It should be understood by those skilled in the art that the embodiments are only to help understand the present invention and should not be regarded as specific limitations of the present invention.

[0051] Preparation Example 1

[0052] This preparation example provides a deep eutectic solvent, which is obtained by reacting betaine and urea, and the molar ratio of betaine to urea is 1:2.

[0053] The preparation method is as follows: betaine and urea are mixed and stirred at 60°C for 1 hour.

[0054] Preparation Example 2

[0055] This preparation example provides a deep eutectic solvent, which is obtained by reacting choline chloride and citric acid, and the molar ratio of choline chloride to citric acid is 1:2.

[0056] The preparation method is as follows: mix choline chloride and citric acid and stir at 60°C for 1 hour.

[0057] Preparation Example 3

[0058] This preparation example provides a deep eutectic solvent, which is obtained by reacting L-proline and urea, and the molar ratio of L-proline to urea is 1:6.

[0059] The preparation method is as follows: L-proline and urea are mixed and stirred at 60°C for 1 hour.

[0060] Preparation Example 4

[0061] This preparation example provides a deep eutectic solvent, which is obtained by reacting betaine and citric acid, and the molar ratio of betaine to citric acid is 1:1.

[0062] The preparation method is as follows: betaine and citric acid are mixed and stirred at 60°C for 1 hour.

[0063] Example 1

[0064] This embodiment provides a method for preparing a trumpet creeper extract, and the preparation flow chart thereof is as follows: Figure 1 As shown, the preparation method comprises:

[0065] (1) drying the raw material of trumpet creeper, removing impurities, and crushing to obtain trumpet creeper powder;

[0066] (2) Mixing the trumpet creeper powder with a solution containing 40% of the deep eutectic solvent described in Preparation Example 1 at a ratio of 1:10 g / mL, reflux extraction at 80° C. for 2 h, extracting twice, and combining the obtained extracts;

[0067] (3) filtering the obtained filtrate under reduced pressure to obtain a filtrate;

[0068] (4) Concentrating the filtrate obtained in step (3) under reduced pressure until the volume is 1 / 5 of the extract in step (2), thereby obtaining a concentrated solution;

[0069] (5) Take macroporous resin AB-8, activate it and load it into the column. The mass ratio of filtrate to macroporous resin is 1:40. After the concentrated solution is adsorbed on the column for 16 hours, it is first eluted with deionized water for 10 column volumes, and the obtained eluate is discarded; then, 20% ethanol aqueous solution is used as the impurity removal solvent to elute for 10 column volumes, and the obtained eluate is discarded. Finally, 50% ethanol aqueous solution is used to elute for 10 column volumes, and the enriched eluate is retained for later use;

[0070] (6) The eluate is concentrated under reduced pressure and freeze-dried to obtain the product.

[0071] Example 2

[0072] This embodiment provides a method for preparing a trumpet creeper extract, the preparation method comprising:

[0073] (1) drying the raw material of trumpet creeper, removing impurities, and crushing to obtain trumpet creeper powder;

[0074] (2) Mixing the trumpet creeper powder with a solution containing 40% of the deep eutectic solvent described in Preparation Example 1 at a ratio of 1:5 g / mL, reflux extraction at 60° C. for 3 h, extracting once, and combining the obtained extracts;

[0075] (3) filtering the obtained filtrate under reduced pressure to obtain a filtrate;

[0076] (4) Concentrating the filtrate obtained in step (3) under reduced pressure until the volume is 1 / 3 of the extract in step (2), thereby obtaining a concentrated solution;

[0077] (5) Take macroporous resin AB-8, activate it and load it into the column. The mass ratio of filtrate to macroporous resin is 1:30. After the concentrated solution is adsorbed on the column for 18 hours, it is first eluted with deionized water for 15 column volumes, and the obtained eluate is discarded; then, 10% ethanol aqueous solution is used as the impurity removal solvent to elute for 15 column volumes, and the obtained eluate is discarded. Finally, 40% ethanol aqueous solution is used to elute for 15 column volumes, and the enriched eluate is retained for later use;

[0078] (6) The eluate is concentrated under reduced pressure and freeze-dried to obtain the product.

