CN111773165B - Hemerocallis fulva flower shampoo and preparation method thereof - Google Patents
Hemerocallis fulva flower shampoo and preparation method thereof Download PDFInfo
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Abstract
The invention discloses day lily flower shampoo and a preparation method thereof. The day lily flower shampoo comprises the following raw materials in parts by weight: 5 to 10 parts of day lily flower extract, 15 to 20 parts of sodium lauroyl sarcosinate, 8 to 12 parts of cocamidopropyl betaine, 4 to 8 parts of sodium cocoyl amphoacetate, 3 to 6 parts of polypropylene glycol-34, 1 to 4 parts of polyquaternary ammonium salt, 0.3 to 0.6 part of sodium hyaluronate, 0.2 to 0.5 part of EDTA-2Na, 0.1 to 0.3 part of citric acid, 0.3 to 0.8 part of sodium chloride, 0.1 to 0.4 part of lemon essence, 0.3 to 0.6 part of sodium benzoate and 100 parts of deionized water. The day lily flower extract is added into the shampoo, so that the use of chemical substances is reduced, the irritation to the scalp is reduced, the effects of moisture preservation, oxidation resistance, sterilization, inflammation resistance, allergy resistance and the like are achieved, the problems of scalp itching, scurf and the like can be solved, and the scalp health can be protected.
Description
Technical Field
The invention relates to day lily shampoo and a preparation method thereof, and belongs to the technical field of hair care products.
Background
Shampoo is a necessary washing and protecting product for everyone in modern life, and is mainly used for cleaning hair, chemical substances harmful to human hair and skin are mixed in the existing shampoo, for example, the shampoo mainly used for removing dandruff and containing ketoconazole and zinc pyrithione, partial people can be reflected in local irritation or allergy when in use, and some shampoos contain strongly irritating preservatives such as methylisothiazolinone and strongly cleaning anionic surfactants such as sodium lauryl sulfate, although the shampoo has a good short-term hair washing and protecting effect, the shampoo is not suitable for long-term washing and protecting, and is easy to cause certain damage to the scalp. Therefore, the development of mild shampoo with natural hair care function is not easy.
Hemerocallis fulva flower, also known as Hemerocallis citrina, hemerocallis fulva, and the like, is a perennial herb of Hemerocallis of Liliaceae (Liliaceae). The cultivation in China has a history of more than 3000 years. The hemerocallis fulva flowers are widely applied to medicine and food, contain various bioactive substances such as flavonoid, lactam, carotenoid, alkaloid and the like, and researches show that effective components extracted from the hemerocallis fulva flowers have the effects of resisting oxidation, inhibiting bacteria, resisting inflammation and the like. In the prior art, the plant shampoo is prepared by mixing the hemerocallis fulva leaf extract with other medicinal plants, but the hemerocallis fulva leaf is utilized, wherein the active component is different from that in the hemerocallis fulva flower, and the exerted effect is not obvious; the anti-dandruff shampoo prepared by mixing the hemerocallis fulva flower alcohol extract with other traditional Chinese medicine components is also beneficial, but the combination adopts monarch, minister, assistant and guide traditional Chinese medicines which are matched with each other, so that the active components in the hemerocallis fulva flower cannot be fully utilized, and the effect of the hemerocallis fulva flower extract is not clear. Therefore, in the prior art, the shampoo prepared by combining the hemerocallis fulva flower with other components does not exist, and the hemerocallis fulva flower extract is used as a main active component or a single active component.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the day lily flower shampoo is provided, and day lily flower extract containing the natural plant active component is added into the shampoo, so that scalp irritation caused by chemical substances is reduced, scalp itching, inflammation allergy, dandruff increase and other conditions can be relieved, scalp self-repair is promoted, and scalp health is improved.
In order to solve the problems, the invention provides day lily shampoo which is characterized by comprising the following raw materials in parts by mass: 5 to 10 parts of hemerocallis fulva extracting solution, 10 to 20 parts of sodium lauroyl sarcosinate, 8 to 12 parts of cocamidopropyl betaine, 4 to 8 parts of sodium cocoyl amphoacetate, 2 to 6 parts of polypropylene glycol-34, 1 to 4 parts of polyquaternary ammonium salt-10, 0.3 to 0.6 part of sodium hyaluronate, 0.2 to 0.5 part of EDTA-2Na, 0.1 to 0.3 part of citric acid, 0.3 to 0.8 part of sodium chloride, 0.1 to 0.4 part of lemon essence, 0.3 to 0.6 part of sodium benzoate and 100 parts of deionized water.
