Chrysanthemum morifolium extracting solution as well as preparation method and application thereof

Abstract

The embodiment of the invention discloses a yellow chrysanthemum flower extracting solution as well as a preparation method and application thereof. The method comprises the following steps: drying yellow chrysanthemum to constant weight, crushing and sieving to obtain yellow chrysanthemum dry powder; mixing the yellow chrysanthemum flower dry powder with water, adding cellulase, and performing enzymolysis reaction under the condition of a shaking table to obtain an enzymolysis product; and carrying out enzyme deactivation treatment on the enzymolysis product, and then centrifuging to obtain the yellow chrysanthemum flower extracting solution. An enzymolysis process is researched, and the obtained yellow chrysanthemum flower extracting solution has excellent oxidation resistance. The yellow chrysanthemum flower extract is used as an active component, under the combined action of the humectant, the emulsifier, the pH regulator and the like, the sensory indexes and physicochemical properties of the prepared skin care emulsion meet the national standard of skin care emulsion, and the skin care emulsion has good oxidation resistance and can be used for skin care.

Description

Technical Field

[0001] The embodiments of the present invention relate to the field of biological extraction technology, and specifically to a chrysanthemum extract and a preparation method and application thereof. Background Art

[0002] Yellow chrysanthemum (Chrysanthemum morifolium) is a perennial herb belonging to the genus Chrysanthemum of the Asteraceae family. It is native to China and is widely cultivated for ornamental purposes, especially in autumn in China, when yellow chrysanthemums bloom, symbolizing good luck and longevity. In addition to its ornamental value, yellow chrysanthemum also has medicinal value. Traditional Chinese medicine believes that it is sweet, slightly bitter, and cool in nature, and has the effects of clearing away heat and detoxifying, calming the liver and improving eyesight, and evacuating wind-heat. It is often used to treat symptoms such as wind-heat colds, headaches, and red eyes. In addition, yellow chrysanthemum is also the main raw material for chrysanthemum tea, which has the effects of clearing heat and relieving summer heat, and relieving throat pain and moisturizing the throat, and is deeply loved by people. When drinking, it can be brewed alone or paired with other herbal teas such as wolfberry and rose to enhance the taste and health care effects.

[0003] The chemical components of chrysanthemum mainly include flavonoids, terpenes and saponins, essential oils, polysaccharides and other compounds. These natural active ingredients not only have good anti-inflammatory and antibacterial effects, but are also good antioxidants. Among them, flavonoids are the most important free radical scavengers, playing an antioxidant and anti-aging role. At present, there are endless beauty and skin care products on the market. In order to meet the needs of people with different skin types, it has become a major trend to develop safe and effective cosmetics. Summary of the invention

[0004] To this end, the embodiment of the present invention provides a chrysanthemum extract and a preparation method and application thereof.

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

[0006] According to a first aspect of an embodiment of the present invention, the present invention provides a method for preparing a chrysanthemum extract, the method comprising the following steps:

[0007] (1) drying the yellow chrysanthemum to constant weight, crushing and sieving to obtain yellow chrysanthemum dry powder;

[0008] (2) mixing the chrysanthemum dry powder with water, adding cellulase, and performing enzymolysis reaction under shaking conditions to obtain an enzymolysis product;

[0009] (3) The enzymatic hydrolysis product is subjected to enzyme inactivation treatment and then centrifuged to obtain the chrysanthemum annuum extract.

[0010] Furthermore, in step (1), the drying temperature is 60° C. and the sieved particle size is 60 mesh.

[0011] Furthermore, in step (2), the mass volume ratio of the chrysanthemum dry powder to water is 1:10 g / mL;

[0012] The amount of cellulase added is 0.4-0.8% of the mass of the chrysanthemum dry powder;

[0013] The rotation speed of the shaking table is 80r / min;

[0014] The temperature of the enzymatic hydrolysis reaction is 40-60° C., the time is 0.5-2.5 h, and the pH is 5.0.

[0015] Furthermore, the added amount of the cellulase is 0.6% of the mass of the chrysanthemum dry powder, the temperature of the enzymatic hydrolysis reaction is 50° C., the time is 1.0 h, and the pH is 5.0.

[0016] Furthermore, in step (3), the temperature of the enzyme inactivation treatment is 90-100°C and the time is 10-15 minutes.

[0017] According to a second aspect of the embodiments of the present invention, the present invention provides a chrysanthemum extract, which is prepared by the method described in any one of the above items.

