CN115607497A - Angelica compound shampoo with function of treating seborrhea dermatitis - Google Patents
Angelica compound shampoo with function of treating seborrhea dermatitis Download PDFInfo
- Publication number
- CN115607497A CN115607497A CN202211266005.XA CN202211266005A CN115607497A CN 115607497 A CN115607497 A CN 115607497A CN 202211266005 A CN202211266005 A CN 202211266005A CN 115607497 A CN115607497 A CN 115607497A
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- CN
- China
- Prior art keywords
- angelica
- compound
- surfactant
- shampoo
- angelica sinensis
- Prior art date
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Abstract
The invention discloses a Chinese angelica compound shampoo with a function of treating seborrhea dermatitis. The angelica compound shampoo is prepared from an angelica compound extract, a surfactant, a cation conditioner, a humectant, a chelating agent, a thickening agent, a solvent and a preservative; the angelica compound shampoo comprises the following components in parts by mass: 0-100% of angelica sinensis compound extract, 0-100% of surfactant, 0-5% of cation conditioner, 0-100% of humectant, 0-1% of chelating agent, 0-20% of thickener, 0-100% of solvent and 0-1% of preservative, wherein the contents of the components are not zero, and the angelica sinensis compound extract is prepared from the following components in percentage by mass: 15-30 g of angelica, 30-45 g of astragalus, 15-30 g of mulberry leaf, 12-30 g of cacumen biotae, 10-20 g of wild chrysanthemum, 12-36 g of codonopsis pilosula, 9-30 g of mint and 6-24 g of rhizoma cyperi. The shampoo disclosed by the invention has an obvious inhibition effect on malassezia and staphylococcus aureus, and can reduce scalp grease secretion and inhibit dandruff generation.
Description
Technical Field
The invention relates to a Chinese angelica compound shampoo with a function of treating seborrhea dermatitis, and belongs to the technical field of washing and caring products.
Background
Seborrheic dermatitis is a common chronic inflammatory disease of the dermatology department, which takes the head and the face as the good hair parts and is common in young and old people or infants. The main clinical manifestations of scalp involvement are that greasy scales are covered on the basis of erythema, pruritus and scalp odor are accompanied, and symptoms such as erosion, exudation, folliculitis and alopecia are accompanied in severe cases, which bring certain influence to the psychology and life of patients. The incidence of seborrheic dermatitis is closely related to immune dysfunction and malassezia furfur infection. The currently accepted main reasons are that sebum is over-secreted, malassezia furfur is over-proliferated, so that local inflammation is induced, and antifungal medicines are mainly used for treatment. At present, the western medicine treatment generally adopts methods such as sebum steroid hormone, antifungal, antiandrogen, anti-inflammatory and the like, but has high recurrence rate, high price and great side effect.
The seborrheic dermatitis is called as 'seborrheic dermatitis' and 'facial wandering wind' in traditional Chinese medicine, and the traditional Chinese medicine believes that the skin heat generates wind, wind evil invades pores, the skin is stagnated for a long time and becomes dry, the skin is not nourished, or the lung is dry, blood heat and stagnated in the skin, or the spleen and the stomach are abnormally transported and transformed due to overeating fat, sweet and thick taste, the dampness is generated and the heat is transformed, and the skin (fumigating the head and the face) overflows. Is prepared through a certain preparation process. For it is suitable for tonifying qi and blood (invigorating spleen to resolve dampness), clearing heat, cooling blood and removing toxicity. The traditional Chinese medicine treatment comprises oral administration and external application of traditional Chinese medicines, acupuncture therapy, percussing with plum-blossom needles and the like. The external application of the traditional Chinese medicine can make the efficacy of the medicine directly reach the focus, and the local treatment effects of dredging the channels and collaterals, clearing away heat and toxic materials, eliminating dampness and fat, eliminating wind and relieving itching and the like are achieved. The existing dosage forms for external treatment of traditional Chinese medicines comprise lotion, tincture, liniment and the like, but the traditional Chinese medicines have certain limitations due to special taste and irritation (such as tincture) of the dosage forms.
In order to facilitate patients and improve the cure rate of seborrheic dermatitis, a bacterium-inhibiting and dandruff-removing shampoo needs to be provided urgently.
Disclosure of Invention
The invention aims to provide the angelica compound shampoo which has an inhibiting effect on malassezia, can reduce scalp grease secretion and inhibit dandruff generation, and is a product with safe components, strong oxidation resistance, good stability and strong bacteriostatic effect.
The invention firstly provides a Chinese angelica compound shampoo which is prepared from the following components in parts by mass:
15 to 30g of angelica, 30 to 45g of astragalus, 15 to 30g of mulberry leaf, 12 to 30g of cacumen biotae, 10 to 20g of wild chrysanthemum, 12 to 36g of codonopsis pilosula, 9 to 30g of mint and 6 to 24g of rhizoma cyperi.