By adopting the technical scheme, the day lily flower extracting solution is used as a main and only active ingredient, so that the effects of moisturizing, resisting oxidation, relieving scalp inflammation, improving scalp itching, dandruff and the like of day lily flower are fully exerted, self repair of scalp is facilitated, scalp health is protected, and hair is smooth and soft after use.
Preferably, the raw materials comprise the following components in parts by mass: 5 parts of day lily flower extracting solution, 10 parts of sodium lauroyl sarcosinate, 8 parts of cocamidopropyl betaine, 8 parts of cocoyl ampho sodium acetate, 2 parts of polypropylene glycol-34, 3 parts of polyquaternary ammonium salt-10 parts of sodium hyaluronate, 0.2 part of EDTA-2Na, 0.1 part of citric acid, 0.4 part of sodium chloride, 0.1 part of lemon essence, 0.3 part of sodium benzoate and the balance of deionized water to 100 parts.
Preferably, the raw materials comprise the following components in parts by mass: 10 parts of day lily flower extracting solution, 20 parts of sodium lauroyl sarcosinate, 12 parts of cocamidopropyl betaine, 7 parts of cocoyl ampho sodium acetate, 3 parts of polypropylene glycol, 10 parts of polyquaternary ammonium salt, 0.5 part of sodium hyaluronate, 0.4 part of EDTA-2Na, 0.3 part of citric acid, 0.6 part of sodium chloride, 0.2 part of lemon essence, 0.4 part of sodium benzoate and 100 parts of deionized water.
Preferably, the hemerocallis fulva flower extract is prepared from hemerocallis fulva flower petals by freeze drying, ultrasonic extraction, centrifugation and concentration. The daylily flower extract can be independently prepared and used, and can be used in the fields of skin care products, cosmetics, shampoos and the like.
More preferably, before freeze drying, the petals of the daylily are washed by running water, and the petal fibers are not damaged in the washing process; and cleaning and then drying.
More preferably, the freeze-drying process parameters are: the temperature is minus 80 ℃ to minus 70 ℃, the freezing time is 24 hours to 48 hours, and the vacuum degree is less than or equal to 50pa. The drying process adopts cold trap drying, and the petals of the hemerocallis fulva are placed in a freezing tray for freeze drying. After drying, the hemerocallis fulva petals are crushed and sieved (preferably 50 meshes) to obtain hemerocallis fulva petal powder.
Further, the specific operation of ultrasonic extraction includes: adding deionized water into freeze-dried day lily flower petal powder according to the material-liquid ratio of (1) - (1).
Through ultrasonic pure water extraction, the active ingredients in the hemerocallis fulva flowers, such as SOD, flavone, polyphenol and other compounds, are high in content and rich in variety compared with other plant parts of the hemerocallis fulva, and can effectively play the roles of moisturizing, antioxidation, anti-inflammation, sterilization and the like.
Further, the centrifugation comprises the following specific steps: centrifuging the filtrate for 2-5 min at the temperature of 2-4 ℃ and the rotating speed of 7500-9500 rpm.
Further, the concentration comprises the following specific steps: evaporating and concentrating the centrifuged filtrate at the temperature of 70-80 ℃ and the rotating speed of 60-70 r/min to concentrate the filtrate to 10-20 times of the weight of the hemerocallis fulva powder, thus obtaining the hemerocallis fulva water extract.
The invention also provides a preparation method of the hemerocallis fulva flower shampoo, which is characterized by comprising the following steps of:
step S1, heating deionized water to 60-70 ℃, adding sodium lauroyl sarcosinate, and stirring for 10-15 minutes;
step S2: then adding cocamidopropyl betaine, sodium cocoyl amphoacetate, polypropylene glycol-34, polyquaternium-10, sodium hyaluronate, EDTA-2Na, citric acid and sodium benzoate in sequence, and maintaining constant-speed stirring at the temperature of 60-70 ℃ to dissolve and mix substances to form a transparent system;
and step S3: stopping heating, cooling, adding the hemerocallis fulva extract and the lemon essence when the temperature is reduced to 35-40 ℃, and continuing stirring;
and step S4: cooling to room temperature, gradually adding sodium chloride for thickening, sampling, checking the pH value and viscosity to be qualified, discharging, standing and filling.