[0018] According to a third aspect of the embodiments of the present invention, the present invention provides use of the above-mentioned chrysanthemum extract in skin care products, wherein the chrysanthemum extract is dried to obtain a chrysanthemum extract.

[0019] According to a fourth aspect of an embodiment of the present invention, the present invention provides a skin care product, which is a skin care lotion, comprising, by weight percentage, 20%-35% of the above-mentioned chrysanthemum extract, 0.5%-3% of butylene glycol, 10%-30% of glycerol, 1%-5% of isononyl isononanoate, 1%-4% of polydimethylsiloxane, 1%-3% of distarch phosphate, 1%-3% of panthenol, and 0.3% of p-hydroxyacetophenone. -0.5%, 1,2-hexanediol 4%-5%, methyl glucose sesquistearate 0.3%-1%, polysorbate 602%-3%, PEG-20 methyl glucose sesquistearate 0.3%-1%, phytosteryl oleate 1%-3%, carbomer 0.1%-3.0%, betaine 0.5%-5%, urea capsule 0.5%-2%, aminomethyl propanol 0.3%-0.5%, and the balance is deionized water.

[0020] The functions of the raw materials in the skin care product of the present invention are as follows:

[0021] Butylene glycol: moisturizing, antibacterial, anti-wrinkle.

[0022] Glycerin: Moisturizing.

[0023] Isononyl Isononanoate: Stabilizer and coupling agent for silicone oils, esterifying, moisturizing, softening, barrier enhancing, antioxidant, soothing and anti-inflammatory.

[0024] Polydimethylsiloxane: moisturizing and lubricating.

[0025] Distarch phosphate: adsorbent, anti-caking agent, adhesive, emulsifier.

[0026] Panthenol: moisturizing and anti-aging.

[0027] Para-Hydroxyacetophenone: Preservative.

[0028] 1,2-Hexanediol: humectant, penetrant.

[0029] Methyl Glucose Sesquistearate: emulsification, dispersion, solubilization.

[0030] Polysorbate-60: Increases product penetration and consistency, moisturizing.

[0031] PEG-20 Methyl Glucose Sesquistearate: emulsification, dispersion, solubilization.

[0032] Phytosteryl Oleate: Moisturizer, antioxidant, sunscreen and anti-skin aging.

[0033] Carbomer: hydrating, moisturizing, anti-oxidant, anti-inflammatory and bactericidal.

[0034] Betaine: Wetting agent, thickening agent.

[0035] Urea capsule: moisturizer, antibacterial.

[0036] Aminomethyl propanol: pH regulator, buffer.

[0037] According to a fourth aspect of an embodiment of the present invention, the present invention provides a method for preparing the skin care product as described above, the method comprising:

[0038] (1) Add chrysanthemum extract, butylene glycol, glycerol, distarch phosphate, panthenol, 1,2-hexanediol, methyl glucose sesquistearate, polysorbate-60, PEG-20 methyl glucose sesquistearate, carbomer, betaine, aminomethyl propanol, and deionized water into a water phase pot in sequence, heat to 70-80° C. under stirring, and keep warm for 20-30 minutes;

[0039] (2) Add isononyl isononanoate, polydimethylsiloxane, p-hydroxyacetophenone, phytosteryl oleate, and urea capsules into the oil phase pot in sequence, raise the temperature to 70-80° C. under stirring conditions, and keep the temperature for 20-30 minutes;

[0040] (3) Add the materials in the water phase pot into the oil phase pot, homogenize for 45-60 minutes at 55-60°C and 8000-12000 rpm to form a fine emulsion, and then cool to room temperature before discharging.

[0041] The embodiments of the present invention have the following advantages:

[0042] The present invention has conducted extensive research on the enzymatic hydrolysis process of chrysanthemum. Under the conditions of 0.6% cellulase addition, pH value of the reaction system = 5.0, and enzymatic hydrolysis at 50°C for 1h, the obtained chrysanthemum extract has excellent antioxidant properties, and its DPPH scavenging rate reaches (102.92±3.23)%.

