CN111803542A - Hair growth traditional Chinese medicine composition and preparation method and application thereof - Google Patents
Hair growth traditional Chinese medicine composition and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a hair growth traditional Chinese medicine composition and a preparation method and application thereof, wherein the traditional Chinese medicine composition is prepared from the following raw materials in parts by weight: 10-60 parts of gallnut, 20-60 parts of polygonum multiflorum, 20-45 parts of gleditsia sinensis, 20-65 parts of snakehead intestine, 20-50 parts of glossy privet fruit, 10-30 parts of ligusticum wallichii and 10-45 parts of isatis indigotica, wherein the traditional Chinese medicine composition comprises the following effective components: tannin compounds, anthraquinone compounds, flavonoid compounds, terpenoid compounds, tetracyclic triterpenoid compounds, saponin compounds, volatile oil and alkaloids. Has effects of promoting hair follicle growth and inhibiting bacteria, and can be used for preventing and treating premature gray hair, alopecia areata, seborrheic alopecia, etc., and alopecia. In the production process, different extraction methods are adopted for matching use, so that the conversion rate of effective substances in the formula can be effectively improved, the process cost can be controlled, and the method is suitable for application in large-scale production of medicines or washing and caring products.
Description
Technical Field
The invention relates to a hair growth traditional Chinese medicine composition, a preparation method and application thereof, in particular to a traditional Chinese medicine composition capable of activating scalp hair follicles and growing hair, a preparation method and application thereof, and belongs to the field of traditional Chinese medicine preparations.
Background
Alopecia is one of the clinically common skin diseases, usually manifested as abnormal or excessive hair loss, such as seborrheic alopecia, alopecia areata, etc., and the common causes include endocrine dyscrasia, mental trauma, vascular dysfunction and hereditary factors. The hair loss treatment by the traditional Chinese medicine has a long history, according to the theory of the traditional Chinese medicine, the hair has close relation with liver and kidney, the kidney stores essence and liver which dominate blood and blooms in the hair, the deficiency of liver and kidney causes insufficiency of essence and blood, and hair follicles can not obtain sufficient nutrition, and one condition is that the capacity of synthesizing melanin is weakened and white hair appears; another condition is atrophy or necrosis of the hair follicle, resulting in hair loss. Otherwise, the liver and kidney are strong and the upper part is good at the head, so the hair is thick and dark. Meanwhile, the existing research also shows that the promotion of hair follicle growth is the key of hair loss prevention and hair growth.
For example: in the prior patent document CN102973727A (a hair follicle activating solution and a preparation method thereof, 2013.03.20), a hair follicle activating solution prepared from red ginseng, angelica sinensis, cacumen biotae, ligusticum wallichii, astragalus membranaceus, safflower carthamus, rheum officinale, saponin, radix rehmanniae, liquorice, black sesame, garden balsam stem, radix polygoni multiflori preparata, mulberry, felwort, chrysanthemum and wolfberry fruit is disclosed, and a comparison test shows that the hair follicle activating solution can improve the hair follicle activation rate by more than 70%, and after a small-scale trial, the hair follicle activating solution has a good hair growth effect.
And the traditional Chinese medicine hair growth solution disclosed in the prior patent document CN103768275A (a traditional Chinese medicine hair growth solution for treating seborrheic alopecia, 2014.05.07) prepared from myrrh, oriental blueberry leaf, folium artemisiae argyi, sweet wormwood, bunge corydalis herb, polygonum multiflorum, rhizoma cibotii, fructus psoraleae, rhizoma drynariae, prepared rhizome of rehmannia, cherokee rose fruit and astragalus membranaceus is sprayed on the surface of alopecia to achieve the effects of eliminating dampness and insects, killing viruses, killing molds, resisting fungi and inflammation, enriching blood and nourishing yin, replenishing essence and benefiting marrow, tonifying kidney, dissipating blood and removing stasis, relieving swelling and promoting granulation and promoting blood circulation, so that chronic inflammation of hair follicles and scalp is eliminated, lipophilicity fungi and head mites are killed, pollutants in the hair follicles are removed, excessive secretion of androgens is inhibited, growth of the hair follicles is activated, and the hairs can be regenerated after two to four months of medication.