[0079] Example 3

[0080] This embodiment provides a method for preparing a trumpet creeper extract, the preparation method comprising:

[0081] (1) drying the raw material of trumpet creeper, removing impurities, and crushing to obtain trumpet creeper powder;

[0082] (2) Mixing the trumpet creeper powder with a solution containing 40% of the deep eutectic solvent described in Preparation Example 1 at a ratio of 1:20 g / mL, reflux extraction at 100° C. for 1 h, extracting three times, and combining the obtained extracts;

[0083] (3) filtering the obtained filtrate under reduced pressure to obtain a filtrate;

[0084] (4) Concentrating the filtrate obtained in step (3) under reduced pressure until the volume is 1 / 10 of the extract in step (2), thereby obtaining a concentrated solution;

[0085] (5) Take macroporous resin AB-8, activate it and load it into the column. The mass ratio of filtrate to macroporous resin is 1:50. After the concentrated solution is adsorbed on the column for 6 hours, it is first eluted with deionized water for 8 column volumes, and the obtained eluate is discarded; then, 25% ethanol aqueous solution is used as the impurity removal solvent to elute for 8 column volumes, and the obtained eluate is discarded. Finally, 80% ethanol aqueous solution is used to elute for 8 column volumes, and the enriched eluate is retained for later use;

[0086] (6) The eluate is concentrated under reduced pressure and freeze-dried to obtain the product.

[0087] Example 4

[0088] This embodiment provides a method for preparing a trumpet creeper extract, which differs from embodiment 1 only in that step (2) is "mixing the trumpet creeper powder with a solution containing 40% of the deep eutectic solvent described in preparation example 2 in a ratio of 1:10 g / mL, extracting under reflux at 80° C. for 2 h, extracting twice, and combining the obtained extracts", and other operations remain unchanged.

[0089] Example 5

[0090] This embodiment provides a method for preparing a trumpet creeper extract, which differs from embodiment 1 only in that step (2) is "mixing the trumpet creeper powder with a solution containing 40% of the deep eutectic solvent described in preparation example 3 in a ratio of 1:10 g / mL, reflux extraction at 80° C. for 2 h, extracting twice, and combining the obtained extracts", and other operations remain unchanged.

[0091] Example 6

[0092] This embodiment provides a method for preparing a trumpet creeper extract, which differs from embodiment 1 only in that step (2) is "mixing the trumpet creeper powder with a solution containing 40% of the deep eutectic solvent described in preparation example 4 at a ratio of 1:10 g / mL, reflux extraction at 80° C. for 2 h, extracting twice, and combining the obtained extracts", and other operations remain unchanged.

[0093] Example 7

[0094] This embodiment provides a method for preparing a trumpet creeper extract, which differs from embodiment 1 only in that step (2) is "mixing the trumpet creeper powder with a solution containing 10% of the deep eutectic solvent described in preparation example 1 at a ratio of 1:10 g / mL, extracting under reflux at 80° C. for 2 h, extracting twice, and combining the obtained extracts", and other operations remain unchanged.

[0095] Example 8

[0096] This embodiment provides a method for preparing a trumpet creeper extract, which differs from embodiment 1 only in that step (2) is "mixing the trumpet creeper powder with a solution containing 80% of the deep eutectic solvent described in preparation example 1 at a ratio of 1:10 g / mL, extracting under reflux at 80° C. for 2 h, extracting twice, and combining the obtained extracts", and other operations remain unchanged.

[0097] Comparative Example 1

[0098] This comparative example provides a method for preparing a trumpet creeper extract, the preparation method comprising:

[0099] (1) drying the raw material of trumpet creeper, removing impurities, and crushing to obtain trumpet creeper powder;

[0100] (2) Mixing the trumpet creeper powder with a 50% ethanol solution, extracting under reflux at 80°C for 2 h, extracting twice, and combining the obtained extracts;

[0101] (3) filtering the obtained filtrate under reduced pressure to obtain a filtrate;

[0102] (4) Concentrating the filtrate obtained in step (3) under reduced pressure until the volume is 1 / 5 of the extract in step (2), thereby obtaining a concentrated solution;

[0103] (5) freeze-drying the concentrated solution in step (4) to obtain the product.

[0104] Comparative Example 2

[0105] This comparative example provides a method for preparing a trumpet creeper extract, which differs from Example 1 only in that step (2) is "mixing the trumpet creeper powder with a 50% ethanol solution, extracting under reflux at 80° C. for 2 h, extracting twice, and combining the obtained extracts", and other operations remain unchanged.

[0106] Comparative Example 3

[0107] This comparative example provides a method for preparing a trumpet creeper extract, and the reference is: "Optimization of microwave extraction process of trumpet creeper polyphenols and its antioxidant research", Zheng Qian et al., Chemical Reagents, 2021, 43(09).

[0108] The method comprises: picking the trumpet creeper, placing it in an oven, drying it at 60°C, crushing it, and sieving it. Accurately weighing 100g of the trumpet creeper powder, adding 40% ethanol, the material-liquid ratio is 32g / mL, the microwave extraction power is 281W, and the extraction time is 37s.

[0109] Comparative Example 4

[0110] This comparative example provides a method for preparing a trumpet creeper extract, and the reference is: patent CN111110713B.