[0043] The present invention uses the chrysanthemum extract as the active ingredient. Under the joint action of a moisturizer, an emulsifier and a pH adjuster, the prepared skin care lotion has sensory indicators and physical and chemical properties that meet national standards for skin care lotions, has good antioxidant properties, and can be used for skin care. DETAILED DESCRIPTION

[0044] The following is a description of the implementation of the present invention by specific embodiments. People familiar with the art can easily understand other advantages and effects of the present invention from the contents disclosed in this specification. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0045] Example 1

[0046] 1 Test method

[0047] 1.1 Single factor test of cellulase hydrolysis of chrysanthemum

[0048] Chrysanthemum (provided by the cultivation base) was dried in an oven at 60°C to constant weight, crushed and passed through a 60-mesh sieve to obtain chrysanthemum dry powder (its moisture content was 4.8%). 1.0 g of chrysanthemum powder was accurately weighed, fixed to volume according to a solid-liquid ratio of 1:10 g / mL, cellulase was added, and the reaction was carried out under shaking conditions (80 r / min), the enzyme was inactivated in a boiling water bath for 10 min, and the supernatant was centrifuged to obtain a chrysanthemum extract (i.e., sample solution).

[0049] DPPH free radical scavenging experiment: 7.88 mg of DPPH reagent was accurately weighed and placed in a 100 mL brown volumetric flask, and anhydrous ethanol was added to fully dissolve to obtain a concentration of 2×10 -4mol / L DPPH solution, refrigerate in the dark, and set aside. Mix equal volumes of sample solution and DPPH reagent, react in the dark for 30 minutes, and measure the absorbance at a wavelength of 517nm. Replace the control solvent with anhydrous ethanol, and calculate the DPPH free radical scavenging rate according to the following formula. 0.05mg / mL VC solution is the positive control.

[0050]

[0051] Where: A 样品 A is the absorbance value of the sample solution and DPPH solution measured at a wavelength of 517 nm; 对照 A is the absorbance value of the mixture of sample solution and anhydrous ethanol; 空白 It is the absorbance value of the mixture of DPPH solution and anhydrous ethanol.

[0052] Under the above process conditions, the effect of different temperatures on the DPPH clearance rate of chrysanthemum extract was studied. The pH of the enzymatic reaction system was fixed at 5.0, the amount of cellulase added (based on the mass of chrysanthemum dry powder, the same below) was 0.6%, the enzymatic hydrolysis time was 1.5h, and the enzymatic hydrolysis reaction temperatures were set to 40, 45, 50, 55, and 60°C for single-factor experiments. The test results of DPPH clearance rate are shown in Table 1 below.

[0053] Table 1

[0054] Temperature / ℃ DPPH removal rate / % 40 92.700±0.01 45 95.350±0.013 50 97.370±0.001 55 96.880±0.014 60 96.200±0.023

[0055] The effect of different enzymatic hydrolysis times on the DPPH clearance rate of chrysanthemum extract was studied. The pH of the enzymatic hydrolysis reaction system was fixed at 5.0, the amount of cellulase added was 0.6%, the enzymatic hydrolysis temperature was 50°C, and the enzymatic hydrolysis time was set to 0.5, 1.0, 1.5, 2.0, and 2.5 h for a single factor experiment. The test results of DPPH clearance rate are shown in Table 2 below.

[0056] Table 2

[0057] Time / h DPPH removal rate / % 0.5 96.02±0.004 1 99.06±0.007 1.5 97.31±0.002 2.0 95.36±0.014 2.5 91.58±0.001

[0058] The effects of different pH values ​​of the enzymatic hydrolysis reaction system on the DPPH clearance rate of the anther extract were studied. The enzymatic hydrolysis temperature was fixed at 50°C, the amount of cellulase added was 0.6%, the enzymatic hydrolysis time was 1.5h, and the pH of the enzymatic hydrolysis reaction system was set at 4.0, 4.5, 5.0, 5.5, and 6.0 for a single factor experiment. The test results of the DPPH clearance rate are shown in Table 3 below.

[0059] Table 3

[0060] pH DPPH clearance 4.0 93.01±0.009 4.5 95.53±0.007 5.0 97.37±0.003 5.5 89.9±0.03 6.0 89.04±0.035

[0061] The effects of different enzyme addition amounts on the DPPH clearance rate of chrysanthemum extract were studied. The pH of the enzymatic reaction system was fixed at 5.0, the enzymatic hydrolysis temperature was 50°C, the enzymatic hydrolysis time was 1.5h, and the addition amounts of cellulase were set at 0.2%, 0.4%, 0.6%, 0.8%, and 1.0% for a single factor experiment. The test results of DPPH clearance rate are shown in Table 4 below.