And a traditional Chinese medicine composition disclosed in the prior patent document CN110755592A (2020.02.07) and prepared from cacumen biotae, saponin, polygonum multiflorum, cortex mori radicis, rhizoma zingiberis, black sesame, salvia miltiorrhiza, angelica sinensis, medlar, semen cuscutae, radix achyranthis bidentatae, poria cocos, fructus psoraleae and rhizoma zingiberis, the traditional Chinese medicine composition can stimulate scalp, accelerate blood circulation of head, activate atrophic hair follicles and reconstruct a nutrition supply system of hair follicles by externally coating hair loss and white hair parts, and the supply system has obvious curative effects on various hair loss and white hair.
We find that the existing traditional Chinese medicine compositions disclose that the hair follicle activation has obvious treatment effect on hair growth, but effective substances for activating hair follicle growth are not found fundamentally, so that the problem of hair follicle growth is solved to a certain extent, but the traditional Chinese medicine compositions are often large in medicine flavor quantity and not beneficial to control of process cost.
Disclosure of Invention
The invention aims to provide a hair growth traditional Chinese medicine composition, which can achieve the effects of promoting hair follicle growth and inhibiting bacteria by adopting reasonable compatibility and use of seven medicines, and can be used for preventing and treating premature graying of hair, alopecia areata, seborrheic alopecia and the like and treating alopecia besides achieving the hair growth effect.
The invention also aims to provide a preparation method of the hair growth traditional Chinese medicine composition, which adopts the matching use of different extraction methods, can effectively improve the conversion rate of effective substances in the formula, can effectively control the process cost, and is suitable for the application in the large-scale production of preparing medicines or washing products.
The invention is realized by the following technical scheme: a hair growth traditional Chinese medicine composition is composed of the following raw materials in parts by weight: 10-60 parts of gallnut, 20-60 parts of polygonum multiflorum, 20-45 parts of gleditsia sinensis, 20-65 parts of snakehead intestine, 20-50 parts of glossy privet fruit, 10-30 parts of ligusticum wallichii and 10-45 parts of isatis indigotica, wherein the traditional Chinese medicine composition comprises the following effective components: tannin compounds are more than or equal to 85.86mg/g, anthraquinone compounds are more than or equal to 0.29mg/g, flavonoid compounds are more than or equal to 97.58mg/g, terpenoid compounds are more than or equal to 1.69mg/g, tetracyclic triterpenoid compounds are more than or equal to 0.95mg/g, saponin compounds are more than or equal to 53.20mg/g, volatile oil is more than or equal to 28.36mg/g, and alkaloid is more than or equal to 40.30 mg/g.
In the traditional Chinese medicine composition, the tannin compound is 85.86-119.27 mg/g, the anthraquinone compound is 0.29-0.85 mg/g, the flavonoid compound is 97.58-116.86 mg/g, the terpenoid compound is 1.69-5.61 mg/g, the tetracyclic triterpenoid compound is 0.95-3.06 mg/g, the saponin compound is 53.20-78.90 mg/g, the volatile oil is 28.36-44.21 mg/g, and the alkaloid is 40.30-64.57 mg/g.
The invention also provides a preparation method of the hair growth traditional Chinese medicine composition, which comprises the following steps according to the parts by weight of the raw materials in the claim 1:
(1) preparing spray-dried powder of a gallnut extract, spray-dried powder of a polygonum multiflorum extract and spray-dried powder of a snakehead intestine extract by respectively taking gallnut, polygonum multiflorum and snakehead intestine as raw materials for later use;
(2) preparing spray-dried powder of a mixed extract of glossy privet fruit and ligusticum wallichii by taking glossy privet fruit and ligusticum wallichii as raw materials for later use;
(3) preparing spray-dried powder of mixed extract of Gleditsia sinensis and Isatis tinctoria from Gleditsia sinensis and Isatis tinctoria;
(4) mixing the spray-dried powder prepared in the steps (1) to (3) and carrying out superfine grinding to prepare the traditional Chinese medicine composition,
the traditional Chinese medicine composition comprises the following effective components: tannin compounds are more than or equal to 85.86mg/g, anthraquinone compounds are more than or equal to 0.29mg/g, flavonoid compounds are more than or equal to 97.58mg/g, terpenoid compounds are more than or equal to 1.69mg/g, tetracyclic triterpenoid compounds are more than or equal to 0.95mg/g, saponin compounds are more than or equal to 53.20mg/g, volatile oil is more than or equal to 28.36mg/g, and alkaloid is more than or equal to 40.30 mg/g.