The preparation method of the angelica sinensis compound extract comprises the following steps:
the extraction is performed with an extraction solvent, which may be, but is not limited to: water, ethanol solution with volume fraction of 0-100%, petroleum ether solution, ethyl acetate solution and the like;
the extraction method can be, but is not limited to: heating reflux extraction, distillation extraction, decoction, percolation, extraction and the like;
the solid-to-liquid ratio can be 6-12: 1.
preferably, the extraction method of the angelica sinensis compound is as follows:
mixing and crushing Chinese angelica compound, adding a mixture of Chinese angelica and Chinese angelica according to a liquid-solid ratio of 10:1, heating and refluxing the ethanol solution with the volume concentration of 75% at the temperature of 80 ℃, extracting for 1h, taking filter residue, and adding the mixture into the mixture with the liquid-solid ratio of 8:1 in 75% strength by volume ethanol and 2 filtrates are combined.
On the basis of the angelica compound extract, the invention further provides an angelica compound shampoo which is prepared from the angelica compound extract, a surfactant, a cation conditioner, a humectant, a chelating agent, a thickening agent, a solvent and a preservative;
the angelica sinensis compound shampoo comprises the following components in parts by mass:
0-100% of angelica compound extract, 0-100% of surfactant, 0-5% of cation conditioner, 0-100% of humectant, 0-1% of chelating agent, 0-20% of thickener, 0-100% of solvent and 0-1% of preservative.
Preferably, the angelica sinensis compound shampoo comprises the following components in percentage by mass:
5 to 15 percent of angelica compound extract, 20 to 40 percent of surfactant, 0.4 to 0.8 percent of cation conditioner, 1 to 8 percent of humectant, 0.1 to 0.5 percent of chelating agent, 1 to 5 percent of thickening agent, 0.1 to 0.5 percent of preservative, and the balance of solvent.
Further preferably, the angelica sinensis compound shampoo comprises the following components in percentage by mass:
10% of angelica compound extract, 30% of surfactant, 0.6% of cation conditioner, 5% of humectant, 0.1% of chelating agent, 3% of thickening agent, 0.1% of preservative and the balance of solvent.
Preferably, the surfactant is at least one of an anionic surfactant, a zwitterionic surfactant and a nonionic surfactant;
the anionic surfactant is an amino acid surfactant or a sulfate surfactant.
Preferably, the anionic surfactants include, but are not limited to: lauroyl sarcosine LS-30, ammonium laureth sulfate ALES;
the zwitterionic surfactants include, but are not limited to: cocamidopropyl betaine CAB-35,
the nonionic surfactants include, but are not limited to: alkyl glycoside APG1214, cocamide methyl MEA.
Further, the anionic surfactant is a combination of:
lauroyl sarcosine LS-30, ammonium laureth sulfate ALES, cocamidopropyl betaine CAB-35, alkyl glycoside APG1214, cocamidomethyl MEA;
the preferred mass ratios are as follows:
lauroyl sarcosine LS-30.24%, lauryl alcohol ether ammonium sulfate ALES 11.24%, cocamidopropyl betaine CAB-35.02%, alkyl glycoside APG1214 1.00%, cocamidomethyl MEA 2.50%.
Preferably, the cationic conditioning agents include, but are not limited to: guar gum, polyquaternium compounds;
the polyquaternium compound comprises quaternary ammonium salt-10, quaternary ammonium salt-7 and quaternary ammonium salt-15;
in the cationic conditioner, the mass ratio of the guar gum to the polyquaternium compound is (0).
Preferably, the humectants include, but are not limited to: propylene glycol, glycerin;
preferably, the chelating agent includes, but is not limited to: disodium ethylene diamine tetraacetate EDTA-2Na, tetrasodium ethylene diamine tetraacetate EDTA-4Na;
preferably, the thickening agents include, but are not limited to: sodium chloride and cocamide methyl MEA;
preferably, the solvents include, but are not limited to: deionized water, double distilled water, propylene glycol, glycerol, pentanediol and hexanediol;
preferably, the preservative is a chemical preservative or a natural preservative, including but not limited to: nipagin esters, cason and p-hydroxyacetophenone.
The angelica compound shampoo prepared by the embodiment of the invention is detected according to the physicochemical indexes of the national standard, and has light brown color, traditional Chinese medicine taste, pH value of 6.17, good cold resistance and heat resistance, foam thickness of 136mm and total solid content of 20.41 percent.
The content of 4 active ingredients in the angelica compound extract adopted by the embodiment of the invention is respectively determined to be rutin 372.1649 mug.g by adopting high performance liquid chromatography -1 Quercetin 953.1612 microgram g -1 Polygonum aviculare glycoside 160.8286 mug. Multidot.g -1 Quercetin 631.6464 mug. Multidot.g -1 。
A series of in vitro antioxidant test results show that the antioxidant capacity of the angelica compound extract is enhanced along with the increase of the content of total flavonoids in a certain concentration range.
