Composite edible fungus granule emulsified water-in-oil-in-water emulsion and preparation method thereof

Abstract

A compound edible fungus granule emulsion, comprising water-in-oil-in-water, and its preparation method, relates to the field of skincare products. The emulsion of this invention comprises purified water, olive oil, pine nut oil, ultrafine black fungus powder, ultrafine matsutake mushroom powder, black fungus polysaccharide, matsutake mushroom polysaccharide, black fungus melanin, ascorbic acid glucoside, and vitamin E. This invention utilizes ultrafine black fungus and matsutake mushroom powder, through appropriate formulation and processing, to develop a compound edible fungus granule emulsion, comprising water-in-oil-in-water, comprising water-in-oil, comprising water-in-oil, comprising water-in-oil, comprising emulsion. The raw materials of this emulsion are entirely composed of substances from the edible fungi themselves, are purely natural, non-toxic, and harmless, avoiding the safety hazards of adding other chemical substances, and the emulsion is green and natural.

Description

Technical Field

[0001] This invention belongs to the field of skin care products, specifically relating to a compound edible fungus granule emulsion water-in-oil-in-water emulsion and its preparation method. Background Technology

[0002] Edible fungi such as black fungus and matsutake mushrooms not only have high nutritional value but also excellent skincare benefits. Black fungus contains polysaccharides that not only moisturize but also repair, protect against UV rays, and slow aging. Matsutake mushrooms contain polysaccharides that have excellent whitening and firming effects. Emulsions are a commonly used formulation in skincare products, but ordinary emulsions are generally oil-in-water or water-in-oil emulsions. Water-in-oil emulsions cannot stabilize water-soluble antioxidants, while oil-in-water emulsions have a poor skin feel and cannot stabilize oil-soluble antioxidants. Therefore, a water-in-oil-in-water emulsion system is needed to simultaneously stabilize both components. However, traditional water-in-oil-in-water emulsions require the addition of large amounts of surfactants to achieve stability, but surfactants pose potential safety risks and environmental hazards. Summary of the Invention

[0003] The purpose of this invention is to solve the problem that current water-in-oil-in-water emulsions of edible fungi all contain surfactants, which pose safety hazards to the human body. The invention provides a composite edible fungi granule emulsion water-in-oil-in-water emulsion and its preparation method.

[0004] This invention utilizes ultrafine powders of black fungus and matsutake mushrooms to develop a compound edible fungus granule emulsion in water-in-oil emulsion through appropriate formulation and process. The raw materials of this emulsion are entirely composed of substances from the edible fungi themselves, making it pure, natural, non-toxic, and harmless. This avoids the safety hazards of adding other chemical substances, and the emulsion is green and natural.

[0005] The present invention discloses a compound edible fungus granule emulsion in water-in-oil-in-water, wherein the emulsion comprises, by mass fraction, 30-80 parts of purified water, 5-20 parts of olive oil, 5-20 parts of pine nut oil, 1-10 parts of black fungus ultrafine powder, 1-10 parts of matsutake ultrafine powder, 1-5 parts of black fungus polysaccharide, 1-5 parts of matsutake polysaccharide, 0.1-1 part of black fungus melanin, 0.1-1 part of ascorbate glucoside, and 0.1-1 part of vitamin E.

[0006] Furthermore, the emulsion is composed of 40-60 parts purified water, 10-20 parts olive oil, 10-20 parts pine nut oil, 5-10 parts black fungus ultrafine powder, 5-10 parts matsutake ultrafine powder, 3-5 parts black fungus polysaccharide, 3-5 parts matsutake polysaccharide, 0.5-1 part black fungus melanin, 0.5-1 part ascorbate glucoside, and 0.5-1 part vitamin E by mass fraction.

[0007] Furthermore, the emulsion is composed of 50 parts purified water, 15 parts olive oil, 15 parts pine nut oil, 8 parts black fungus ultrafine powder, 8 parts matsutake ultrafine powder, 4 parts black fungus polysaccharide, 4 parts matsutake polysaccharide, 0.8 parts black fungus melanin, 0.8 parts ascorbate glucoside and 0.8 parts vitamin E by mass fraction.