By adopting the technical scheme, the effects of oxidation resistance, inflammation resistance, bacteriostasis, moisture preservation and the like of the active component of the hemerocallis fulva flower can be exerted to the maximum, the effects of other components can be ensured, and the prepared shampoo has a stable effect and has the basic characteristics of cleanness and smoothness.
Compared with the prior art, the invention has the beneficial effects that:
1) The day lily flower shampoo is simple in preparation method and low in cost, the natural plant active ingredient of the day lily flower extracting solution is added as a single active ingredient, the use of chemical substances is reduced to a certain extent, the day lily flower shampoo is safe and mild, and the irritation to the scalp is reduced;
2) The day lily shampoo has the effects of moisturizing and resisting oxidation, and by utilizing the benefits of day lily on skin, hair is fresh and soft after washing, the hair is easy to comb, and the self-repairing capacity of scalp is promoted;
3) The hemerocallis fulva flower shampoo disclosed by the invention has the effects of bacteriostasis, inflammation resistance and allergy resistance, can effectively relieve scalp itching, reduces dandruff and is beneficial to protecting scalp health.
Drawings
FIG. 1 is a graph showing the results of the irritation test of the daylily shampoo prepared in examples 1-3; wherein, A is a test result chart of the embodiment 1, B is a test result chart of the embodiment 2, and C is a test result chart of the embodiment 3;
FIG. 2 is a graph showing the results of the irritation test for the daylily shampoo prepared in comparative examples 1-3; wherein, A is a graph of the irritation test result of the shampoo added with hemerocallis fulva leaves in the comparative example 1, B is a graph of the irritation test result of the shampoo without hemerocallis fulva extract in the comparative example 2, and C is a graph of the irritation test result of the shampoo sold in the comparative example 3.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments are described in detail below with reference to the accompanying drawings.
The raw materials, effects and manufacturers used in the examples of the present invention are shown in Table 1.
TABLE 1
Example 1
The hemerocallis fulva flower shampoo comprises the following components in parts by weight: 5 parts of day lily flower extracting solution, 10 parts of sodium lauroyl sarcosinate, 8 parts of cocamidopropyl betaine, 8 parts of cocoyl ampho sodium acetate, 2 parts of polypropylene glycol-34, 3 parts of polyquaternary ammonium salt-10 parts of sodium hyaluronate, 0.2 part of EDTA-2Na, 0.1 part of citric acid, 0.4 part of sodium chloride, 0.1 part of lemon essence, 0.3 part of sodium benzoate and the balance of deionized water to 100 parts.
The preparation process of the day lily flower extracting solution comprises the following steps:
(1) Cleaning: the hemerocallis fulva flowers are washed for 3 times by using running water, and petal fibers are not damaged in the washing process; drying in the air and freeze-drying.
(2) And (3) freeze drying: adjusting the temperature of a cold trap of the vacuum freeze dryer to-75 ℃, wherein the vacuum degree of the cold trap is as follows: pre-running for 25min at a temperature of less than or equal to 10pa, placing daylily petals in a freezing tray, and regulating the temperature of a cold trap as follows: -80 ℃ and the freezing time: 30h, the vacuum degree of the cold trap is as follows: less than or equal to 50pa, and sieving with a 50-mesh sieve to obtain the day lily flower pollen.
(3) Ultrasonic extraction: weighing 5g of day lily flower pollen, adding 250g of deionized water according to the material-liquid ratio of 1.
(4) Centrifuging: centrifuging at 8000rmp at 4 deg.C for 5min to obtain centrifuged extractive solution.
(5) And (3) concentrating: concentrating the filtrate in a rotary evaporator at 70 deg.C and rotation speed of 70r/min, and concentrating the filtrate to obtain water extractive solution of flos Hemerocallis 10 times of the dry powder.
The preparation process of the hemerocallis fulva flower shampoo comprises the following steps:
(1) Heating deionized water to 65 ℃, adding sodium lauroyl sarcosinate, and stirring for 15 minutes;
(2) Sequentially adding cocamidopropyl betaine, sodium cocoyl amphoacetate, polypropylene glycol-34, polyquaternium-10, EDTA-2Na, citric acid and sodium benzoate, and stirring at a constant speed at 70 ℃ to dissolve and mix the substances to form a transparent system;
(3) Stopping heating, cooling, adding flos Hemerocallis extract and lemon essence when the temperature is reduced to 35 deg.C, and stirring;
(4) Cooling to room temperature, gradually adding a small amount of salt for thickening, sampling, checking the pH value and viscosity to be qualified, discharging, standing and filling.
