Preparation process of lucid ganoderma compound shampoo

Abstract

The invention discloses a preparation process and quality evaluation of ganoderma lucidum compound shampoo, which is characterized in that ganoderma lucidum, polygonum multiflorum, saponin, angelica sinensis, cacumen biotae and black sesame are used as raw materials, stability, foamability, flexibility and viscosity are used as evaluation standards, and the formula of the ganoderma lucidum compound shampoo is optimized through experiments. The optimization result is as follows: 20 mL of plant extract, 20 g of detergent sodium alcohol ether sulphate and fatty alcohol polyoxyethylene ether ammonium sulfate, 2.2 g of hydrolyzed silk protein, 6.0 g of sodium chloride, 0.005 g of citric acid, 0.3 g of phenoxyethanol, 0.005 g of piroctone olamine salt, and the balance of pure water to 100 mL. After the lucid ganoderma compound shampoo is used for 15 days, the oil control rate is 56.27 + / -0.97%; when the concentration of the raw medicinal materials is 5.0 mg / mL, the ABTS free radical scavenging rate of the shampoo is 68.37 + / -1.03%, and the prepared shampoo can improve the scalp environment, has the effects of controlling oil and resisting oxidation, and is safe and non-irritant.

Description

Technical Field

[0001] The invention relates to the technical field of natural cosmetics, and in particular to the preparation and quality evaluation of a natural plant ganoderma lucidum compound shampoo. Background Art

[0002] Chemical shampoo products are usually made using modern chemical synthesis technology and have multiple functions and advantages. The main ingredients are mostly silicone oil and surfactant compound systems. [1] . It can provide a certain degree of cleaning effect in the initial stage, but excessive or poor quality silicone oil is easy to accumulate on the hair. Long-term use of shampoo containing excessive silicone oil will make the hair feel more greasy. In addition, the deposition of silicone oil may irritate the scalp, causing itching and dandruff. When silicone oil accumulates to a certain extent, it may clog the pores, affect the normal growth of hair, and cause irreversible damage to the scalp and hair. [2] . Sodium lauryl sulfate is a powerful cleanser that can clean the scalp and hair, but it can deprive the hair of its natural oils, causing it to become dry and break easily. Long-term use can also damage the hair and cause hair loss. It also often contains irritating ingredients such as sulfates and alcohol. Long-term use can cause damage to the scalp and hair, such as dry scalp and dry hair. Parabens are often used as preservatives. Long-term use can also cause dry scalp, increased dandruff, and even hair loss in severe cases. Therefore, in order to protect the health of your hair, choose a shampoo that contains natural, mild, non-irritating ingredients.

[0003] Chinese herbal shampoo products are made from natural Chinese herbal ingredients and are safe, healthy and mild. [3] Chinese herbal shampoo products can nourish the scalp, relieve itching and dandruff, prevent hair loss and promote hair growth, soften hair, are gentle and non-irritating, and protect the health and beauty of the scalp and hair.

[0004] Lingzhi can promote blood circulation in the scalp, increase the nutrient supply to the scalp, and help the growth and health of hair. At the same time, Lingzhi can also inhibit the growth of dandruff, reduce the production of dandruff, and keep the scalp clean and healthy. [4] Polygonum multiflorum can nourish hair, making it healthier and more lustrous. It can also improve hair quality and alleviate problems such as rough hair and gray hair. [5] Gleditsia sinensis can supplement the hair with natural nutrients, remove dandruff, prevent hair loss, and promote hair regeneration. In addition, the extract of gleditsia sinensis also has good cleaning and bactericidal effects, which can inhibit the formation of dandruff. [6] Angelica can protect hair and prevent hair loss. [7] Platycladus orientalis leaves can effectively improve scalp blood circulation and strengthen the metabolic function of hair follicles. Its total flavonoids can divide, proliferate and differentiate, increase the growth rate of hair, restore the vitality of hair follicles and further promote blood circulation.[7] , especially suitable for treating permanent hair loss and premature graying of hair caused by blood heat. Black sesame helps maintain hair and prevent hair loss and graying. [8] .

[0005] According to the characteristics of Chinese herbal medicine, the present invention screens the raw material ratio through anti-oxidation, and then optimizes the ratio with auxiliary materials. The prepared Chinese herbal shampoo reduces the stimulation to the scalp and hair, can deeply nourish the hair and scalp, and is suitable for various skin types, especially sensitive scalp.

[0006] [1] Xiao Jinxin. Overview of the development of shampoo surfactant technology (continued) [J]. Daily Chemicals Science, 2019, 42(03): 14-19.