[0111] The method comprises: placing choline chloride and glycerol in a water bath at 80°C in a molar ratio of 1:2 to synthesize an extraction solvent, mixing 100 g of trumpet creeper with the extraction solvent in a mass ratio of 1:6, performing ultrasonic extraction for 40 minutes, taking a supernatant after centrifugation, eluting the supernatant with an HP-20 macroporous resin to remove the extraction solvent, eluting with 0.1% formic acid water and 50% ethanol solution in sequence, collecting a 50% ethanol elution fraction, and concentrating and drying to obtain polyphenol compounds in the trumpet creeper.

[0112] Test Example 1

[0113] Polyphenol content test

[0114] Test method: Referring to GBT8313-2018, gallic acid was used as the reference substance, and the polyphenol content in the sample was determined by spectrophotometry. The specific experimental steps were as follows: prepare 200 μg / mL sample, add Folin phenol reagent and sodium carbonate reagent in sequence, react for 1 hour in the dark, and measure the sample absorbance at 760 nm. Using gallic acid as the standard reference substance, a standard curve was prepared, and the polyphenol content was obtained by calculation.

[0115] Gallic acid standard curve: Y = 0.228X + 0.0853, R 2 =0.9992

[0116] Table 1

[0117]

[0118]

[0119] It can be seen from the data in Table 1 that the Trumpet Creeper extract prepared by the preparation method of the present invention has a high polyphenol content, and the selection of hydrogen bond donors and hydrogen bond acceptors of the deep eutectic solvent will affect the polyphenol content, and the concentration of the deep eutectic solvent will also affect the polyphenol content.

[0120] Test Example 2

[0121] Antioxidant activity test

[0122] Test method:

[0123] The antioxidant capacity of the trumpet creeper extract was evaluated by the 2,2-diphenyl-1-pyridohydrazine (DPPH) free radical scavenging experiment. The specific test method was as follows: using VC (vitamin C) as a positive control, 0.5 mg / mL of the trumpet creeper extract was prepared as the stock solution, and 8 half-diluted concentrations were added, DPPH reagent was added, shaken and reacted at room temperature in the dark for 30 minutes, and the absorbance was measured at 517 nm.

[0124] The DPPH free radical scavenging rate formula is:

[0125]

[0126] OD L Determine the absorbance for the sample experimental group

[0127] OD LB Determine the absorbance of the sample blank

[0128] OD C Determine absorbance for the solvent experiment group

[0129] OD CB Determine the absorbance for the solvent blank group

[0130] Table 2

[0131]

[0132]

[0133] From the data in Table 2, we can see that vitamin C has an IC value of scavenging DPPH free radicals. 50 The value is 11.40 μg / mL. The IC value of the DPPH free radical scavenging effect of the trumpet creeper extract prepared in Example 1 is 50The value is 16.69 μg / mL, and its DPPH free radical scavenging effect is equivalent to that of vitamin C.

[0134] Test Example 3

[0135] Anti-aging effect test

[0136] Test method:

[0137] The experiment was set up with H2O2 group and H2O2+Campsicolor extract group (100μg / mL). After HDFa cells were treated with H2O2 for 2h, the test substances were added and cultured overnight. The supernatant was collected and the secretion of human type I procollagen (PC-1) and type III collagen (COL-3) was detected by ELISA kit.

[0138] Table 3

[0139] sample PC-1 relative content COL-3 relative content Example 1 3.33 2.34 Example 2 3.01 2.16 Example 3 3.04 2.08 Example 4 1.62 1.34 Example 5 1.88 1.42 Example 6 2.55 1.29 Example 7 2.73 1.72 Example 8 3.14 1.81 Comparative Example 1 1.64 1.41 Comparative Example 2 1.96 1.63 Comparative Example 3 1.32 1.25 Comparative Example 4 1.89 1.62 <![CDATA[H2O2]]> 1.00 1.00

[0140] As shown in the results of Table 3, compared with the control group, the trumpet creeper extract prepared in Examples 1-3 can significantly promote the secretion of collagen I and collagen III, wherein the secretion of collagen I can be promoted by more than 3 times, and the secretion of collagen III can be promoted by more than 2 times, indicating that the trumpet creeper extract prepared by the present invention can delay skin aging by significantly promoting collagen secretion.

[0141] Test Example 4

[0142] With reference to the Technical Specification for Safety of Cosmetics (2015), the trumpet creeper extract prepared in Examples 1-3 was subjected to acute eye irritation / corrosion tests, skin irritation / corrosion tests, skin allergy tests, skin phototoxicity tests, hormone, pesticide residue, microorganism, heavy metal and H-Clat sensitization tests to comprehensively evaluate the safety of the trumpet creeper extract.