Example 2
The hemerocallis fulva flower shampoo comprises the following components in parts by weight: 8 parts of day lily flower extracting solution, 15 parts of sodium lauroyl sarcosinate, 10 parts of cocamidopropyl betaine, 5 parts of cocoyl ampho sodium acetate, 3 parts of polypropylene glycol, 10 parts of polyquaternary ammonium salt, 0.4 part of sodium hyaluronate, 0.3 part of EDTA-2Na, 0.2 part of citric acid, 0.5 part of sodium chloride, 0.15 part of lemon essence, 0.3 part of sodium benzoate and 100 parts of deionized water.
The preparation process of the hemerocallis fulva flower extracting solution comprises the following steps:
(1) Cleaning: the hemerocallis fulva flowers are washed for 3 times by running water, and petal fibers are not damaged in the washing process; drying in the air and freeze-drying.
(2) And (3) freeze drying: adjusting the temperature of a cold trap of the vacuum freeze dryer to-75 ℃, wherein the vacuum degree of the cold trap is as follows: pre-running for 35min at a temperature of less than or equal to 10pa, placing daylily petals in a freezing tray, and regulating the temperature of a cold trap as follows: -80 ℃ and freezing time: and 35h, the vacuum degree of the cold trap is as follows: less than or equal to 50pa, and sieving with a 50-mesh sieve to obtain the day lily flower pollen.
(3) Ultrasonic extraction: weighing 5g of day lily flower pollen, adding 200g of deionized water according to a material-liquid ratio of 1.
(4) Centrifuging: centrifuging at 4 deg.C and 8500rmp for 3min to obtain centrifuged extractive solution.
(5) And (3) concentrating: evaporating and concentrating the filtrate obtained after centrifugation in a rotary evaporator at the temperature of 75 ℃ and the rotating speed of 65r/min, and concentrating the filtrate by 10 times of the weight of the dry powder to obtain the water extract of the hemerocallis fulva flowers.
The preparation process of the hemerocallis fulva flower shampoo comprises the following steps:
(1) Heating deionized water to 65 ℃, adding sodium lauroyl sarcosinate, and stirring for 15 minutes;
(2) Sequentially adding cocamidopropyl betaine, sodium cocoamphoacetate, polypropylene glycol-34, polyquaternium-10, EDTA-2Na, citric acid and sodium benzoate, and stirring at a constant speed at the temperature of 75 ℃ to dissolve and mix the substances into a transparent system;
(3) Stopping heating, cooling, adding flos Hemerocallis extract and lemon essence when the temperature is reduced to 35 deg.C, and stirring;
(4) Cooling to room temperature, gradually adding a small amount of salt for thickening, sampling, checking the pH value and viscosity, discharging, standing and filling.
Example 3
The formula of the hemerocallis fulva flower shampoo comprises: 10 parts of day lily flower extract, 20 parts of sodium lauroyl sarcosinate, 12 parts of cocamidopropyl betaine, 7 parts of sodium cocoyl amphoacetate, 3 parts of polypropylene glycol-34, 10 parts of polyquaternary ammonium salt-10 parts of sodium hyaluronate, 0.4 part of EDTA-2Na, 0.3 part of citric acid, 0.6 part of sodium chloride, 0.2 part of lemon essence, 0.4 part of sodium benzoate and 100 parts of deionized water.
The preparation process of the day lily flower extracting solution comprises the following steps:
(1) Cleaning: the hemerocallis fulva flowers are washed for 3 times by running water, and petal fibers are not damaged in the washing process; drying in the air and freeze-drying.
(2) And (3) freeze drying: the temperature of a cold trap of the vacuum freeze dryer is adjusted to-75 ℃, and the vacuum degree of the cold trap is as follows: pre-running for 30min at a temperature of less than or equal to 10pa, placing the petals of the hemerocallis fulva in a freezing tray, and regulating the temperature of a cold trap to be as follows: -80 ℃ and the freezing time: 32h, the vacuum degree of the cold trap is: less than or equal to 50pa, and sieving with a 50-mesh sieve to obtain the day lily flower pollen.