[0007] [2] Li Qiang, Wan Yuepeng, Gong Shengzhao, et al. Application of disodium cocoyl glutamate in silicone-free shampoo[J]. Guangdong Chemical Industry, 2018, 45(20): 41-43.

[0008] [3] Wang Wei, Ya Hongbo, Xin Xing, et al. Research on the development and anti-dandruff efficacy of Chinese herbal shampoo [J]. Science and Technology, 2016, (14): 175.

[0009] [4] Xiao Zhiyuan. Herbal hair care solution: CN201710222241.

[0010] [5] Zhao Longwei. A Chinese medicine composition with hair-fixing effect and its application: CN202210011869.0

[0011] [6] Pi Yongbo. Exploring the formula optimization and performance improvement effect of green shampoo with natural saponin extract[J]. Contemporary Chemical Research, 2022, (19): 84-86.

[0012] [7] Wang Qingfeng. A herbal hair care essential oil and its preparation process. CN201910350111.8

[0013] [8] Liao Jiaping. Chinese herbal medicine composition for hair growth: CN201810899190.3

[0014] [9] Liu Xue. Screening of Chinese herbal compound for hair growth and hair darkening and its pharmacodynamics study[D]. China Pharmaceutical Industry Research Institute, 2020. Summary of the invention

[0015] The raw materials and auxiliary materials of shampoos on the market contain harmful chemical ingredients, such as sodium lauryl sulfate, sodium benzoate, methylisothiazolinone, silicone oil, etc., which will cause unhealthy scalp and hair if used for a long time and in large quantities. Plant shampoo retains natural nutrients and active substances, is mild and non-irritating to the scalp and hair, is suitable for all skin types, and reduces the side effects that may be caused by chemical additives. The plants used in the present invention are carefully selected and scientifically proportioned, and have antioxidant functions while controlling oil, and are safe and non-irritating, and nourish the hair.

[0016] To achieve the above purpose, the present invention adopts the following experimental scheme:

[0017] The invention provides a ganoderma lucidum compound shampoo, comprising plant extract, auxiliary materials such as sodium fatty alcohol polyoxyethylene ether sulfate (AES), ammonium fatty alcohol polyoxyethylene ether sulfate (AESA), hydrolyzed silk protein, sodium chloride, citric acid, phenoxyethanol and piroctone olamine.

[0018] Preferably, the preparation of the plant extract: take dried Ganoderma lucidum, Polygonum multiflorum, Gleditsia sinensis, Angelica sinensis, Platycladus orientalis leaves, and black sesame, crush them, accurately weigh them according to the mass ratio of 3:2.0:1.8:1.9:0.8:0.6, the solid-liquid ratio is 1:20 (g / mL), soak for 0.5h, the temperature is 90°C, heat reflux extraction for 3h, filter with 3 layers of gauze, put the filtrate into a centrifuge and centrifuge at a speed of 4800r / min for 10min, the supernatant is the plant extract, and the concentration of the raw medicinal materials is 50mg / mL.

[0019] Preferably, the Ganoderma lucidum compound shampoo uses sodium alcohol polyoxyethylene ether sulfate (AES) and ammonium alcohol polyoxyethylene ether sulfate (AESA) for the purpose of removing dirt and oil, hydrolyzed silk protein for conditioning hair to make it smooth and not dry, sodium chloride for adjusting the viscosity to achieve the optimal viscosity, the citric acid is used to adjust the pH of the system, phenoxyethanol is a preservative, and piroctone olamine salt is an anti-dandruff agent.

[0020] Preferably, based on 100 mL, 20 mL of plant extract, 20 g of AES:AESA (7:3), 2.2 g of hydrolyzed silk protein, 6 g of sodium chloride, 0.005 g of citric acid, 0.3 g of phenoxyethanol, 0.005 g of piroctone olamine salt are used, and pure water is added to make up to 100 mL.

[0021] According to a second aspect of the present invention, the present invention provides a method for preparing a Ganoderma lucidum compound shampoo, comprising the following steps:

[0022] Add AES, AESA and hydrolyzed silk protein into pure water at 80-85°C, then add citric acid, phenoxyethanol and piroctone olamine salt. After all are dissolved, cool to 30-40°C, add plant extract, and then add sodium chloride in batches to adjust the viscosity to obtain Ganoderma lucidum compound shampoo.