The liquid-based dilution method is used for determining the effect of the angelica sinensis compound shampoo on inhibiting malassezia, and the result shows that the angelica sinensis compound shampoo has a remarkable inhibiting effect on the malassezia, and the inhibiting rate is about 21.7-85.0%.
The angelica sinensis compound shampoo is used for inhibiting staphylococcus aureus by a bacteriostatic ring method, and the result shows that the angelica sinensis compound shampoo has a remarkable inhibiting effect on the staphylococcus aureus.
Compared with the prior art, the invention has the beneficial effects that:
(1) The invention carries out content measurement on 4 effective components in the angelica compound extract and researches the antioxidation of the angelica compound extract. Research shows that the Chinese angelica compound extract has strong antioxidation and gradually increases the mass concentration range of the tested total flavone.
(2) The invention screens the proportion and the total amount of the anionic surfactant and the cationic conditioner to determine the optimal formula of the angelica compound shampoo.
The shampoo disclosed by the invention has an obvious inhibition effect on malassezia and staphylococcus aureus, and can reduce scalp grease secretion and inhibit dandruff generation.
The invention fundamentally removes the scurf by combining the functions of antioxidation and bacteriostasis.
Drawings
FIG. 1 shows the effect of different concentrations of the Angelica sinensis compound shampoo on the activity of Malassezia (P < 0.05;. P < 0.01;. P < 0.001;. P < 0.0001).
FIG. 2 is a graph showing the effect of different shampoo volume concentrations on Staphylococcus aureus activity; position 1: sterile water; position 2: shampoo with volume concentration of 0.1; position 3: shampoo with volume concentration of 0.4; position 4: shampoo with volume concentration of 0.8.
Detailed Description
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
The main materials, reagents and instruments used in the following examples are as follows:
angelica sinensis (batch number: 20190820), hebei Quantai pharmaceutical Co., ltd, and other herbs were purchased from Beijing Tongrentang. Rutin (lot number: 7916, purity 90.2%), quercetin (lot number: 8173, purity 88.2%), quercetin (lot number: 5951, purity 91.9%), polygonin (lot number: 6454, purity 99.3%), shanghai Shidande Standard technology services, inc.; TPTZ (batch No. C10928364), shanghai Mielin Biotechnology Ltd; DPPH (batch number: D4313), TCI Chiloe (Shanghai) chemical industry development Co., ltd; 30% hydrogen peroxide (batch: 20160601), fengshan chemical reagents science and technology, tianjin; ferric chloride (batch No. 20100910), kyou chemist co ltd, tianjin.
Sodium lauroyl sarcosinate LS-30, cocamidopropyl betaine CAB-35, laureth ammonium sulfate ALES, cocamidomethyl MEA, disodium EDTA-2Na, alkyl glycoside APG1214, cationic hydroxyethyl cellulose, guar hydroxypropyl trimonium chloride (batch No.: 089391007100, 089194005100, 089191005200, 039296002060, 0404109, 079117664560, 039420002050, 075007030) were provided by Shandong Yokoku technical Co., ltd.
Beef extract, batch No.: 20211218, tokyo star biotechnology, llc of beijing; peptone, lot No.: 20211024, bio-technology ltd, obo star, beijing; sodium chloride, batch No.: 20181109, shin-shin science and technology development ltd, tianjin; agar, lot No.: 2018906, tianjin Guangfu technology development Co., ltd.
Malassezia is provided by Guangdong collection of microorganisms, olive oil liquid medium is provided by Beijing three-medicine technology development company, and ketoconazole is produced by Nanjing Baijing pharmacy Limited liability company.
Staphylococcus aureus (Staphylococcus aureus) was maintained in the microbiological laboratory of Shanxi university of medicine (in Shanxi).
Model L-3500 HPLC chromatograph, RIGOL technologies, inc.; multiskan FC microplate reader, thermo Fisher instruments ltd.
SCB-1520 clean bench, beijing Dong Union Harr Instrument manufacturing, inc.; HXP-9082MBE electric heating constant temperature incubator, shanghai Bo Xun medical biological instruments, inc.; DY04-13-44-00 vertical pressure steam sterilizer, manufactured by east Asia pressure vessel of Shanghai, ltd.; filter paper (6 mm, after pressure steam sterilization, baking at 120 deg.C for 2h, storing for use).
Example 1 preparation and Performance measurement of Compound extract of Angelica sinensis
1. Preparation of compound angelica extract
The weight portions of the components are as follows:
20g of angelica sinensis, 30g of astragalus membranaceus, 20g of mulberry leaves, 18g of cacumen biotae, 16g of wild chrysanthemum, 30g of codonopsis pilosula, 18g of mint and 12g of rhizoma cyperi.