(3) Ultrasonic extraction: weighing 5g of day lily flower pollen, adding 150g of deionized water according to a material-liquid ratio of 1.
(4) Centrifuging: centrifuging at 9000rmp for 2min at 4 deg.C to obtain centrifuged extractive solution.
(5) And (3) concentrating: concentrating the filtrate in a rotary evaporator at 80 deg.C and rotation speed of 60r/min, and concentrating the filtrate to obtain water extractive solution of flos Hemerocallis 10 times of the dry powder.
The preparation process of the hemerocallis fulva flower shampoo comprises the following steps:
(1) Heating deionized water to 70 ℃, adding sodium lauroyl sarcosinate, and stirring for 10 minutes;
(2) Sequentially adding cocamidopropyl betaine, sodium cocoyl amphoacetate, polypropylene glycol-34, polyquaternium-10, EDTA-2Na, citric acid and sodium benzoate, and stirring at a constant speed at 80 ℃ to dissolve and mix the substances to form a transparent system;
(3) Stopping heating, cooling, adding flos Hemerocallis extract and lemon essence when the temperature is reduced to 40 deg.C, and stirring;
(4) Cooling to room temperature, gradually adding a small amount of salt for thickening, sampling, checking the pH value and viscosity to be qualified, discharging, standing and filling.
Comparative example 1
The formula of the hemerocallis fulva leaf shampoo comprises the following components: 10 parts of day lily leaf extracting solution, 20 parts of sodium lauroyl sarcosinate, 12 parts of cocamidopropyl betaine, 7 parts of sodium cocoyl amphoacetate, 3 parts of polypropylene glycol-34, 10 parts of polyquaternary ammonium salt-10 parts of sodium hyaluronate, 0.4 part of EDTA-2Na, 0.3 part of citric acid, 0.6 part of sodium chloride, 0.2 part of lemon essence, 0.4 part of sodium benzoate and 100 parts of deionized water.
The preparation method of the extracting solution of the hemerocallis fulva leaves is the same as that in example 1, and the preparation process of the shampoo is the same as that in example 1.
Comparative example 2
The shampoo comprises the following components in parts by weight: 20 parts of sodium lauroyl sarcosinate, 12 parts of cocamidopropyl betaine, 7 parts of sodium cocoyl amphoacetate, 3 parts of polypropylene glycol-34, 4 parts of polyquaternary ammonium salt-10, 0.5 part of sodium hyaluronate, 0.4 part of EDTA-2Na, 0.3 part of citric acid, 0.6 part of sodium chloride, 0.2 part of lemon essence, 0.4 part of sodium benzoate and 52 parts of deionized water. The preparation method is the same as that in example 3 except that the hemerocallis fulva flower extracting solution is not contained and deionized water is used for supplementing, and the process flow of shampoo preparation is the same as that in example 3.
Comparative example 3
A shampoo is sold in the market.
1. Evaluation of Properties
The shampoos prepared in examples 1-3 and comparative examples 1-3 were subjected to the performance test, and the results are shown in table 2.
TABLE 2
As can be seen from table 2, the shampoo formulation of the present invention is sufficiently feasible and meets the national standards, and can increase the smoothness of hair (i.e., reduce combing power), improve the feeling of use, and maintain a suitable degree of foam enrichment. Compared with the shampoos without the hemerocallis fulva flower extract and the hemerocallis fulva leaf extract, the shampoo with the hemerocallis fulva flower extract has small dry and wet combing power after use, and is easier to comb.
2. Irritation test
The shampoos of examples 1 to 3 and comparative examples 1 to 3 were formulated into a 1% by mass solution with deionized water.
According to the standards of cosmetic eye irritation/corrosiveness chick embryo chorioallantoic membrane tests in the entry-exit inspection and quarantine industry standards, a reaction time method is adopted in the research, egg examination is carried out on 9-day-old chick embryos, and the positions of air chambers are marked on the surfaces of eggshells; the marked eggshell portion was stripped with dental saw bent forceps to expose the white eggshell membrane. Sucking appropriate amount of NaCl solution 0.9% (by mass) with pipette to moisten egg membrane, and pouring out. Carefully remove the intima with forceps to ensure the vascular membrane is not damaged. 0.3mL of the test agent is respectively sucked and dripped on the surface of the chorioallantoic membrane, the time for beginning bleeding, vessel thawing and blood coagulation within 5min is recorded, and video recording and photo taking are carried out during the period.