[0008] Furthermore, the particle size of both the black fungus ultrafine powder and the matsutake ultrafine powder is less than 2 micrometers.

[0009] The present invention provides a method for producing a water-in-oil-in-water emulsion of compound edible fungi granules as follows:

[0010] 1) Preparation of black fungus and matsutake mushroom ultrafine powder: Fresh black fungus and matsutake mushroom were collected, freeze-dried to constant weight, and freeze-pulverized to less than 2 micrometers to obtain black fungus ultrafine powder and matsutake mushroom ultrafine powder.

[0011] 2) Preparation of compound edible fungus granule emulsion oil-in-water emulsion: Mix matsutake mushroom ultrafine powder, purified water, black fungus melanin, and ascorbate glucoside to obtain mixed phase A. Add mixed phase A to olive oil, pine nut oil, and vitamin E and mix well. Then, perform ultrahomogenization at a pressure of 400-500 MPa, a temperature of 6-15 degrees Celsius, and a time of 20-30 minutes to obtain compound edible fungus granule emulsion oil-in-water emulsion.

[0012] 3) Preparation of compound edible fungus granule emulsion water-in-oil-in-water: After mixing purified water, black fungus ultrafine powder, black fungus polysaccharide, and matsutake polysaccharide, a mixed phase B is obtained. The prepared compound edible fungus granule emulsion water-in-oil is added to the mixed phase B and mixed evenly. Then, high-pressure homogenization is performed at a pressure of 100-200 MPa, a temperature of 6-15 degrees Celsius, and a time of 15-30 minutes to obtain the compound edible fungus granule emulsion water-in-oil-in-water.

[0013] Further, in step 1), fresh black fungus and matsutake mushrooms were collected and freeze-dried at -80 degrees Celsius to constant weight, and then frozen and pulverized at 15,000 r / min at -20 degrees Celsius to a fine powder of less than 2 micrometers.

[0014] Furthermore, in step 2), the homogenization pressure is 400 MPa, the homogenization temperature is 10 degrees Celsius, and the homogenization time is 20 minutes.

[0015] Furthermore, in step 3), the homogenization pressure is 150 MPa, the homogenization temperature is 10 degrees Celsius, and the homogenization time is 15 minutes.

[0016] The present invention has the following beneficial effects:

[0017] This invention utilizes ultrafine powders of black fungus and matsutake mushrooms to create an emulsified water-in-oil-in-water emulsion. The matsutake ultrafine powder acts as an emulsifier for the water-in-oil particles. Not only does the matsutake ultrafine powder emulsify the oil phase and inner aqueous phase to form a stable water-in-oil emulsion, but its antioxidant active ingredients, such as matsutake polysaccharides and matsutake alcohol, effectively synergistically enhance the antioxidant efficacy and stability of the black fungus pigments and ascorbate glucoside in the inner aqueous phase. The black fungus ultrafine powder also acts as an emulsifier for the oil-in-water particles. It not only enables the outer aqueous phase to emulsify the water-in-oil emulsion to form a stable water-in-oil-in-water emulsion, but its antioxidant components also synergistically enhance the antioxidant efficacy and stability of the vitamin E and unsaturated fatty acids in the oil phase, working together with the black fungus polysaccharides and matsutake polysaccharides in the outer aqueous phase to provide moisturizing effects.

[0018] The compound edible fungus granule emulsion water-in-oil-in-water emulsion of the present invention uses black fungus ultrafine powder and matsutake ultrafine powder, which solves the problem of safety hazards to human health caused by the addition of surfactants. Attached Figure Description

[0019] Figure 1 Photograph of the compound edible fungus granule emulsion water-in-oil-in-water emulsion of the present invention;

[0020] Figure 2 Microscopic image of the composite edible fungus granule emulsion water-in-oil-in-water emulsion of the present invention;

[0021] Figure 3 This is a schematic diagram of a water-in-oil-in-water emulsion made from compound edible fungi granules. Detailed Implementation

[0022] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the spirit of the contents disclosed in the present invention will be described in detail below. After understanding the embodiments of the present invention, any person skilled in the art can make changes and modifications based on the technology taught in the present invention without departing from the spirit and scope of the present invention.