[0062] Table 4

[0063] Cellulase addition amount DPPH clearance 0.2％ 92.38±0.018 0.4％ 95.46±0.007 0.6％ 97.37±0.002 0.8％ 96.09±0.009 1.0％ 85.55±0.058

[0064] 1.2 Response surface experiment of cellulase hydrolysis of chrysanthemum

[0065] According to the results of single factor test, the temperature, time, system pH and enzyme addition amount of enzymatic hydrolysis reaction were combined for optimization, and the DPPH clearance rate of chrysanthemum extract was used as the response value to carry out response surface test design. The scheme is shown in Table 5.

[0066] Table 5 Factors and coding levels of Box-Behnken experimental design

[0067]

[0068]

[0069] The model is:

[0070] Y=1.00-0.026A+0.033B-0.012C-0.086D-0.20AB+0.065AC+0.032AD+0.026BC+0.048BD-0.037CD+0.025A 2 -0.026B 2 -0.12C 2 -0.052D 2 +0.010A 2 B+0.075A 2 C+0.019A 2 D-0.10AB 2 -0.066AC 2 +0.023B 2 C+0.052B 2 D+0.000485BC 2 , R 2 =0.9995, P<0.0001.

[0071] The model reached an extremely significant level, and the P value of the lack of fit term was 0.1985>0.05, indicating that the model fit was good. The model fit was as high as 99.95%, indicating that the experimental error was small, and the model could be used to predict the effect of enzymatic hydrolysis on the DPPH removal ability of chrysanthemum extract. From the P values ​​of each factor in Table 6, it can be seen that the influence of all factors reached an extremely significant level (P<0.01), indicating that each factor had an effect on the DPPH removal ability of chrysanthemum extract.

[0072] Table 6 Analysis of variance

[0073]

[0074]

[0075] Note: “**” indicates P<0.01, and “-” indicates no significant difference.

[0076] The optimal solution predicted by the model was 0.6% cellulase addition, pH of the reaction system = 5.0, and enzymatic hydrolysis at 50℃ for 1h. The predicted DPPH clearance rate of the chrysanthemum extract was (99.63±0.63)%. The DPPH clearance rate under this condition was verified to be (102.92±3.23)%, which was not significantly different from the predicted value (P>0.05). Therefore, the model can be used to predict the enzymatic hydrolysis process of chrysanthemum.

[0077] Under the above optimal scheme, the obtained chrysanthemum extract is dried to obtain a chrysanthemum extract, which is used to prepare the skin care product of Example 2.

[0078] Example 2

[0079] The present embodiment provides a skin care lotion, and its raw materials are, by weight percentage: 30% of anthemis nobilis extract, 1.2% of butylene glycol, 18% of glycerol, 5% of isononyl isononanoate, 2.2% of polydimethylsiloxane, 1.2% of distarch phosphate, 2.5% of panthenol, 0.3% of p-hydroxyacetophenone, 4% of 1,2-hexanediol, 0.8% of methyl glucose sesquistearate, 2.2% of polysorbate-60, 0.6% of PEG-20 methyl glucose sesquistearate, 1.8% of phytosteryl oleate, 1.5% of carbomer, 2.8% of betaine, 1.2% of urea capsule, 0.3% of aminomethyl propanol, and the balance is deionized water.

[0080] The preparation method thereof comprises the following steps:

[0081] (1) Chrysanthemum extract, butylene glycol, glycerol, distarch phosphate, panthenol, 1,2-hexanediol, methyl glucose sesquistearate, polysorbate-60, PEG-20 methyl glucose sesquistearate, carbomer, betaine, aminomethyl propanol, and deionized water were sequentially added into a water phase pot, heated to 80° C. under stirring, and kept warm for 25 min;

[0082] (2) Add isononyl isononanoate, polydimethylsiloxane, p-hydroxyacetophenone, phytosteryl oleate, and urea capsules into the oil phase pot in sequence, raise the temperature to 80° C. under stirring conditions, and keep the temperature for 20 minutes;

[0083] (3) Add the materials in the water phase pot to the oil phase pot and homogenize at 55°C and 12,000 rpm for 45 min to form a fine emulsion. Cool to room temperature and then discharge.

[0084] Test Example 1

[0085] 1. Sensory, physical, chemical and hygiene index tests

[0086] The test results of the skin care lotion of Example 2 are shown in Table 7 below.