According to the test of chick embryo chorioallantoic membrane for irritation/corrosiveness of cosmetics eyes, a reaction time method, namely an IS (irritation score) method IS adopted as a scoring standard, and the calculation formula IS as follows:
in the formula, secH (bleeding time): the average time in seconds(s) at which bleeding begins to occur on the CAM membrane;
secL (vascular fusion time): the average time to onset of vascular melting observed on the CAM membrane in seconds(s);
secC (clotting time): the mean time to onset of clotting observed on the CAM membrane is given in table 3 as the classification criteria for the second(s) stimulation score.
TABLE 3
| Stimulation scoring | Irritation classification |
| IS＜1 | Has no irritation |
| 1≤IS＜5 | Light irritation |
| 5≤IS＜9 | Moderate irritation |
| IS≥10 | Strong irritation/corrosion |
The irritation results are shown in Table 4, and bleeding is shown in FIGS. 1-2.
TABLE 4
From the above results, it can be seen that the shampoos of examples 1 to 3 and comparative examples 1 to 3 are both light-irritant, and it is seen that the shampoo formula is mild and has little irritation to the scalp, and is suitable for most people, and as can be seen from comparison between examples 1 to 3 and comparative examples 1 to 3, compared with the shampoo without the added daylily flower extract and the shampoo with the added daylily leaf extract, the shampoo with the added daylily flower extract has a smaller irritation score, and it is seen that the daylily flower extract has an effect of relieving the irritation of the shampoo to a certain extent.
3. DPPH clearance rate
The DPPH clearance of the shampoos of examples 1-3 and comparative examples 1-3 were determined separately. 2.0X 10-4mol/L DPPH prepared in absolute ethanol, blank sample DPPH absorbance (A0) determination: transferring 4mL of absolute ethyl alcohol, adding 2mL of DPPH solution, fully and uniformly mixing, and measuring the absorbance of the solution at 517 nm; measurement of DPPH + shampoo sample liquid Absorbance (A1): respectively transferring 2mL of sample liquid with a certain concentration, adding 2mL of DPPH solution, transferring 2mL of absolute ethyl alcohol, fully mixing, reacting for 30min at room temperature in a dark place, and measuring absorbance at 517 nm; measurement of Absorbance (A2) of Hemerocallis shampoo sample by transferring 2mL of the sample solution of the same concentration, adding 4mL of absolute ethanol, mixing, and measuring Absorbance at 517 nm. The clearance rate is calculated as follows:
in the formula, A 0 : absorbance value of blank control;
A 1 : absorbance values of the samples after reaction with DPPH;
A 2 : the absorbance values of DPPH were replaced with the same volume of deionized water.
The results of the DPPH radical scavenging ability measurement are shown in Table 5.
TABLE 5
As shown in Table 5, the shampoo containing the extract of Hemerocallis fulva in example 1-3 and comparative example 1-3 showed higher DPPH clearance, and the shampoo in example 3 showed the highest DPPH clearance, indicating the strongest oxidation resistance.
4. Antibacterial test (in vitro drug sensitive MIC test)
Preparing a bacterial suspension from each test strain (staphylococcus aureus, escherichia coli, candida albicans and malassezia furfur) subjected to subculture by using normal saline, enabling the bacterial content to be 1.0 multiplied by 107CFU/mL, diluting a test group (shampoo in examples 1-3 and comparative examples 1-3 of the invention) and a positive control group (zinc pyrithione) to different concentrations by using an Oxford cup bacteriostasis method, uniformly coating a certain amount of test bacterial liquid on a culture medium plate, gently placing a sterile Oxford cup into a culture dish by using tweezers, adding sample liquid with different concentrations into the Oxford cup, and culturing for 24 hours in a constant-temperature incubator at 37 ℃, wherein the results are shown in Table 6.
