Gambiered canton gauze powder as well as preparation method and application thereof

By alkaline dissolving Xiangyunsha raw materials in alkaline solution and adding acid treatment, Xiangyunsha powder with high tyrosinase inhibition rate was prepared, which solved the problem of complex and high cost of Xiangyunsha preparation process and achieved its The efficient application of skin care products has significantly improved the activity and biological activity of tyrosinase.

CN119157811APending Publication Date: 2024-12-20SERICULTURAL &AGRI FOOD RESEARCH INSTITUTE GUANGDONG ACADEMY OF AGRICULTURAL SCIENCES
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Patent Information

Application Number
CN202411259458.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-09-10
Publication Date
2024-12-20

AI Technical Summary

Technical Problem

The preparation process of Xiangyunya is complex and costly, and the foot material has not been used in high value. The production cost of existing two-way fermentation broth preparation methods is also relatively high, making it difficult to expand its application in the field of skin care products.

Method used

By alkalinely dissolving the Xiangyunsha raw material in alkali solution, neutralizing acid, dialysis and drying, Xiangyunsha powder with high tyrosinase inhibition is prepared, and tannin flavonoids and silk proteins in the potato shreds are used. Interactions to improve their biological activity.

Benefits of technology

It significantly improves the tyrosinase activity, antioxidant ability, anti-ultraviolet ability and moisturizing properties of Xiangyunsha powder, and becomes an effective cosmetic raw material for whitening, sun protection, anti-oxidation and moisturizing.

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Abstract

The invention discloses gambiered canton gauze powder as well as a preparation method and application thereof, gambiered canton gauze raw materials are subjected to alkaline hydrolysis in an alkaline solution, after the gambiered canton gauze raw materials are completely dissolved, acid is added for neutralization, and then dialysis and drying are performed to prepare the gambiered canton gauze powder. Compared with common silk powder, fibroin and sericin, the gambiered canton gauze powder has the advantages that the tyrosinase activity is improved to 94% from 14.03%-18.83%, the oxidation resistance is improved to 93% from 0-15%, the ultraviolet resistance is improved to 97% from 24%-46%, and the moisture retention is improved to 10.39% from 1.65%-5.65%. The gambiered canton gauze powder can be used as a tyrosinase inhibitor, is applied to cosmetics, and is beneficial to high-value utilization of gambiered canton gauze leftovers.
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Description

Technical Field

[0001] The invention belongs to the field of skin care products and relates to Xiangyunsha powder and a preparation method and application thereof. Background Art

[0002] Xiangyunsha is a kind of silk fabric, which is known as "soft gold" in the textile field. It was included in the national intangible cultural heritage in 2008. The raw and auxiliary materials for preparing Xiangyunsha include grey silk (pure silk fabric), yam (Dioscorea, Dioscorea, the tuber of a perennial sturdy vine) and river mud (rich in ferrous ions, gray-black in color, no bad smell, delicate to the touch, and does not contain debris that affects use). The process includes the preparation of grey silk, the preparation of yam liquid, soaking in yam water, sunning yam, sprinkling yam, sealing yam water once, boiling silk once, sealing yam water twice, boiling silk twice, sealing yam water three times (commonly known as "starting"), mud passing, cleaning river mud, sealing yam water four times (commonly known as "re-black"), and misting. It can be seen that the preparation process of Xiangyunsha is complicated and the cost is high. At the same time, the scraps after making clothing and bags have not been used at a high value.

[0003] Chinese patent 202211433046.3 provides a medicinal culture medium, a bidirectional fermentation liquid with tyrosinase inhibition effect, a preparation method, and an application. The medicinal culture medium includes Schisandra powder, a carbon source, malt extract powder, and a nitrogen source. By using the medicinal culture medium to inoculate Ganoderma lucidum liquid for bidirectional fermentation, the tyrosinase inhibition rate of the obtained bidirectional fermentation liquid is as high as 99.5%. The bidirectional fermentation liquid can effectively inhibit the production of melanin and can be used as a raw material for cosmetics. Since this method is mainly prepared by strain fermentation process, the production cost is relatively high.