[0023] The illustrative embodiments and descriptions of the present invention are used to explain the present invention, but are not intended to limit the present invention.

[0024] Example 1

[0025] This embodiment of a compound edible fungus granule emulsion in water-in-oil emulsion is composed of 65 parts purified water, 12 parts olive oil, 12 parts pine nut oil, 3 parts black fungus ultrafine powder, 3 parts matsutake ultrafine powder, 2 parts black fungus polysaccharide, 2 parts matsutake polysaccharide, 0.4 parts black fungus melanin, 0.4 parts ascorbate glucoside and 0.2 parts vitamin E by mass fraction.

[0026] To verify the difference in stability between the composite edible fungus granule emulsion in water-in-oil-in-water prepared in Example 1 and other types of emulsifiers, a comparative example was designed for verification.

[0027] Comparative Example 1

[0028] The difference between this comparative example and Example 1 is that "black fungus ultrafine powder and matsutake ultrafine powder" are omitted. Everything else is the same as in Example 1.

[0029] Comparative Example 2

[0030] The difference between this comparative example and Example 1 is that "black fungus ultrafine powder" is omitted. Everything else is the same as in Example 1.

[0031] Comparative Example 3

[0032] The difference between this comparative example and Example 1 is that "matsutake mushroom ultrafine powder" is omitted. Everything else is the same as in Example 1.

[0033] Comparative Example 4

[0034] The difference between this comparative example and Example 1 is that the black fungus ultrafine powder and matsutake ultrafine powder are replaced with synthetic emulsifiers (a mixture of Tween-80 and Span-80). Otherwise, they are the same as in Example 1.

[0035] I. Emulsion stability test

[0036] The stability study of the composite edible fungi granule emulsion water-in-oil-in-water emulsion prepared in Example 1 is as follows:

[0037] The stability of the prepared emulsion was determined by centrifugation at 4000 rpm under different pH values ​​and different NaCl concentrations. The stabilization time gradients were (5 min, 10 min, 15 min, 20 min, 25 min, and greater than 30 min). Each group of samples was tested in triplicate, and the average value of the results was taken. The test results are shown in Table 2.

[0038] Table 1. Stability test of compound edible fungi granule emulsion (water-in-oil-in-water emulsion)

[0039]

[0040]

[0041]

[0042]

[0043]

[0044] The results above show that, under the same preparation process conditions, the emulsions prepared from the matsutake and wood ear ultrafine powder groups exhibited a stability time of over 30 minutes after centrifugation at 4000 rpm under different pH values ​​and NaCl concentrations, demonstrating significantly better stability than Comparative Examples 1, 2, 3, and 4. This proves that the matsutake and wood ear ultrafine powder emulsions prepared in this embodiment possess excellent stability.

[0045] II. Emulsion Functional Testing

[0046] 1. Antioxidant test

[0047] The water-in-oil-in-water emulsion of the compound edible fungi granules from Example 1 was prepared with pure water to a concentration of 5.00 × 10⁻⁶. -3 Sample solution of g / mL.

[0048] The concentration to be prepared is 2×10 -4 The following solutions were prepared: anhydrous ethanol solution of DPPH at a concentration of g / mL, anhydrous ethanol solution of salicylic acid at a concentration of 10 mmol / L, aqueous solution of FeSO4 at a concentration of 10 mmol / L, aqueous solution of H2O2 at a concentration of 8.8 mmol / L, Tris-HCl buffer solution at pH 8.2, HCl solution at a concentration of 10 mmol / L, and pyrogallol solution at a concentration of 5 mmol / L (using HCl solution at a concentration of 10 mmol / L as solvent).

[0049] (1) Inhibition rate test of DPPH· free radical

[0050] Transfer 3 mL of the sample solution to a 10 mL volumetric flask, then add 3 mL of a 2×10⁻⁶ solution. -4 Prepare a 2 × 10⁻⁶ g / mL DPPH solution. Stopper the solution, shake well, and allow to react for 30 min. Measure the absorbance A1 at 517 nm. Measure the absorbance A2 of a mixture of 3 mL of sample solution and 3 mL of ethanol. Measure the absorbance A2 of a 3 mL solution with a concentration of 2 × 10⁻⁶ g / mL DPPH solution. -4 The absorbance A3 of a g / mL DPPH solution mixed with 3 mL of pure water.