TABLE 6 minimum inhibitory concentrations (unit: mg/mL) of test samples against various microorganisms
| Examples | Staphylococcus aureus | Escherichia coli | Candida albicans | Malassezia furfur var (berk.) Kuntze |
| Example 1 | 2.41±0.51 | 3.10±1.30 | 1.88±0.85 | 1.46±0.66 |
| Example 2 | 2.62±0.90 | 2.84±0.61 | 1.67±0.32 | 1.33±0.72 |
| Example 3 | 1.62±0.51 | 2.58±0.11 | 1.51±0.36 | 1.07±0.13 |
| Comparative example 1 | 2.80±1.26 | 3.06±0.71 | 1.97±0.36 | 1.55±0.63 |
| Comparative example 2 | 3.02±1.71 | 3.40±0.50 | 2.33±0.46 | 1.83±0.50 |
| Comparative example 3 | 2.82±1.33 | 3.22±1.02 | 1.99±0.76 | 1.69±0.81 |
| Control group | 2.2±0.56 | 2.62±2.03 | 1.84±0.02 | 1.13±0.21 |
As is apparent from table 6, from comparison between examples 1 to 3 and comparative examples 1 to 3, the MIC value of the shampoo containing the extract solution of daylily flower is lower than that of the shampoo containing no extract solution of daylily flower and the shampoo containing the extract solution of daylily leaf, indicating that the daylily flower shampoo has a good effect of inhibiting various bacteria such as malassezia furfur and staphylococcus aureus which can cause dandruff, and the effect is equivalent to that of zinc pyrithione. Among them, the bacteriostatic effect of example 3 was the best.
5. Anti-inflammatory and anti-allergy assays
The hyaluronidase inhibition was determined by the ELsonn-Morga method.
0.5mL of hyaluronidase (500U/mL) is added into tubes A and C, 0.5mL of acetic acid buffer solution is added into tubes B and D, 0.1mL of 2.5mmol/LCaCl2 is respectively added into four tubes, the temperature is kept for 20 minutes at 37 ℃,0.5mL of sample solution is added into tubes A and B, distilled water is added into tubes C and D, the temperature is kept for 20 minutes at 37 ℃,0.5mL of sodium hyaluronate solution (0.5 mg/mL) is added into tubes A and C, 0.5mL of acetic acid buffer solution is added into tubes B and D, the temperature is kept for 40 minutes at 37 ℃, the tubes are placed at room temperature for 10 minutes, 1mL of acetylacetone is added, the reaction is finished after 15 minutes of boiling water bath, 1.0mL of P-DAB color developing agent is added after cooling, 0.4mL of ethanol solution is added, the tubes are placed at room temperature for 30 minutes, and then the light absorption value A value is measured at 530 nm. The calculation formula of the hyaluronidase inhibition ratio is as follows:
in the formula, A: absorbance values of the (hyaluronidase + sample + sodium hyaluronidase) solution;
b: (acetic acid buffer + sample + acetic acid buffer) solution absorbance value;
c: (hyaluronidase + distilled water + sodium hyaluronidase) solution absorbance values;
d: absorbance values of (acetate buffer + distilled water + acetate buffer) solutions.
The hyaluronidase inhibition rates are shown in table 7.
TABLE 7
| Sample(s) | Hyaluronidase inhibition (%) |
| Example 1 | 43.6±1.59 |
| Example 2 | 68.01±0.33 |
| Example 3 | 78.32±1.63 |
| Comparative example 1 | 32.78±1.02 |
| Comparative example 2 | 21.65±1.70 |
| Comparative example 3 | 23.14±1.09 |
According to table 7, as can be seen from comparison between examples 1 to 3 and comparative examples 1 to 3, the hyaluronidase inhibition rate of the shampoo containing the daylily flower extract is higher, and the hyaluronidase inhibition rate of the shampoo of example 3 is the highest, which indicates that the shampoo has the strongest anti-inflammatory and anti-allergy capabilities.
6. Human body experiment
120 (male and female halves) patients with itchy head and dandruff, which are 20-30 years old, are selected, the shampoos of the embodiments 1-3 and the comparative example 1 are adopted for experiments, each embodiment corresponds to 30 (male and female halves), the shampoos are used for 2 times each day, 30 days are continuously observed, the scalp itching and dandruff removing conditions and the hair conditions after use are observed, and the statistical number of the test results is shown in a table 8.
TABLE 8
As can be seen from table 8, the hemerocallis fulva shampoo provided by the invention can improve the problems of itching and scurf, and can keep the hair smooth and soft without damaging the hair quality. By comparing examples 1 to 3 with comparative examples 1 to 3, the shampoo containing the daylily flower extract is more effective in improving scalp itching and dandruff than the shampoo containing no daylily flower extract, and the effect of example 3 is the best.