[0004] Therefore, using the leftovers of Xiangyunsha as raw materials to prepare raw materials with a high inhibition rate on tyrosinase and expand its application in the field of skin care products are of great significance to promoting the development of the Xiangyunsha industry. Summary of the invention

[0005] In order to solve the above technical problems, the present invention provides a Xiangyunsha powder having a high inhibition rate on tyrosinase, and a preparation method and application thereof.

[0006] The technical solution of the present invention is as follows:

[0007] A method for preparing Xiangyunsha powder comprises the following steps: subjecting a Xiangyunsha raw material to alkaline hydrolysis in an alkaline solution, adding acid to neutralize the raw material after the raw material is completely dissolved, and then dialyzing and drying the raw material to prepare the Xiangyunsha powder.

[0008] Preferably, the alkaline solution is mainly composed of sodium hydroxide solution and / or potassium hydroxide solution.

[0009] Preferably, the alkaline solution is supplemented with a urea aqueous solution.

[0010] Preferably, the concentration of the sodium hydroxide solution and / or potassium hydroxide solution is 0.05-2.0 mol / L, and the concentration of the urea aqueous solution is 3-15 mol / L.

[0011] Preferably, the concentration of the sodium hydroxide solution and / or potassium hydroxide solution is 1.2±0.2 mol / L, and the concentration of the urea aqueous solution is 8±2 mol / L.

[0012] Preferably, the acid is dilute hydrochloric acid, the pH value of the solution is adjusted to 7-8, and the salt (NaCl and / or KCl) is removed by dialysis. The dialysis is followed by concentration, the concentration is rotary evaporation concentration, and the drying is freeze drying or spray drying.

[0013] Preferably, the Xiangyunsha raw material is the leftovers of Xiangyunsha.

[0014] The Xiangyunsha powder prepared by the method is used as a tyrosinase inhibitor.

[0015] Preferably, the Xiangyunsha powder is used in cosmetics.

[0016] The mechanism of action of the present invention may be that the tannin flavonoids in Dioscorea paniculate and silk protein interact with each other, and are combined through intermolecular forces such as chemical bonds, hydrogen bonds, π-π stacking and hydrophobic interactions, so that the Xiangyunsha powder sample exerts outstanding synergistic and stronger biological activity. No related research has been reported yet.

[0017] Compared with the prior art, the present invention has the following beneficial effects:

[0018] (1) Compared with ordinary silk powder, fibroin and sericin, the tyrosinase activity of the Xiangyunsha powder of the present invention is increased from 14.03% to 18.83% to 94%, the antioxidant capacity is increased from 0-15% to 93%, the anti-ultraviolet capacity is increased from 24% to 46% to 97%, and the moisture retention is increased from 1.65% to 5.65% to 10.39%.

[0019] (2) The Xiangyunsha powder prepared by the present invention is used as a core raw material or a composite raw material for microcapsule wall materials to prepare cosmetics, including skin care products, and has whitening, sun protection, anti-oxidation and moisturizing effects. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 These are scanning electron microscope images of different samples, (A) silk powder, (B) Xiangyunsha powder.

[0021] Figure 2 Figure 2 is the tyrosinase inhibition activity of different samples.

[0022] Figure 3 The antioxidant activity of different samples.

[0023] Figure 4 The moisturizing performance diagram of different samples.

[0024] Figure 5 This is a graph showing the UV absorption resistance of different samples. DETAILED DESCRIPTION

[0025] The present invention is further described in detail below in conjunction with specific examples, but the embodiments of the present invention are not limited thereto. For process parameters not specifically noted, conventional techniques may be used. The Xiangyunsha raw material used in this experiment comes from Guangdong Lunjiao Silkworm Seed Farm Co., Ltd.