Taking a Chinese angelica compound, crushing medicinal materials (sieving the medicinal materials by a No. 5 sieve after crushing, uniformly mixing), then mixing, adding 75% ethanol solution with the liquid-solid ratio of 10 to perform heating reflux extraction at the temperature of 80 ℃, extracting for 1h, taking filter residues, adding 75% ethanol solution with the liquid-solid ratio of 8 to perform extraction again, and combining 2 times of filtrates.
2. Experimental methods
1. Analysis and determination of 4 active ingredients in Chinese angelica compound
1) Chromatographic conditions
A chromatographic column: CAPCELL PAK C18 MG II (250 mm. Times.4.6 mm,5 μm); mobile phase: methanol and phosphoric acid aqueous solution (containing 0.2% by volume); gradient program of 25% methanol → 55% methanol is carried out for 0-20 min; at 30 deg.C and 257nm, the mobile phase is 1.0 mL/min -1 A5. Mu.L sample was analyzed under the conditions of (1).
2) Preparation of test solution
Precisely weighing about 1.0g of the angelica compound sample, adding 25mL of methanol solution, carrying out ultrasound for 1h, and filtering to obtain the angelica compound sample.
3) Preparation of Standard solution
Single standard solution: taking appropriate amount of 4 standard substances, and diluting with methanol to constant volume to obtain rutin reference substance solution (0.30 mg. ML) -1 ) Quercetin control solution (0.35 mg. ML) -1 ) Quercetin control solution (0.41 mg/mL) -1 ) Comparison solution of herba Polygoni Avicularis glycoside (0.50 mg. ML) -1 ) And storing at-20 deg.C.
Mixing standard solutions: adding rutin control solution 2mL, quercetin control solution 1mL, herba Polygoni Avicularis control solution 1mL into 10mL volumetric flask, and adding methanol to balance. The mixed reference solution contains rutin 0.060 mg/mL -1 Quercetin 0.070 mg/mL -1 Quercetin 0.041 mg/mL -1 0.050 mg/mL of polygonin -1 。
4) Analysis methodology review
Linear relationship, detection limit and quantitative limit investigation: and (4) taking mixed standard solutions with different concentrations, and calculating a standard curve after sample injection.
Precision in the day: the peak areas of the 6 mixed control solutions were measured to calculate the Relative Standard Deviation (RSD).
Day precision: the mixed reference solution is measured for 3 times at intervals of 24h, the sample injection is continuously carried out for 2 times for each measurement, and the RSD of the peak area is calculated.
And (3) repeatability test: taking 6 parts of the same batch of angelica compound, each part is 1.0g, preparing and injecting samples in parallel, recording peak areas, and respectively calculating the percentage content of 4 active ingredients contained in the sample and an RSD value by using a standard curve method.
And (3) stability test: taking the same sample solution, respectively recording peak areas at 0h, 2h, 4h, 8h, 16h and 24h after preparation, and respectively calculating the percentage content of 4 active ingredients contained in the sample and the RSD value by using a standard curve method.
5) Determination of 4 active ingredients of angelica compound
Precisely weighing 3 parts of the Chinese angelica compound, each part is 1.0g, and carrying out ultrasonic treatment for 1 hour by 25mL of methanol, and filtering to obtain the Chinese angelica compound preparation. Taking 1.5mL of test solution, filtering with a microporous filter membrane (0.45 mu m) to a sample injection bottle (1.5 mL), and analyzing and recording the peak area by sample injection. And calculating the content of each active ingredient in the sample by a standard curve method.
2. In vitro antioxidant test of compound radix Angelicae sinensis extract
1) DPPH radical scavenging ability test
Aluminum nitrate color development method for measuring total flavone content in radix Angelicae sinensis compound extractive solution to 5.76 mg/mL in ultraviolet spectrophotometer -1 . Taking total flavone concentration of 0.74, 0.79, 0.83, 0.88, 0.92 mg/mL -1 The activity of the compound extract of radix Angelicae sinensis, and the preparation and quality of shampoo were studied by calculating the clearance rate (Jiaying, zhao Jing, xiao \29495; qin. Radix Codonopsis) by the method described in the literature [ J]Daily chemical industry, 2021,51 (05): 421-427.).
2) Hydroxy radical scavenging test
Taking total flavone concentration of 0.74, 0.79, 0.83, 0.88, 0.92 mg/mL -1 The activity and shampoo preparation and quality research of radix Angelicae sinensis compound extractive solution (Jiaying, zhao Jing, xiao 29495; qin, radix Codonopsis compound extractive solution) are calculated by literature method]Daily chemical industry, 2021,51 (05): 421-427.)
3) Total antioxidant capacity of FRAP
Taking total flavone concentration of 0.38, 0.47, 0.56, 0.65, 0.74 mg/mL -1 Mixing FRAP working solution 6mL and distilled water 0.6mL in 5 test tubes, reacting in 37 deg.C constant temperature water bath for 10min, measuring absorbance at 593nm, and performing FeSO in laboratory 4 The standard curve of (2) is calculated.