[0023] In the oil control experiment described in the present invention, the oil control rate of the Ganoderma lucidum compound shampoo group is 56.27±0.97%; in the antioxidant experiment, when the raw medicinal material concentration of the Ganoderma lucidum compound shampoo is 5.0 mg / mL, the ABTS free radical scavenging rate is 68.37±1.03%, which can improve the scalp environment and achieve the effects of oil control and antioxidant.

[0024] The shampoo of the present invention is a light yellow viscous liquid with a pH value of 6.3±0.02, which is consistent with the value of human skin. Viscosity: 9900±200 mPa·s, with good stability and safety.

[0025] Compared with the prior art, the present invention has the following beneficial effects:

[0026] (1) The present invention uses Ganoderma lucidum as the main ingredient, and mixes Polygonum multiflorum, Gleditsia sinensis, Chinese angelica, Platycladus orientalis leaves, and black sesame to prepare a plant extract in a specific ratio, which can effectively cleanse hair.

[0027] (2) The traditional hot water soaking method can retain the effective ingredients to the maximum extent, with the polysaccharide content reaching 28.9±0.67% and the flavonoid content reaching 3.91±0.31%. The ABTS clearance rate of the extract when the raw medicinal material concentration was 5 mg / mL was 69.56±0.23%.

[0028] (3) The shampoo of the present invention has the effects of oil control and anti-oxidation. The oil control rate of the shampoo group is 7.64% higher than that of the positive control group, and the anti-oxidation rate is 17.14% higher than that of the control group, which effectively protects the hair.

[0029] (4) The shampoo of the present invention adopts a multi-index evaluation method. The raw materials and auxiliary materials are dissolved by cooling for multiple times, and the viscosity regulator is added in batches. The product has rich and lasting foam and good cleaning effect. It can also moisturize the hair, and the viscosity is moderate, which is easy to apply and rinse, and will not cause waste or inconvenience. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] Figure 1 ABTS free radical scavenging rate curve of Ganoderma lucidum, Polygonum multiflorum, Gleditsia sinensis, Chinese angelica, Platycladus orientalis, and black sesame

[0031] Figure 2 Ganoderma lucidum compound plant extract (5 mg / mL) and negative control group (3.5 mg / mL)

[0032] Antioxidant comparison chart

[0033] Figure 3 Interaction curve and contour plot of plant extract addition amount and AES:AESA

[0034] Figure 4 Curve and contour map of the interaction between the amount of plant extract added and hydrolyzed silk protein Figure 5 Statistical difference of oil control rate and antioxidant effect of Ganoderma lucidum compound shampoo (raw material concentration 5mg / mL) DETAILED DESCRIPTION

[0036] Example 1 Determination of active ingredient content

[0037] 1. Polysaccharide content determination method

[0038] Preparation of glucose standard curve: Prepare 1 mg / mL glucose standard solution, dilute the standard solution with concentrations of 0.015 mg / mL, 0.030 mg / mL, 0.045 mg / mL, 0.060 mg / mL, and 0.075 mg / mL, respectively. Add 1 mL of 5% phenol and 5 mL of 98% concentrated sulfuric acid, let stand for 30 minutes, and measure the absorbance at a wavelength of 490 nm.

[0039] Standard curve: y = 6.935x + 0.0959, R 2 =0.9992

[0040] 2. Flavonoid content determination method

[0041] Preparation of rutin standard curve: prepare 0.2mg / mL rutin standard solution, accurately measure 1.5mL, 2mL, 3mL, 4mL, and 5mL of the standard solution respectively and place them in a 25mL volumetric flask, add 30% ethanol to 6mL, add 5% sodium nitrite solution 1mL and let it stand for 6min, add 10% aluminum nitrate solution 1mL and let it stand for 6min, add 4% sodium hydroxide solution 10mL, finally make up to volume with 30% ethanol, shake well and let it stand for 15min, and measure the absorbance at a wavelength of 500nm

[0042] Standard curve y = 1.347x + 0.0517, R 2 =0.9991

[0043] Example 2 ABTS free radical scavenging experiment

[0044] Take 1.8mL ABTS solution and mix it with 0.2mL sample solution, shake it for 10s as the experimental sample solution, and let it stand in the dark for 6min. At the same time, take another 1.8mL ABTS solution and mix it with 0.2mL distilled water, shake it for 10s as the control solution, and let it stand in the dark for 6min. After that, adjust the wavelength of the UV spectrophotometer to 734nm, preheat it for 30min, and measure the absorbance. Finally, according to the measured absorbance, use a specific formula to calculate the clearance rate. The higher the clearance rate, the stronger the antioxidant activity of the sample. Formula:

[0045]

[0046] Among them, A0, A1 and A2 are the absorbance values ​​of the blank group, control group and sample group respectively.