[0087] Table 7

[0088]

[0089]

[0090] The results show that the skin care lotion provided by the embodiment of the present invention meets the requirements of the national standard QB / T 29665-2013.

[0091] 2. Antioxidant performance test

[0092] The skin care lotion of Example 2 was diluted with distilled water at a mass ratio of 1:5 to obtain a sample to be tested. After testing, the total antioxidant capacity of the sample to be tested was 62.92%. The results showed that the emulsion provided by the embodiment of the present invention has good antioxidant properties and can be used for skin care.

[0093] Although the present invention has been described in detail above by general description and specific embodiments, it is obvious to those skilled in the art that some modifications or improvements can be made to the present invention. Therefore, these modifications or improvements made without departing from the spirit of the present invention all belong to the scope of protection claimed by the present invention.

Claims

1. A method for preparing a chrysanthemum extract, characterized in that: The method comprises the following steps: (1) drying the yellow chrysanthemum to constant weight, crushing and sieving to obtain yellow chrysanthemum dry powder; (2) mixing the chrysanthemum dry powder with water, adding cellulase, and performing enzymolysis reaction under shaking conditions to obtain an enzymolysis product; (3) The enzymatic hydrolysis product is subjected to enzyme inactivation treatment and then centrifuged to obtain the chrysanthemum annuum extract.

2. The method for preparing the chrysanthemum extract according to claim 1, characterized in that: In step (1), The drying temperature is 60° C. and the sieved particle size is 60 mesh.

3. The method for preparing the chrysanthemum extract according to claim 1, characterized in that: In step (2), The mass volume ratio of the chrysanthemum dry powder to water is 1:10 g / mL; The amount of cellulase added is 0.4-0.8% of the mass of the chrysanthemum dry powder; The rotation speed of the shaking table is 80r / min; The temperature of the enzymatic hydrolysis reaction is 40-60° C., the time is 0.5-2.5 h, and the pH is 4.0-6.

0.

4. The method for preparing the chrysanthemum extract according to claim 3, characterized in that: The added amount of the cellulase is 0.6% of the mass of the chrysanthemum dry powder, the temperature of the enzymatic hydrolysis reaction is 50° C., the time is 1.0 h, and the pH is 5.

0.

5. The method for preparing the chrysanthemum extract according to claim 1, characterized in that: In step (3), The temperature of the enzyme inactivation treatment is 90-100°C and the time is 10-15 minutes.

6. A chrysanthemum extract, characterized in that: It is made by the method according to any one of claims 1-5.

7. The use of the chrysanthemum extract according to claim 6 in skin care products, characterized in that: The chrysanthemum extract is dried to obtain the chrysanthemum extract.

8. A skin care product, characterized in that: The skin care product is a skin care lotion, which comprises, by weight percentage, 20%-35% of the anthemis nobilis extract described in claim 7, 0.5%-3% of butylene glycol, 10%-30% of glycerol, 1%-5% of isononyl isononanoate, 1%-4% of polydimethylsiloxane, 1%-3% of distarch phosphate, 1%-3% of panthenol, 0.3%-0.5% of p-hydroxyacetophenone, 4%-5% of 1,2-hexanediol, 0.3%-1% of methyl glucose sesquistearate, 2%-3% of polysorbate-60, 0.3%-1% of PEG-20 methyl glucose sesquistearate, 1%-3% of phytosteryl oleate, 0.1%-3.0% of carbomer, 0.5%-5% of betaine, 0.5%-2% of urea capsule, 0.3%-0.5% of aminomethyl propanol, and the balance is deionized water.

9. The method for preparing the skin care product according to claim 8, characterized in that: The method comprises: (1) Add chrysanthemum extract, butylene glycol, glycerol, distarch phosphate, panthenol, 1,2-hexanediol, methyl glucose sesquistearate, polysorbate-60, PEG-20 methyl glucose sesquistearate, carbomer, betaine, aminomethyl propanol, and deionized water into a water phase pot in sequence, heat to 70-80° C. under stirring, and keep warm for 20-30 minutes; (2) Add isononyl isononanoate, polydimethylsiloxane, p-hydroxyacetophenone, phytosteryl oleate, and urea capsules into the oil phase pot in sequence, raise the temperature to 70-80° C. under stirring conditions, and keep the temperature for 20-30 minutes; (3) Add the materials in the water phase pot to the oil phase pot, homogenize at 55-60°C and 8000-12000 rpm for 45-60 min to form a fine emulsion, and then cool to room temperature before discharging.

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