[0051] According to the formula P=[1-(A1-A2) / A3]×100%, the measured absorbance is substituted into the formula to obtain the inhibition rate of the test solution on DPPH· free radicals.

[0052] (2) Inhibition rate test of ·OH free radicals

[0053] Add 2 mL each of 10 mmol / L salicylic acid solution and 10 mmol / L FeSO4 solution to a 10 mL volumetric flask, then add 2 mL of the test solution, followed by 2 mL of 8.8 mmol / L H2O2 solution. Shake well and react in a 37°C water bath for 30 min. Measure the absorbance A1 at 510 nm; measure the absorbance A2 using 2 mL of pure water instead of H2O2; and measure the absorbance A3 using 2 mL of pure water instead of the test solution.

[0054] According to the formula P=[1-(A1-A2) / A3]×100%, the measured absorbance is substituted into the formula to obtain the inhibition rate of the test solution against ·OH free radicals.

[0055] (3) For ·O 2- Free radical inhibition rate test

[0056] Take 5 mL of Tris-HCl buffer solution with pH 8.2 into a 10 mL volumetric flask, preheat in a 25 °C water bath for 20 min, then add 2 mL of the test solution and 0.5 mL of 5 mmol / L pyrogallol solution, shake well immediately, react in a 25 °C water bath for 4 min, and immediately measure the absorbance A1 at 320 nm; replace pyrogallol with 0.5 mL of 10 mmol / L HCl solution and measure the absorbance A2; replace the test solution with 2 mL of pure water and measure the absorbance A3.

[0057] According to the formula P = [1 - (A1 - A2) / A3] × 100%, the measured absorbance is substituted into the formula to calculate the ·O of the test liquid pair. 2- Free radical inhibition rate.

[0058] 2. Efficacy Test

[0059] Fifty participants with an average age of 45 were selected as test subjects; most had wrinkled and dry skin. The participants applied the product evenly to their face after cleansing, morning and evening, for a total of 90 days. Their skin condition was tested using a skin analyzer every 15 days.

[0060] result:

[0061] 3. Antioxidant test results

[0062]

[0063]

[0064] As shown in the table above, the average level of the compound edible fungus granule emulsion in water-in-oil-in-water emulsion in Example 1 is above 70% for the inhibition of the three free radicals, which can effectively remove free radicals.

[0065] 4. Trial Results

[0066] index Before use After use Oil content / % 15 8 Moisture / % 7 10 elasticity / % 36 49 Collagen fiber / % 57 70 pigment / % 32 28

[0067] Fifty test participants with an average age of 45 years used the compound edible fungus granule emulsion (water-in-oil-in-water emulsion) from Example 1 for 90 consecutive days. Their skin texture became noticeably lighter, and their skin problems such as dehydration and dullness improved, resulting in firmer skin.

[0068] After pore testing, the subjects' pores were significantly reduced. Observations showed that the subjects' wrinkles were significantly reduced compared to before using the compound edible fungus granule emulsion (water-in-oil-in-water emulsion) of Example 1.

[0069]

[0070] III. Stimulation Testing

[0071] The skin irritation and corrosiveness of the compound edible fungi granule emulsion water-in-oil-in-water emulsion of this embodiment were tested multiple times.

[0072] 1. Test substance

[0073] Example 1: 20g of compound edible fungi granule emulsion in water-in-oil emulsion.

[0074] 2. Detection Object

[0075] New Zealand rabbits, from Huadong Xinhua Experimental Animal Farm in Huadu District, Guangdong Province.

[0076] 3. For testing methods, please refer to Part II, 2.3.3 of the 2002 edition of the "Disinfection Technical Specifications".

[0077] Experimental steps

[0078] Before the experiment, trim or remove the hair on both sides of the animal's spine. Do not damage the epidermis. The hair removal area should be 3cm x 3cm on each side, and the application area should be 2.5cm x 2.5cm. Apply 0.5g of the test substance directly to one side of the skin, using the other side as a self-control. Apply once daily, and wash with water 4 hours after application to remove any residue. Continue application for 14 consecutive days, trimming the hair before each application.