[0047] Example 3: Plant extract ratio screening experiment

[0048] Take dried Ganoderma lucidum, Polygonum multiflorum, Gleditsia sinensis, Platycladus orientalis leaves, and black sesame, crush them, pass through a 20-mesh sieve, accurately weigh them according to the mass ratio, the solid-liquid ratio is 1:20 (g / mL), soak for 0.5h, temperature 90℃, heat reflux extraction for 3h, filter with 3 layers of gauze after extraction, put the filtrate into a centrifuge and centrifuge at 4800r / min for 10min, the supernatant is the plant extract, and the raw medicinal material concentration is 50mg / mL. Dilute 10 times, that is, the raw medicinal material concentration is 5mg / mL for ABTS free radical scavenging rate experiment. Formula:

[0049]

[0050] Among them, A1 and A2 are the amount of raw medicinal materials and pure water used respectively.

[0051] 1. Single Factor Experiment

[0052] A single factor experiment was conducted to screen the dosage of raw materials for extraction, and the clearance rate of plant extracts was used as an indicator.

[0053] The fixed factors were Ganoderma lucidum 3g, Polygonum multiflorum 2.0g, Gleditsia sinensis 2.0g, Angelica sinensis 1.5g, Platycladus orientalis leaves 1.0g, and Black sesame 0.5g. The screening range is shown in Table 1.

[0054] Table 1 Screening range of dosage of traditional Chinese medicine

[0055]

[0056]

[0057] The dosage of 4 kinds of Chinese medicines were selected, and the clearance rate was used as an indicator to examine the effect of each Chinese medicine on the clearance rate.

[0058] The results showed that when the amount of Ganoderma lucidum was 3g, the scavenging rate of the extract was the highest, which was 44.34%; when the amount of Polygonum multiflorum was 1.8g, the scavenging rate of the extract was the highest, which was 49.55%; when the amount of Gleditsia sinensis was 2.0g, the scavenging rate of the extract was the highest, which was 53.23%; when the amount of Angelica sinensis was 1.7g, the scavenging rate of the extract was the highest, which was 57.32%; when the amount of Platycladus orientalis leaves was 1.0g, the scavenging rate of the extract was the highest, which was 67.48%; when the amount of Black Sesame was 0.5g, the scavenging rate of the extract was the highest, which was 69.31%. The specific effects of ABTS free radical scavenging rate are as follows: Figure 1 .

[0059] 2. Orthogonal experiment

[0060] The amount of raw materials of Ganoderma lucidum, Polygonum multiflorum, Gleditsia sinensis, Chinese angelica, Platycladus orientalis and black sesame were screened, and three levels were selected for each amount (see Table 2) according to L3 (3 6 ) orthogonal table (see Table 3) was used to conduct experiments, and the clearance rate was used as the evaluation index to select the optimal ratio of plant extracts.

[0061] Table 2 Orthogonal factors and levels

[0062]

[0063] The results are shown in Table 2. The order of influence of the six factors on the clearance rate is Ganoderma lucidum > Platycladus orientalis leaf > Gleditsia sinensis > Black sesame > Polygonum multiflorum > Angelica sinensis. The results showed that Ganoderma lucidum had a significant effect on the results. The optimized composite extract contained 3.0g of Ganoderma lucidum, 2.0g of Polygonum multiflorum, 1.8g of Gleditsia sinensis, 1.7g of Angelica sinensis, 1.2g of Platycladus orientalis leaf and 0.6g of Black sesame.

[0064] Table 3 Orthogonal experimental results and intuitive analysis

[0065]

[0066] 3. Verification experiment

[0067] The process conditions of the verification experiment were: 3g of Ganoderma lucidum, 2.0g of Polygonum multiflorum, 1.8g of Gleditsia sinensis, 1.7g of Angelica sinensis, 1.2g of Platycladus orientalis, and 0.6g of black sesame. The experiments were repeated three times in parallel. When the concentration of the raw materials was 5mg / mL, the average scavenging rate was 69.56±0.23%, and when the concentration of VC was 7.25ug / mL, the ABTS free radical scavenging rate was 70%. This shows that the Chinese medicine liquid has a certain antioxidant capacity. Its polysaccharide content is 28.9±0.67%, and the flavonoid content is 3.91±0.31%.

[0068] 4. Negative control experiment

[0069] Ganoderma lucidum compound plant extract: the preparation method in Example 3.