3. Results of the experiment
1. Analysis and determination of 4 active ingredients of angelica compound
1.1 analysis methodology investigation
Linear relationship, detection limit and quantitation limit: the results are shown in Table 1, where the regression equation is shown according to the standard curve with the peak area value of the control as ordinate (Y) and the concentration as abscissa (X). The 4 components have good linear relation. The detection limit LOD (signal-to-noise ratio S/N = 3) and the quantification limit LOQ (signal-to-noise ratio S/N = 10.
TABLE 1 regression equation, correlation coefficient, linear range for determination of active ingredient content
Precision in the day: the results are shown in Table 2, the daily precision RSD range of 4 components is 0.12-0.31%, and the results show that the precision test results of the used instruments meet the requirements.
TABLE 2 precision in day (n = 6)
Precision in the daytime: the results are shown in Table 3, the daytime precision RSD range of 4 components is 1.86-2.85%, and the results show that the precision test results of the used instruments meet the requirements.
TABLE 3 precision between days (n = 6)
And (3) repeatability test: the results are shown in Table 4, the range of the repetitive RSD of 4 components is 1.84-2.93%, and the results show that the repetitive test results of the established test method meet the requirements.
TABLE 4 repeatability test for determination of Multi-active ingredient content
And (3) stability test: the results are shown in Table 5, where the RSD range for the stability of the 4 components is 1.70-2.88%, indicating that the stability of the samples tested is good.
TABLE 5 stability study of the determination of the content of the multiple active ingredients
1.2 determination of active ingredients of Compound 4 of Dang Gui
The content of each active ingredient in the sample was calculated by the standard curve method, and the results are shown in table 6. The content of 4 active ingredients in the radix Angelicae sinensis compound is rutin 372.1649 μ g/g -1 Quercetin 953.1612 microgram g -1 Polygonum aviculare glycoside 160.8286 mug. Multidot.g -1 Quercetin 631.6464 mug. Multidot.g -1 。
TABLE 6 determination result of content of 4 active ingredients in the Chinese angelica compound preparation
2. In vitro antioxidant test of compound radix Angelicae sinensis extract
2.1 DPPH radical scavenging ability test
The result of removing DPPH free radical by the compound Dang Gui is shown in Table 7.
TABLE 7 DPPH radical scavenging Rate
2.2 hydroxy radical scavenging ability test
The hydroxyl radical scavenging effect of Dang Gui Fufang is shown in Table 8.
TABLE 8 hydroxyl radical scavenging Rate
2.3 Total antioxidant capacity of FRAP
According to the existing FeSO 4 The standard curve of (A) is Y =0.5821X +0.005, and the total antioxidant capacity result of the angelica compound FRAP is shown in a table 9.
TABLE 9 FRAP antioxidant capacity
The results of the three antioxidant tests show that the antioxidant capacity of the angelica compound extract is enhanced along with the increase of the content of the total flavone within a certain concentration range.
Example 2 preparation and Performance measurement of Angelica sinensis Compound shampoo
1. Preparation of angelica compound shampoo
The angelica compound extract prepared in example 1 is concentrated into an extract, then is re-dissolved with deionized water in equal amount, and is added into the formula as an active ingredient. Putting a surfactant into a beaker, stirring and heating to 70 ℃ in a water bath kettle, adding components such as a cation conditioner, a humectant, a chelating agent and the like, cooling to 40 ℃, adding a preservative, completely and uniformly mixing, adding a NaCl saturated solution for thickening, and finally adding deionized water for complementing weight.
2. Experimental method
2.1 sensory evaluation of Angelica Compound shampoo
The prepared shampoo is subjected to sensory evaluation by taking appearance, experience feeling of use and the like as indexes, and the detection result is determined by the mean value of the scores jointly scored by 10 persons of an evaluation team. Because the angelica compound recipe aims at oily hair and more dandruff hair clinically, the oil stain removing capability score is higher, and the sensory score is shown in a table 10. In addition, the heat resistance and the cold resistance are tested, wherein 40 points are added for no layering, and 0 point is added for layering.
TABLE 10 sensory evaluation chart
2.2 screening of anionic surfactants
The total amount of the surfactant is 30 percent, the total amount of other components in the formula is 70 percent, and the total weight of the surfactant, namely lauroyl sarcosine LS-30: the mass ratio of ammonium laureth sulfate ALES 1 to 5; and comprehensively scoring the blank formula with the surfactant amount of 10-30% to determine the total amount of the surfactant.
2.3 screening of cationic Conditioning Agents
The total amount of the surfactant is 30 percent, the total amount of the cationic conditioner is 0.9 percent, and the weight ratio of guar gum: quaternary ammonium salt-10 mass ratio =1, 0, 1, 2; and comprehensively scoring a blank formula with the total amount of the cationic conditioner of 0.5-0.9% to determine the total amount of the cationic conditioner.