Claims (4)
1. The hemerocallis fulva flower shampoo is characterized by comprising the following raw materials in parts by mass: 5 to 10 parts of a tawny daylily flower extracting solution, 10 to 20 parts of sodium lauroyl sarcosinate, 8 to 12 parts of cocamidopropyl betaine, 4 to 8 parts of sodium cocoamphoacetate, 2 to 6 parts of polypropylene glycol-34, 1 to 4 parts of polyquaternium-10, 0.3 to 0.6 part of sodium hyaluronate, 0.2 to 0.5 part of EDTA-2Na, 0.1 to 0.3 part of citric acid, 0.3 to 0.8 part of sodium chloride, 0.1 to 0.4 part of lemon essence, 0.3 to 0.4 part of sodium benzoate and 100 parts of deionized water; the hemerocallis fulva flower extracting solution is prepared by freeze drying hemerocallis fulva flower petals, ultrasonic extracting, centrifuging and concentrating; the hemerocallis fulva petals are washed by running water before being frozen and dried, and petal fibers are not damaged in the washing process; cleaning and then drying; the freeze drying process parameters are as follows: the temperature is minus 80 to minus 70 ℃, the freezing time is 24 to 48h, and the absolute pressure is less than or equal to 50pa; the specific operation of ultrasonic extraction comprises the following steps: adding deionized water into freeze-dried petal powder of the daylily flower according to a material-liquid ratio of 1 to 30 to 1, carrying out ultrasonic extraction at a working frequency of 40kHz and a temperature of 40 to 60 ℃ for 30 to 50min, and filtering to obtain a filtrate; the centrifugation comprises the following specific steps: centrifuging the filtrate for 2 to 5min under the conditions of the temperature of 2 to 4 ℃ and the rotating speed of 7500 to 9500rpm; the concentration comprises the following specific steps: and (3) evaporating and concentrating the filtrate after centrifugation at the temperature of 70-80 ℃ and the rotating speed of 60-70r/min to obtain the filtrate, and concentrating the filtrate to be 10-20 times of the weight of the hemerocallis fulva flower powder to obtain the hemerocallis fulva flower water extract.
2. The day lily shampoo as claimed in claim 1, wherein the raw materials comprise the following components in parts by mass: 5 parts of day lily flower extract, 10 parts of sodium lauroyl sarcosinate, 8 parts of cocamidopropyl betaine, 8 parts of sodium cocoyl amphoacetate, 2 parts of polypropylene glycol-34, 3 parts of polyquaternary ammonium salt-10, 0.3 part of sodium hyaluronate, 0.2 part of EDTA-2Na, 0.1 part of citric acid, 0.4 part of sodium chloride, 0.1 part of lemon essence, 0.3 part of sodium benzoate and 100 parts of deionized water.
3. The hemerocallis fulva flower shampoo as set forth in claim 1, wherein the raw materials comprise the following components in parts by mass: 10 parts of day lily flower extract, 20 parts of sodium lauroyl sarcosinate, 12 parts of cocamidopropyl betaine, 7 parts of sodium cocoyl amphoacetate, 3 parts of polypropylene glycol-34, 4 parts of polyquaternary ammonium salt-10, 0.5 part of sodium hyaluronate, 0.4 part of EDTA-2Na, 0.3 part of citric acid, 0.6 part of sodium chloride, 0.2 part of lemon essence, 0.4 part of sodium benzoate and 100 parts of deionized water.
4. The method for preparing day lily shampoo according to any one of claims 1 to 3, comprising the following steps:
s1, heating deionized water to 60-70 ℃, adding sodium lauroyl sarcosinate, and stirring for 10-15 minutes;
step S2: sequentially adding cocamidopropyl betaine, sodium cocoamphoacetate, polypropylene glycol-34, polyquaternium-10, sodium hyaluronate, EDTA-2Na, citric acid and sodium benzoate, and stirring at a constant speed at the temperature of 60-70 ℃ to dissolve and mix substances to form a transparent system;
and step S3: stopping heating, cooling, adding the daylily flower extracting solution and the lemon essence when the temperature is reduced to 35-40 ℃, and continuing stirring;
and step S4: cooling to room temperature, gradually adding sodium chloride for thickening, sampling, checking the pH value and viscosity to be qualified, discharging, standing and filling.
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