[0143] Table 4

[0144] Example 1 Example 2 Example 3 Multiple skin irritations Non-irritating Non-irritating Non-irritating Acute eye irritation Non-irritating Non-irritating Non-irritating Skin allergies No skin allergy No skin allergy No skin allergy Skin phototoxicity No phototoxicity No phototoxicity No phototoxicity hormone Not detected Not detected Not detected Pesticide residues Not detected Not detected Not detected microorganism qualified qualified qualified heavy metal qualified qualified qualified H-Clat Allergenicity Test Non-allergenic Non-allergenic Non-allergenic

[0145] The test results are shown in Table 4. The Trumpet Creeper extracts obtained by deep eutectic extraction of the extracts obtained in Examples 1-3 are non-irritating, non-skin allergic, non-sensitizing and non-phototoxic, and no hormones, pesticide residues, etc. are detected.

[0146] The applicant declares that the present invention uses the above-mentioned embodiments to illustrate the preparation method of a trumpet creeper extract of the present invention, its product and application, but the present invention is not limited to the above-mentioned embodiments, that is, it does not mean that the present invention must rely on the above-mentioned embodiments to be implemented. Those skilled in the art should understand that any improvement of the present invention, equivalent replacement of various raw materials of the product of the present invention, addition of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

[0147] The preferred embodiments of the present invention are described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the technical concept of the present invention, a variety of simple modifications can be made to the technical solution of the present invention, and these simple modifications all belong to the protection scope of the present invention.

[0148] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable manner without contradiction. In order to avoid unnecessary repetition, the present invention will not further describe various possible combinations.

Claims

1. A method for preparing a Trumpet Creeper extract, characterized in that: The preparation method comprises: (1) mixing the trumpet creeper with a solution containing a deep eutectic solvent, and performing reflux extraction to obtain an extract; The solution containing the deep eutectic solvent comprises a deep eutectic solvent and water; the mass percentage of the deep eutectic solvent in the solution containing the deep eutectic solvent is 10-80%; The deep eutectic solvent is obtained by reacting a hydrogen bond donor and a hydrogen bond acceptor; the hydrogen bond donor includes citric acid and / or urea; the hydrogen bond acceptor includes any one or a combination of at least two of choline chloride, L-proline or betaine; the molar ratio of the hydrogen bond donor to the hydrogen bond acceptor is (1-6):1; The ratio of the trumpet creeper to the solution containing the deep eutectic solvent is 1 g: (5-20) mL; (2) filtering the extract to obtain a filtrate; (3) concentrating the filtrate to obtain a concentrated solution; (4) using a macroporous resin to adsorb the concentrated solution and then eluting to obtain an eluate; (5) Concentrate and dry the eluate to obtain the product.

2. The method for preparing the Trumpet Creeper extract according to claim 1, characterized in that: The reaction temperature is 40-70°C and the reaction time is 1-2h.

3. The method for preparing the Trumpet Creeper extract according to claim 1, characterized in that: The temperature of the reflux extraction is 60-100° C., and the time is 1-3 h.

4. The method for preparing the Trumpet Creeper extract according to claim 1, characterized in that: The number of reflux extraction is 1-3 times.

5. The method for preparing the Trumpet Creeper extract according to claim 1, characterized in that: The filtration pressure is 50-150 mbar.

6. The method for preparing the Trumpet Creeper extract according to claim 1, characterized in that: The volume ratio of the filtrate to the concentrated solution is (3-10):

1.

7. The method for preparing the Trumpet Creeper extract according to claim 1, characterized in that: The macroporous resin includes AB-8 or D101.

8. The method for preparing the Trumpet Creeper extract according to claim 1, characterized in that: The mass ratio of the concentrated solution to the macroporous resin is 1:(30-50).

9. The method for preparing the Trumpet Creeper extract according to claim 1, characterized in that: The adsorption time is 6-18h.

10. The method for preparing the Trumpet Creeper extract according to claim 1, characterized in that: The elution comprises eluting with water, 10-25% ethanol aqueous solution, and 40-80% ethanol aqueous solution in sequence.

11. The method for preparing the Trumpet Creeper extract according to claim 10, characterized in that: The volume ratio of water, 10-25% ethanol aqueous solution, 40-80% ethanol aqueous solution and macroporous resin is independently (8-15):

1.

12. The method for preparing the Trumpet Creeper extract according to claim 1, characterized in that: The concentration pressure in step (5) is 50-150 mbar and the temperature is 40-60°C.

13. The method for preparing the Trumpet Creeper extract according to claim 1, characterized in that: The drying is freeze drying, the temperature is -80 to -50°C, and the time is 48 to 72 hours.

14. The Trumpet Creeper extract prepared according to the method for preparing the Trumpet Creeper extract according to any one of claims 1 to 13.

15. Use of the Trumpet Creeper extract according to claim 14 in preparing anti-aging products.

16. Use of the Trumpet Creeper extract according to claim 14 in preparing antioxidant products.

17. The use according to claim 15 or 16, characterized in that: The mass percentage of the trumpet creeper extract in the product is 0.005-0.02%.

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