2.4 evaluation of Angelica Compound shampoo
And adding the angelica compound extracting solution into the optimized blank formula of the shampoo to prepare the angelica compound shampoo, and detecting the appearance, smell, pH and total solid according to the national standard GB/T29679-20133 shampoo and cream shampoo, and detecting the foam performance.
2.5 bacteriostatic test of Compound radix Angelicae sinensis shampoo
Activating the freeze-stored malassezia strain, diluting the strain to 4.0 × 10 5 CFU/mL. Diluting each well of the bacterial solution by 100 μ L, adding dropwise into 96-well plate, adding 100 μ L of shampoo solution with different concentrations, and setting up positive control group (250 μ g. ML) -1 Ketoconazole solution) and blank control. The bacterial liquid of the sample group was replaced with the same volume of culture medium as a negative control group. Putting the 96-well plate into a bacterial incubator for incubation for 48h, taking out, and detecting OD of each well by using an enzyme-labeling instrument 530mm Determining the bacteria content, OD, in each well system according to the absorbance 530mm The lower the value, the more obvious the bacteriostatic effect.
3. Results of the experiment
3.1 preparation of Angelica sinensis Compound shampoo
3.1.1 screening of anionic surfactants
1) Ratio of primary surfactant
The total amount of the surfactant is 30%, the total amount of other components in the formula is 70%, and the total weight of the surfactant LS: ALES mass ratio 1. The results are shown in Table 11, formula 1, primary surfactant lauroylsarcosine LS-30: the ammonium laureth sulfate ALES has the highest mass ratio = 1.
TABLE 11 anionic surfactant ratio
2) Total amount of primary surfactant
Determination of the primary surfactant lauroylsarcosine LS-30: the mass ratio of laureth ammonium sulfate ALES =1, and the screening total amount: 10%, 15%, 20%, 25%, 30%, the results are shown in table 12, with the highest score for formula 9 with a total surfactant of 30%.
TABLE 12 Total amount of surfactant
3.1.2 screening of cationic Conditioning Agents
1) Cationic conditioner ratio
The total amount of the cationic conditioner is 0.9%, and the cationic conditioner proportion is screened, wherein the weight ratio of guar gum: quaternary ammonium salt-10 mass ratio =1, 0, 1, 2. The results are shown in table 13, with formula 9 having the highest overall score for cationic conditioner ratio 1.
TABLE 13 cationic conditioner ratio
2) Total amount of cationic conditioner
Determining a mass ratio of guar gum to quaternary ammonium salt-10 =1, and screening the total amount of the cationic conditioner: 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, the results are shown in table 14, and the highest overall score was obtained when the total amount of cationic conditioning agent of formula 15 was 0.6%.
TABLE 14 Total amount of cationic conditioning agent
3.1.3 preparation of shampoos
Concentrating the radix Angelicae sinensis compound extractive solution, re-dissolving with deionized water, and adding 10% of the extract into the formula as active ingredient. Putting the A-phase surfactant in a beaker, stirring and heating to 70 ℃ in a water bath kettle, adding the B-phase other components, cooling to 40 ℃, adding the C-phase preservative, completely and uniformly mixing, adding a NaCl saturated solution for thickening, and finally adding deionized water for supplementing the weight. The formulation is shown in Table 15, taking 100g as an example.
Formula of compound shampoo containing angelica sinensis in table 15
3.2 evaluation of Angelica Compound shampoo
The appearance, smell, pH, stability and total solid were tested according to the national standard GB/T29679-20133 shampoo and cream shampoo, and the foam properties were tested, the results are shown in Table 16.
TABLE 16 measurement results of Compound shampoo of Angelica sinensis
3.3 bacteriostatic test of Compound shampoo containing radix Angelicae sinensis
When the volume concentration of the angelica compound shampoo is 0.1-25.0% (diluted volume concentration), the angelica compound shampoo has obvious inhibition effect on malassezia, and the inhibition rate is about 21.7-85.0%. The results of the bacteriostatic action are shown in FIG. 1.
Example 3 inhibitory Effect of Angelica sinensis Compound shampoo on Staphylococcus aureus
1. Inhibition effect of angelica sinensis compound shampoo on staphylococcus aureus
And (3) taking the activated staphylococcus aureus strains, and determining the inhibitory action of the angelica sinensis compound shampoo on staphylococcus aureus by adopting a bacteriostatic ring method.
2. Experimental methods
2.1 preparation of nutrient agar Medium (Staphylococcus aureus)
Weighing 10.0g of peptone, 5.0g of beef extract and 5.0g of sodium chloride, adding 1000mL of distilled water for dissolving, adjusting the pH value to 7.2-7.4, then adding 15.0g of agar, heating for dissolving (boiling state), subpackaging, and sterilizing for 20min at 121 ℃ by steam for later use. The liquid medium contained no agar.