[0070] Negative control group: Ganoderma lucidum, Polygonum multiflorum, Gleditsia sinensis, Chinese angelica, Platycladus orientalis leaves, and black sesame were not added, and the comparison was carried out according to the experimental method in Example 3, keeping the volumes consistent.

[0071] Experimental results: When the raw material concentration of Ganoderma lucidum compound plant extract was 5 mg / mL, the ABTS free radical scavenging rate was 69.56±1.34% (P<0.05), and when the raw material concentration was 3.5 mg / mL, the ABTS free radical scavenging rate of the negative control group was 58.51±0.64% (P<0.05). Figure 2 This indicates that Ganoderma lucidum has antioxidant capacity and works synergistically with other Chinese medicinal ingredients.

[0072] Example 4: Screening of the dosage of auxiliary materials for Ganoderma lucidum compound shampoo

[0073] 1. Single Factor Experiment

[0074] (1) Surfactant AES: AESA dosage screening

[0075] 2 g of hydrolyzed silk protein and 6 g of sodium chloride were fixed, and foaming tests were carried out when AES:AESA was 6:4, 7:3, 8:2, 9:1, and 10:0, and the evaluation index was H5 / H0.

[0076] Weigh 1g of each sample, add 50mL of deionized water preheated to 50℃ for pyrolysis, dissolve the sample to be tested, and keep the solution at 50℃. Record 5 groups of initial foam heights (H0 / cm) and heights at 5 minutes (H5 / cm). The initial foam height is the foamability. The larger the value, the better the foamability. The size of (H5 / H0) is the foam stability. The closer the ratio is to 1, the better the foam stability.

[0077] As shown in Table 4: when the ratio of AES:AESA is 7:3, the foaming property is better and the foam stability is optimal, so this ratio is selected as the optimal ratio of surfactant AES:AESA.

[0078] Table 4 Shampoo foam performance test results

[0079]

[0080] (2) Screening of the amount of hydrolyzed silk protein used as a conditioning agent

[0081] AES:AESA was fixed at 7:3 (g), 6 g of sodium chloride, and when the hydrolyzed silk protein was 1.6 g, 1.8 g, 2 g, 2.2 g, and 2.4 g, the combing test was carried out. The evaluation index was the sensory score, see Table 5.

[0082] Take a 40cm long hair bundle, soak it with warm water, blow dry 3g of sample with a hair dryer, apply it evenly on the front and back of the comb and rub it thoroughly, rinse with warm water, and test.

[0083] Table 5 Evaluation criteria for combability of shampoo

[0084]

[0085]

[0086] Table 6 Shampoo combing score table

[0087]

[0088]

[0089] The sensory evaluation results of the shampoo are shown in Table 6: When the hydrolyzed silk protein is 2.2g, the sensory evaluation score of the shampoo is the highest. Apply it evenly on the front and back of the comb and rub it thoroughly. The foam is rich and dense during the rubbing process, and the foam is easy to rinse off, and its softening effect is the best. Therefore, 2.2g is selected as the optimal addition amount of hydrolyzed silk protein.

[0090] (3) Screening of viscosity agent sodium chloride dosage

[0091] AES:AESA was fixed at 7:3 (g), hydrolyzed silk protein was 2.2g, citric acid, phenoxyethanol, and piroctone olamine salt were all appropriate, and when the amount of sodium chloride added was 4g, 5g, 6g, 7g, and 8g, the viscosity was measured: the viscosity before and after the measurement. Viscosity was used as an evaluation index.

[0092] According to GB / T15357, the optimal viscosity of shampoo is 8000-10000mPa.s. The comprehensive sensory score is shown in Table 6. The results are shown in Table 7. It can be obtained that when the addition amount of sodium chloride is 6g, the viscosity of the prepared shampoo is optimal.

[0093] Table 6 Shampoo Viscosity Scoring Standard

[0094]

[0095] Table 7 Shampoo Viscosity Score Data Table

[0096]

[0097]

[0098] (4) Screening of the amount of plant extract added

[0099] AES:AESA was fixed at 7:3 (g), 2.2 g of hydrolyzed silk protein, 6 g of sodium chloride, appropriate amounts of citric acid, phenoxyethanol, and piroctone olamine salt. When the amount of plant extract added was 10 mL, 20 mL, 30 mL, 40 mL, and 50 mL, the ABTS free radical scavenging rate became higher and higher. After sealing and standing for two weeks, the stratification effect was observed.