[0026] Example 1

[0027] A method for preparing Xiangyunsha powder, comprising collecting the scraps of Xiangyunsha after making clothes and bags, and preparing the Xiangyunsha powder through alkaline hydrolysis, neutralization, dialysis, concentration, and freeze drying. The specific steps are as follows:

[0028] (1) Dissolution: Weigh 1 g of Xiangyunsha sample and dissolve it in a solution of 1.2 mol / L sodium hydroxide and 8 mol / L urea for 0.5 h;

[0029] (2) Neutralization: Use dilute hydrochloric acid to neutralize sodium hydroxide to a pH of 7;

[0030] (3) Dialysis: remove NaCl;

[0031] (4) Concentration: rotary evaporation concentration;

[0032] (5) Drying: Freeze-dry the sample (-88°C, 5.7Pa, 72h) to obtain Xiangyunsha powder.

[0033] The Xiangyunsha powder prepared in Example 1 was subjected to the following experiment. Ordinary silk powder, silk fibroin powder and sericin powder were used as controls, and the above controls were all from Hangzhou Linran Biotechnology Co., Ltd.

[0034] 1. Tyrosinase inhibitory activity

[0035] In a phosphate buffer system at pH 6.8, a series of different samples (Xiangyunsha powder, ordinary silk powder, sericin powder, and silk fibroin powder) were added to keep the concentration of tyrosinase constant (0.2 mg / ml), mixed, incubated in a constant temperature water bath at 37°C for 10 min, added 1 mg / mL L-DOPA, mixed, and immediately transferred 200 μL of the reaction solution from each tube into a 96-well plate, and the absorbance was measured at 475 nm using an ELISA reader. The tyrosinase inhibition rate was calculated according to the following formula.

[0036] Inhibition rate (%) = (1-(T-T0) / (C-C0)) × 100% (1)

[0037] (1) Where: T, sample absorbance; T0, sample background absorbance; C, absorbance of tyrosinase and DOPA reaction without sample; C0, solution background absorbance.

[0038] The tyrosinase inhibition rates of silk, sericin, fibroin and Xiangyunsha were 14.03%, 14.25%, 18.83% and 94.50%, respectively.

[0039] 2. Antioxidant Activity

[0040] (1) Total antioxidant activity

[0041] Fe 3+ The total antioxidant capacity of the sample is determined by the reduction kit. The determination method refers to the kit instructions and the total antioxidant capacity is calculated. The total antioxidant capacity is expressed by the concentration of the FeSO4 standard solution. If the OD value of the serum is the same as the OD value of 1mM FeSO4, the total antioxidant capacity of the sample is 1mM.

[0042] T-AOC (mM) = (sample OD value - control OD value) × total volume of reaction solution / sampling volume × sample dilution multiple. The OD value was measured at a wavelength of 520 nm using an ultraviolet spectrophotometer.

[0043] The sample concentrations were all 10 mg / mL, and the total antioxidant capacities of silk, sericin, fibroin and xiangyunsha were 3.4 mM, 15 mM, 0 mM and 93 mM, respectively.

[0044] 3. Moisturizing

[0045] The sample was dried in a closed oven at 45°C for 24 h. The dried sample was exposed to air at a relative humidity of 65% at 25°C for 24 h, and its hygroscopicity was measured relative to the dry weight and expressed in %, hygroscopicity = (M 1- M0) / M0×100%.

[0046] The results showed that the moisture absorption rates of silk, sericin, fibroin and Xiangyun yarn were 4.48%, 1.65%, 5.65%, and 10.39%, respectively.

[0047] 4. Anti-ultraviolet absorption ability

[0048] The absorption spectrum was measured using an enzyme-labeled instrument. The sample was resuspended in deionized water at a mass-volume ratio of 1:1000, and ultrasonically dispersed for 10 minutes using an ultrasonic cleaner. 150 μL was aspirated into a 96-well plate, and a full-wavelength scanning absorption spectrum was obtained at a wavelength of 230-400 nm using an enzyme-labeled instrument. The OD value was recorded, and the absorption spectrum of pure deionized water was measured as the background at the same time. The conversion relationship between the OD value and the transmittance was converted to the transmittance using the formula: OD = lg (1 / transmittance).