2.2 preparation of the bacterial suspension
Taking staphylococcus aureus activated by a slant, selecting 1-3 rings by using an inoculating ring, inoculating into a sterilized triangular flask filled with 25mL of liquid culture medium, slightly stirring uniformly, and placing in a shaking table for culturing for 24h,37 ℃ and 150r/min. Controlling the concentration of the bacterial liquid to 10 5 ～10 6 And C, after CFU/mL, the solution is ready for use.
2.3 measurement of bacterial liquid concentration
Taking 1mL liquid containing bacteria liquid to culture in a test tube containing 9mL physiological saline, blowing and sucking for 3 times, and mixing the bacteria liquid uniformly to obtain 10 -1 And (4) diluting the solution. Then the pipette is used for sucking 10 -1 Diluting with 1mL of the diluted solution, transferring into a test tube containing 9mL of physiological saline, blowing and sucking for 3 times, and mixing the bacteria solution uniformly to obtain 10 -2 And (4) diluting the solution. By analogy, continuously diluting to obtain 10 -1 、10 -2 、10 -3 、10 -4 、10 -5 、10 -6 、10 -7 And a series of diluted bacterial liquids.
Smearing plate counting method: sterile flat plate is knitted 10 -5 、10 -6 、10 -7 The number of each number is set to be three times, the bacterial culture medium which is melted and cooled to 45-50 ℃ is poured into 9 sterile plates, the plates are slightly rotated, and 10 bacteria are absorbed by a pipette according to the requirement of sterile operation -5 300. Mu.L of each dilution was put in number 10 -5 The 3 plates are lightly coated by a coater to ensure that the bacterial liquid permeates into the culture medium, then the plates are inverted and cultured for 24 hours at 37 ℃, and the count can be carried out after the bacterial growth.
From this, it can be calculated that the concentration of the test tube 2 is 10 5 ～10 6 CFU/mL range.
2.4 preparation of bacteriostatic tablets
Preparing bacteriostatic experiment products (volume concentration is 0.8, 0.4 and 0.1) with different volume concentrations, taking sterile dry filter paper sheets, dropwise adding 20 mu L of bacteriostatic experiment sample solution with a certain concentration into each filter paper sheet, taking dropwise adding 20 mu L of sterile water as a blank, then flatly placing the filter paper sheets in a clean sterile plate, opening a cover and drying in a thermostat for later use.
2.5 inoculation of test bacteria
Pouring the sterilized solid culture medium into a culture dish, solidifying to a thickness of about 2/3 of the culture dish, sucking 300 mu L of the bacterial suspension in the test tube 2 by using a pipette under an aseptic condition, and uniformly smearing the bacterial suspension on the surface of a nutrient agar culture medium flat plate for 3 times. After each application for 1 time, the plate should be rotated 60 °, and finally the plate is applied with an applicator around the edge of the plate for a circle, covered with a plate, and left to dry at room temperature for 5min.
2.6 sticking antibacterial experimental samples
Each test is stuck with a bacteria-infected plate, and each plate is stuck with 3 test sample sheets and 1 reference sample sheet for 4 sheets in total. And (3) using sterile forceps to sample the slices and attaching the slices to the surface of the flat plate, wherein the distance between the centers of the slices is more than 25mm, and the distance between the centers of the slices is more than 15 mm. After the sample is placed, the sample is lightly pressed by using sterile tweezers to be tightly attached to the surface of the flat plate. The plate is covered, and the plate is placed in a constant temperature box at 37 ℃, and the result is observed after the plate is cultured for 16 to 18 hours. The diameter of the zone (including the patch) was measured with a ruler and recorded. The experiment was repeated 3 times.
When the inhibition zone is measured, the inhibition zone which is uniform and completely aseptically grows is selected for measurement. The diameter of the catheter is measured by taking the outer edge of the bacteriostatic ring as a boundary.
3. Results of the experiment
The experimental result is shown in table 17, the shampoo has a significant inhibitory effect on staphylococcus aureus, and the bacteriostatic effect is stronger along with the increase of volume concentration, and the bacteriostatic effect graph is shown in fig. 2.
TABLE 17 diameter of zone of inhibition for shampoos of different volume concentrations
Note: the size of the filter paper used in the experiment was 7.0mm, compared to the blank ** P<0.01。
4. Conclusion
1) The content of active ingredients in the angelica compound 4 is respectively determined to be rutin 372.1649 mug.g by adopting a high performance liquid chromatography -1 Quercetin 953.1612 microgram g -1 Herba Polygoni Avicularis 160.8286 μ g/g -1 Quercetin 631.6464 mug. Multidot.g -1 ；
2) A series of in vitro antioxidant test results show that the antioxidant capacity of the Chinese angelica compound is enhanced along with the increase of the content of the total flavone within a certain concentration range;
3) The preferable preparation conditions of the angelica compound shampoo are as follows: surfactant a phase total 30% (11.24% lauroylsarcosine LS-30, 11.24% ammonium laureth sulfate ALES, 4.02% cocamidopropyl betaine CAB-35, 1.00% alkyl glycoside APG1214, 2.50% cocamidomethyl MEA); other component B phase, 10.00% angelica compound extract, 5.00% glycerin, 0.10% disodium edetate EDTA-2Na,0.60% cation conditioner (guar gum: quaternary ammonium salt-10 = 1; the cason is phase C.