[0100] The evaluation index adopts a comprehensive score (ABTS free radical scavenging rate × 0.5 / ABTS free radical scavenging rate + stability × 0.5 / stability) × 100. The results show that when the amount of plant extract added is 10mL and 20mL, the shampoo has good stability, and the shampoo samples prepared at 30mL, 40mL, and 50mL show stratification.

[0101] Therefore, when the amount of Chinese medicine extract water added is 20 mL, the concentration of raw medicinal materials is 5 mg / mL and its ABTS free radical scavenging rate is 68.37±1.03%, which is the optimal value of the amount of plant extract added to the shampoo formula.

[0102] 2. Response surface experiment for process optimization of Ganoderma lucidum compound shampoo

[0103] Based on the single factor experiment of surfactant AES: AESA, conditioning agent hydrolyzed silk protein, viscosity agent sodium chloride, and plant extract, the response surface experiment was designed using Design-Expert 8.0.6 software, and the design table is shown in Table 8. With H5 / H0 (foaming), softness, viscosity, and stability each with 25 points as indicators, the optimal formula ratio of Lingzhi compound shampoo was selected. The total formula evaluation score (100) = (H5 / H0×25+softness×25+viscosity×25+stability×25)

[0104] Table 8 Factor levels and coding of formulation response surface design

[0105]

[0106]

[0107] Table 9 Total score table of Lingzhi compound shampoo formula

[0108]

[0109]

[0110] Design-Expert 8.0.6 software was used to process the data by binomial equation fitting and multiple linear regression. 2 ) and confidence level (P) were used as the model judgment criteria, and variance analysis was performed on the regression parameters of the response surface. The quadratic fitting equation was:

[0111] M=91.80+2.58A+0.17B+1.92C-2.00D-1.75AB-1.25AC-1.75AD+3.00BC-0.75BD+3.00CD-7.94A2-4.32B 2 -6.69C 2 -5.82D 2 (R 2 =0.9667, P<0.05), correlation coefficient R 2 The higher the value, the better the model fits. The regression model P<0.05 indicates that the regression model is significant.

[0112] The results of the response surface experiment are shown in Figure 3-4 When the surfactant is 7:3, the foam is fine and dense with good stability; when the thickener is 6g of sodium chloride, the measured viscosity meets the requirements of shampoo, no precipitation occurs, and it has the advantage of uniform dissolution; when the conditioning ingredient is 2.2g of hydrolyzed silk protein, it plays a role in nutrition and repairing damage, making the hair shiny and elastic, and the conditioning effect is the best. The optimal formula of the process parameters of Lingzhi compound shampoo is: the amount of Chinese medicine liquid added is 20mL, the amount of AES:AESA added is 7:3 (20g), the amount of hydrolyzed silk protein added is 2.2g, the amount of sodium chloride added is 6g, citric acid is 0.005g, phenoxyethanol is 0.3g, and piroctone olamine salt is 0.005g.

[0113] Example 5: Preparation method of Ganoderma lucidum compound shampoo

[0114] Add AES, AESA and hydrolyzed silk protein into pure water at 80-85°C, stir for 10 minutes until completely dissolved, then cool down by 50°C, add phenoxyethanol and piroctone olamine salt, after all dissolved, cool down to 30-40°C, add citric acid and wait for it to dissolve, then add plant water extract, cool down several times, add sodium chloride to adjust the viscosity, stir evenly until there is no insoluble matter, and encapsulate to obtain Ganoderma lucidum compound shampoo.

[0115] Example 6: Functional evaluation

[0116] (1) Oil control performance

[0117] The test subjects were tested for scalp oil content using an oil tester, and the product was used to wash hair every two days to test the oil content, and the data were recorded, where the rate of change of oil content (%) = (oil content after using the test sample - oil content before using the test sample) / oil content before using the sample × 100. The control group was washed with an oil-control shampoo on the market (formula: sodium laureth sulfate, cocamidopropyl betaine, glycerin, sodium chloride, citric acid, PPG-5-cetoeth-20, propylene glycol, PEG-60, hydrogenated castor oil, polysorbate-20, sodium hydroxide, citric acid, PEG-55, propylene glycol oleate, glyceryl oleate, salicylic acid, polyquaternium-10, piroctone ammonium salt, etc.).

[0118] The results show that the oil control rate of the shampoo prepared by the optimal process of Example 4 is 56.07±0.97%, and the oil control rate of the shampoo in the control group is 48.43±1.27%, indicating that the shampoo sample has a better oil control effect.

[0119] (2) Antioxidant test

[0120] According to the method in Example 2, the Ganoderma lucidum compound shampoo of the present invention and the commercially available shampoo were used as the positive control group, and each was diluted 1 times with pure water to measure its clearance ability.