[0079] 1. Result Evaluation:

[0080] Observe the results 24 hours after each application and evaluate the skin reaction according to the skin irritation response rating scale. Calculate the average score per animal per day using the following formula, and determine the skin irritation intensity according to the skin irritation intensity grading standard.

[0081]

[0082] 2. Experimental Results

[0083] Table 1

[0084]

[0085]

[0086] The results above show that the compound edible fungus granule emulsion in water-in-oil-in-water prepared in Example 1 was non-irritating to New Zealand rabbits in multiple stimulation experiments.

Claims

1. A composite edible fungus granule emulsion, characterized in that... The emulsion is composed of 40-60 parts purified water, 10-20 parts olive oil, 10-20 parts pine nut oil, 5-10 parts black fungus ultrafine powder, 5-10 parts matsutake ultrafine powder, 3-5 parts black fungus polysaccharide, 3-5 parts matsutake polysaccharide, 0.5-1 part black fungus melanin, 0.5-1 part ascorbate glucoside, and 0.5-1 part vitamin E by mass fraction. The preparation method of the compound edible fungus granule emulsion water-in-oil-in-water emulsion is as follows: 1) Preparation of black fungus and matsutake mushroom ultrafine powder: Fresh black fungus and matsutake mushrooms were collected, freeze-dried to constant weight, and freeze-pulverized to less than 2 micrometers to obtain black fungus ultrafine powder and matsutake mushroom ultrafine powder. 2) Preparation of compound edible fungus granule emulsion oil-in-water emulsion: Mix matsutake ultrafine powder, purified water, black fungus melanin, and ascorbate glucoside to obtain mixed phase A. Add mixed phase A to olive oil, pine nut oil, and vitamin E and mix well. Then, perform ultrahomogenization at a pressure of 400-500 MPa, a temperature of 6-15 degrees Celsius, and a time of 20-30 minutes to obtain compound edible fungus granule emulsion oil-in-water emulsion. 3) Preparation of compound edible fungus granule emulsion water-in-oil-in-water: After mixing purified water, black fungus ultrafine powder, black fungus polysaccharide, and matsutake polysaccharide, a mixed phase B is obtained. The prepared compound edible fungus granule emulsion water-in-oil is added to the mixed phase B and mixed evenly. Then, high-pressure homogenization is performed at a pressure of 100~200MPa, a temperature of 6~15 degrees Celsius, and a time of 15~30 minutes to obtain the compound edible fungus granule emulsion water-in-oil-in-water.

2. The composite edible fungus granule emulsion water-in-oil-in-water emulsion according to claim 1, characterized in that... The emulsion is composed of 50 parts purified water, 15 parts olive oil, 15 parts pine nut oil, 8 parts black fungus ultrafine powder, 8 parts matsutake ultrafine powder, 4 parts black fungus polysaccharide, 4 parts matsutake polysaccharide, 0.8 parts black fungus melanin, 0.8 parts ascorbate glucoside and 0.8 parts vitamin E by mass fraction.

3. A composite edible fungus granule emulsion in water-in-oil-in-water according to claim 1 or 2, characterized in that... The particle size of the black fungus ultrafine powder and matsutake ultrafine powder is less than 2 micrometers.

4. The composite edible fungus granule emulsion water-in-oil-in-water emulsion according to claim 1, characterized in that... In step 1), fresh black fungus and matsutake mushrooms were collected and freeze-dried at -80 degrees Celsius to constant weight, and then frozen and pulverized at 15,000 r / min at -20 degrees Celsius to a fine powder of less than 2 micrometers.

5. The composite edible fungus granule emulsion water-in-oil-in-water emulsion according to claim 1, characterized in that... In step 2), the homogenization pressure is 400 MPa, the homogenization temperature is 10 degrees Celsius, and the homogenization time is 20 minutes.

6. The composite edible fungus granule emulsion water-in-oil-in-water emulsion according to claim 1, characterized in that... Step 3) Homogenization pressure is 150 MPa, homogenization temperature is 10 degrees Celsius, and homogenization time is 15 minutes.

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