4) The liquid-based dilution method is used for determining the malassezia inhibition effect of the angelica sinensis compound shampoo, and the result shows that the angelica sinensis compound shampoo has a remarkable inhibition effect on the malassezia when the volume concentration is 0.1-25.0%, and the inhibition rate is about 21.7-85.0%;
5) The angelica compound shampoo is detected according to the physical and chemical indexes of the national standard, is light brown, has the traditional Chinese medicine flavor, has the pH value of 6.17, good cold resistance and heat resistance, has the foam thickness of 136mm, and has the total solid content of 20.41 percent.
6) The angelica compound shampoo can reduce scalp grease secretion and inhibit dandruff generation, and is a product with safe components, strong oxidation resistance, good stability and strong bacteriostatic action.
Claims (10)
1. A compound angelica sinensis extract is prepared from the following components in parts by mass:
15-30 g of angelica, 30-45 g of astragalus, 15-30 g of mulberry leaf, 12-30 g of cacumen biotae, 10-20 g of wild chrysanthemum, 12-36 g of codonopsis pilosula, 9-30 g of mint and 6-24 g of rhizoma cyperi.
2. The preparation method of the angelica sinensis compound extract as claimed in claim 1, comprising the following steps:
mixing and crushing the angelica, the astragalus, the mulberry leaves, the cacumen biotae, the wild chrysanthemum flowers, the codonopsis pilosula, the mint and the rhizoma cyperi, then extracting for 2-3 times by adopting a solvent to obtain an extracting solution, and concentrating the extracting solution to obtain the Chinese herbal medicine;
the solvent is water, ethanol water solution, petroleum ether solution or ethyl acetate solution, and the volume fraction of the ethanol water solution, the petroleum ether solution or the ethyl acetate solution is 0-100%;
the extraction method comprises the following steps: reflux extraction, distillation extraction, decoction, percolation or extraction.
3. A radix Angelicae sinensis compound shampoo is prepared from radix Angelicae sinensis compound extract of claim 1, surfactant, cation conditioner, humectant, chelating agent, thickener, solvent and antiseptic;
the angelica sinensis compound shampoo comprises the following components in parts by mass:
0-100% of angelica compound extract, 0-100% of surfactant, 0-5% of cation conditioner, 0-100% of humectant, 0-1% of chelating agent, 0-20% of thickener, 0-100% of solvent and 0-1% of preservative, but all are not zero.
4. The angelica sinensis compound shampoo according to claim 3, characterized in that: the surfactant is at least one of an anionic surfactant, a zwitterionic surfactant and a nonionic surfactant;
the anionic surfactant is amino acid surfactant or sulfate surfactant.
5. The angelica sinensis compound shampoo according to claim 4, characterized in that: the anionic surfactants include, but are not limited to: lauroyl sarcosine LS-30, ammonium laureth sulfate ALES;
the zwitterionic surfactants include, but are not limited to: cocamidopropyl betaine CAB-35;
the nonionic surfactants include, but are not limited to: alkyl glycoside APG1214, cocamide methyl MEA.
6. The angelica sinensis compound shampoo according to any one of claims 3-5, wherein: the cationic conditioning agents include, but are not limited to: guar gum, polyquaternary ammonium salt compounds;
in the cationic conditioner, the mass ratio of the guar gum to the polyquaternium compound is (0).
7. The angelica sinensis compound shampoo according to any one of claims 3-6, characterized in that: such humectants include, but are not limited to: propylene glycol, glycerin;
such chelating agents include, but are not limited to: disodium ethylene diamine tetraacetate and tetrasodium ethylene diamine tetraacetate.
8. The angelica sinensis compound shampoo according to any one of claims 3-7, characterized in that: such thickeners include, but are not limited to: cocamide methyl MEA, sodium chloride NaCl.
9. The angelica sinensis compound shampoo according to any one of claims 3-8, characterized in that: such solvents include, but are not limited to: deionized water, double distilled water, propylene glycol, glycerol, pentanediol and hexanediol.
10. The angelica sinensis compound shampoo according to any one of claims 3-9, characterized in that: the preservative is a chemical preservative or a natural preservative, including but not limited to: parabens, cason, and p-hydroxyacetophenone.
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| US5925615A (en) * | 1998-03-06 | 1999-07-20 | Nu Skin International, Inc. | Awapuhi (Zingiber zerumbet) -containing hair cleansing and conditioning compositions |
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| CN103566066A (en) * | 2013-11-27 | 2014-02-12 | 高飞 | Medicine for treating seborrheic dermatitis and preparation method of medicine |
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