[0121] The results showed that the ABTS free radical scavenging rate of the 1-fold diluted Ganoderma lucidum compound shampoo (equivalent to the raw medicinal material concentration of 5 mg / mL) was 68.37±1.03%, and the ABTS free radical scavenging rate of the commercially available positive control shampoo diluted 1-fold was 51.23±0.72%, indicating that the Ganoderma lucidum compound shampoo sample has a good antioxidant effect.

[0122] from Figure 5 It can be seen that in the oil control experiment, the oil control rate of Lingzhi compound shampoo is 7.64% higher than that of the positive control group (p<0.0001), and the ABTS free radical scavenging rate of Lingzhi compound shampoo diluted 1 times is 17.14% higher than that of the control group diluted with the same times (p<0.0001). This shampoo can effectively protect hair.

[0123] The shampoo prepared in this study has the activity of scavenging ABTS free radicals by Ganoderma lucidum, Polygonum multiflorum, Gleditsia sinensis, Platycladus orientalis and black sesame. After the above six plants are compounded with shampoo, the Ganoderma lucidum compound shampoo has better efficacy and performance than the control group.

[0124] Example 7 Sensory Evaluation

[0125] Fifty healthy people aged 20 to 40 with correct discrimination ability were selected as volunteers. Each volunteer was given 10 mL of sample and asked to give sensory scores on the samples in four aspects: appearance, color, aroma, and foaming degree (each aspect has a full score of 25 points). The scoring standards were excellent (19-25 points), good (12-18 points), and passing (0-11 points). The scores of the volunteers were statistically analyzed using the questionnaire survey method, and the results are shown in Figure 14.

[0126] Table 13 Sensory evaluation standards for shampoo

[0127]

[0128]

[0129] Table 14 Shampoo sensory evaluation results

[0130]

[0131] The evaluation results of Lingzhi Shampoo's appearance, color, aroma, foaming degree and direct usability are all excellent. During the production process, high standards of quality control are followed, high-quality raw materials and formulas are used, and attention is paid to the practicality and user experience of the product.

[0132] Example 8 Evaluation of physical and chemical properties

[0133] Properties: By observing the color and gloss of the shampoo, we can judge whether the color and gloss of the product are comfortable, beautiful, uniform and without stratification. By smelling, we can check whether the product has a pungent smell. The relevant quality inspection of the "Safety Technical Specifications for Cosmetics" (2015 Edition) shows that the product is a yellow viscous liquid with a light Chinese herbal medicine fragrance, which meets the specified fragrance.

[0134] pH value determination: According to the national standard for the detection of pH value of cosmetics (GB / T13531.1-2008), the pH value of the shampoo sample was measured at room temperature of 25°C. The pH meter was calibrated according to the instrument instructions, the electrode was inserted into the shampoo, the reading was taken, and the data was recorded. The experiment was repeated three times. The result showed: 6.3±0.02, which is consistent with the value of human skin.

[0135] Viscosity: According to the national standard method for measuring liquid products by rotational viscometer for surfactants and detergents (GB / T15357), a rotational viscometer is used for measurement. Pour the Lingzhi compound shampoo into a 100mL beaker and let it stand at room temperature for 24 hours to remove bubbles. Then pour the shampoo into a 50mL beaker and adjust the shampoo to 25°C in a constant temperature water bath. Select a suitable rotor and immerse it in the test solution to prevent the shampoo from foaming. When the rotational viscometer reading is stable, record the data and repeat three times. The result shows: 9798±10.8mPa·s, the shampoo has moderate viscosity and is easy to apply.

[0136] Centrifugal test: According to the experimental method described in the National Standard of the People's Republic of China for Shampoo and Shampoo Cream (GB / T29679-2013), 10 mL of shampoo was centrifuged at 2000r / min, 3000r / min, 4000r / min, and 5000r / min for 10 minutes to observe whether the shampoo has stratification or separation. The results show that there is no precipitation or stratification of the shampoo at different centrifugal speeds.

[0137] Heat resistance test: According to the experimental method described in the National Standard of the People's Republic of China for Shampoo and Shampoo Cream (GB / T29679-2013), take two portions of shampoo, 10 mL each, place one portion of shampoo in a constant temperature incubator at 40±1℃ for 24 hours, then take it out, cool it to room temperature, and compare it with the other portion to observe whether the waterproofing becomes thinner, discolored, stratified, precipitated, etc. The results show that: at 40±1℃, placed for 24 hours, there is no obvious difference from before the experiment, and both can maintain the original state.