[0049] The light transmittance of silk, sericin, fibroin and xiangyun yarn in the wavelength range of 280-400nm are 76%, 54%, 71% and 3% respectively, and the UV shielding power increases from 24%-46% to 97%.

[0050] 5. Scanning Electron Microscopy (SEM)

[0051] SEM was used to analyze the structural characteristics of Xiangyunsha powder. A certain amount of sample was sprinkled on a sample platform with double-sided tape, and a capillary was used to slightly compact it so that part of the powder was trapped in the double-sided tape. After scraping off the surface powder with a blade, the excess sample was blown off, and then placed in an ion sputtering instrument and sprayed with gold at a current of 10mA to coat the surface of the material with a layer of platinum film. The morphological structure of the sample was then observed with SEM. For details, see Figure 1 .

[0052] Example 2

[0053] The difference between the present invention and Example 1 is that spray drying (air inlet temperature 170°C, air inlet volume 0.1m 3 / min) to obtain the product.

[0054] Example 3

[0055] The difference between the present invention and Example 1 is that the solution is dissolved in 1.8 mol / L sodium hydroxide (without adding urea) and the dissolution time is 45 min.

[0056] Comparative Example 1

[0057] The difference between the present invention and Example 1 is that the raw materials are the leftovers of mulberry silk cloth (not Xiangyun yarn) sourced from Guangdong Zhongshan Silk Import and Export Group Co., Ltd.

[0058] Comparative Example 2

[0059] The difference between the present invention and Example 1 is that the raw materials are the leftovers of chiffon (chemical fiber) cloth, which comes from Guangdong Zhongshan Silk Import and Export Group Co., Ltd.

[0060] The experimental test results of the above embodiments are detailed in Table 1.

[0061] Table 1

[0062]

[0063] The above embodiments are preferred implementation modes of the present invention, but the implementation modes of the present invention are not limited to the above embodiments. Any other changes, modifications, substitutions, combinations, and simplifications that do not deviate from the spirit and principles of the present invention should be equivalent replacement methods and are included in the protection scope of the present invention.

Claims

1. A method for preparing Xiangyunsha powder, characterized in that: The Xiangyunsha raw material is subjected to alkaline hydrolysis in an alkaline solution, and after being completely dissolved, acid is added for neutralization, and then dialyzed and dried to prepare the Xiangyunsha powder.

2. The preparation method according to claim 1, characterized in that: The alkaline solution includes sodium hydroxide solution and / or potassium hydroxide solution.

3. The preparation method according to claim 2, characterized in that: The alkaline solution also includes a urea aqueous solution.

4. The preparation method according to claim 3, characterized in that: The concentration of the sodium hydroxide solution and / or potassium hydroxide solution is 0.05-2.0 mol / L, and the concentration of the urea aqueous solution is 3-15 mol / L.

5. The preparation method according to claim 4, characterized in that: The concentration of the sodium hydroxide solution and / or potassium hydroxide solution is 1.2±0.2 mol / L, and the concentration of the urea aqueous solution is 8±2 mol / L.

6. The preparation method according to any one of claims 1 to 5, characterized in that: The acid is dilute hydrochloric acid, the pH value of the solution is adjusted to 7-8, and the salt is removed by dialysis. After the dialysis, concentration is performed, and the concentration is rotary evaporation concentration. The drying is freeze drying or spray drying.

7. The preparation method according to any one of claims 1 to 5, characterized in that: The Xiangyunsha raw material is the leftovers of Xiangyunsha.

8. Xiangyunsha powder obtained by the method according to any one of claims 1 to 7.

9. Use of the Xiangyunsha powder according to claim 8 as a tyrosinase inhibitor.

10. The use according to claim 9, characterized in that: Application of the Xiangyunsha powder in cosmetics.