[0138] Cold resistance test: According to the test method described in the National Standard of the People's Republic of China for Shampoo and Shampoo Cream (GB / T29679-2013), take two portions of shampoo, 10 mL each, place one sample in a refrigerator at -15±1℃ for 24 hours, take it out, cool it to room temperature, and compare it with the other portion to observe whether the shampoo becomes thinner, discolored, stratified, precipitated, etc. The results show that: at -15±1℃, after being placed for 24 hours, there is no significant difference from before the experiment, and both can maintain their original state.

[0139] Hot and cold alternating test: According to the experimental method described in the National Standard of the People's Republic of China for Shampoo and Shampoo Cream (GB / T29679-2013), the shampoo still did not change its state by thinning, discoloration, stratification, or precipitation. The result shows that the shampoo has good stability.

[0140] The experimental results show that the shampoo has good stability in centrifugal test, heat resistance test and cold resistance test.

[0141] Example 9 Safety Evaluation

[0142] Skin irritation test method: 10 healthy volunteers aged 20-25 years old with correct identification ability were selected as volunteers. An area of ​​5 cm was selected behind the ears and the lower part of the palmar forearm of the volunteers. 2 Wipe the area with alcohol using a cotton swab, and keep the test area dry and clean. Apply shampoo evenly to the test area twice a day with a thickness of about 1mm. During the experiment, the test area of ​​the subject should be kept dry and clean, and observe the skin for abnormal phenomena such as erythema, edema and allergy after 2h, 4h, 8h, 16h, 32h and 48h.

[0143] Table 15 Human trial skin reaction scoring standards

[0144]

[0145] Skin irritation test: The irritation evaluation results showed that the volunteers did not experience allergic phenomena such as erythema and edema after applying the shampoo, and the evaluation level was 0.

Claims

1. A preparation method for a ganoderma lucidum compound shampoo, the raw materials comprising plant extract, detergents sodium sulfate of fatty alcohol polyoxyethylene ether and ammonium sulfate of fatty alcohol polyoxyethylene ether, combing agent hydrolyzed silk protein, viscosity agent sodium chloride, pH regulator citric acid, preservative phenoxyethanol, anti-dandruff agent piroctone olamine salt and pure water.

2. The ganoderma lucidum compound shampoo according to claim 1, wherein the compound plant extract is prepared by the following method: 3.0 g of ganoderma lucidum, 2.0 g of polygonum multiflorum, 1.8 g of sapodilla, 1.7 g of angelica, 1.2 g of platycladus orientalis, and 0.6 g of black sesame are crushed with a solid-liquid ratio of 1:20 (g / mL), soaked for 0.5 h, then the temperature is 90 ° C, and the extraction time is 3 h; after the extraction is completed, it is filtered with 3 layers of gauze, centrifuged at 4800 rpm for 10 min, and the supernatant is the plant extract, that is, the raw drug concentration is 50 mg / mL, its polysaccharide content is 28.9 ± 0.67%, and its flavonoid content is 3.91 ± 0.31%.

3. The plant extract according to claim 1, wherein the ABTS free radical scavenging rate of the plant extract is 69.56±1.54% when the raw material concentration is 5 mg / mL.

4. The Ganoderma lucidum compound shampoo according to claim 1, based on 100 mL, comprises 20 mL of plant extract, 20 g of AES:AESA (7:3), 2.2 g of hydrolyzed silk protein, 6 g of sodium chloride, 0.005 g of citric acid, 0.3 g of phenoxyethanol, and 0.005 g of piroctone olamine salt, and pure water is added to make up to 100 mL.

5. A method for preparing the Ganoderma lucidum compound shampoo according to claim 1, comprising the following steps: First, add AES, AESA and hydrolyzed silk protein into pure water at 80-85°C according to the mass ratio, stir until completely dissolved, then add citric acid, phenoxyethanol and piroctone olamine salt, after all dissolved, cool to 30-40°C, then add plant extract, and finally add sodium chloride in batches to adjust the viscosity, stir until there is no insoluble matter, and encapsulate to obtain the compound shampoo.

6. Use of the Ganoderma lucidum compound shampoo according to claim 1, wherein the oil control rate after 15 days is 56.27±0.97%, and the ABTS free radical scavenging rate of the shampoo containing 5 mg / mL of the raw medicinal material is 68.37±1.03%, which can improve the scalp environment, achieve the effects of oil control and anti-oxidation, and is safe and non-irritating.

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