In the step (1), the step of preparing spray-dried powder of the gallnut extract comprises:
(1.1 a) taking gallnut as a raw material, carrying out superfine grinding, then using 70% ethanol as an extraction solvent, carrying out reflux extraction for 40min in a dynamic continuous circulating extraction device, then starting circulating extraction, wherein the extraction temperature is 78-82 ℃, extracting for 3h, and then collecting an extracting solution;
(1.2 a) mixing the extracting solution obtained in the step (1.1 a) with water at 90 ℃, concentrating, recovering alcohol during concentration, and when the alcohol concentration is lower than 45%, not recovering, and then concentrating under reduced pressure at 55-65 ℃ to obtain a clear paste crude extract with the relative density of 1.05-1.10;
(1.3 a) feeding the clear paste crude extract obtained in the step (1.2 a) into a high-speed countercurrent extraction device, controlling the flow rate to be 1.2-1.6 mL/min, the rotation speed to be 795-805 r/min, the temperature of an extraction column to be 25-27 ℃, and using an ethyl acetate-n-butyl alcohol-water solvent system (5: 1.8: 6), standing, phase-splitting and ultrasonic degassing for 30min, then using an upper phase as a stationary phase and a lower phase as a mobile phase, separating extract extractum, and collecting an extract;
(1.4 a) carrying out reduced pressure concentration on the extract obtained in the step (1.3 a) at the temperature of 60-70 ℃ to obtain clear paste with the density of 1.01-1.05, and carrying out spray drying on the clear paste at the air inlet temperature of 178-182 ℃ and the air outlet temperature of 83-87 ℃ to obtain spray-dried powder of the gallnut extract.
In the step (1), the step of preparing the spray-dried powder of the polygonum multiflorum extract comprises:
(1.1 b) taking polygonum multiflorum as a raw material, carrying out superfine grinding, then using 70% ethanol as an extraction solvent, carrying out reflux extraction for 45min in a dynamic continuous circulating extraction device, then starting circulating extraction, wherein the extraction temperature is 78-82 ℃, extracting for 3h, and then collecting an extracting solution;
(1.2 b) mixing the extracting solution obtained in the step (1.1 b) with water at 90 ℃, concentrating, recovering alcohol during concentration, and when the alcohol concentration is lower than 45%, not recovering, and then concentrating under reduced pressure at 55-65 ℃ to obtain a clear paste crude extract with the relative density of 1.05-1.10;
(1.3 b) feeding the clear paste crude extract obtained in the step (1.2 b) into a high-speed countercurrent extraction device, controlling the flow rate to be 1.2-1.6 mL/min, the rotation speed to be 725-735 r/min, the temperature of an extraction column to be 25-27 ℃, and using a solvent system of n-hexane-ethyl acetate-methanol-water (9: 1: 5: 5), standing for phase separation, ultrasonically degassing for 30min, using an upper phase as a stationary phase and a lower phase as a mobile phase, separating extract, and collecting an extract;
(1.4 b) carrying out reduced pressure concentration on the extract obtained in the step (1.3 b) at the temperature of 60-70 ℃ to obtain clear paste with the density of 1.01-1.05, and carrying out spray drying on the clear paste at the air inlet temperature of 178-182 ℃ and the air outlet temperature of 83-87 ℃ to obtain spray-dried powder of the polygonum multiflorum extract.
In the step (1), the step of preparing the spray-dried powder of the snakehead gut extract comprises the following steps:
(1.1 c) taking snakehead gut as a raw material, carrying out superfine grinding, then using 70% ethanol as an extraction solvent, carrying out reflux extraction for 40min in a dynamic continuous circulating extraction device, then starting circulating extraction, wherein the extraction temperature is 68-72 ℃, extracting for 3h, and then collecting an extracting solution;
(1.2 c) mixing the extracting solution obtained in the step (1.1 c) with water at 90 ℃, concentrating, recovering alcohol during concentration, and when the alcohol concentration is lower than 45%, not recovering, and then concentrating under reduced pressure at 55-65 ℃ to obtain a clear paste crude extract with the relative density of 1.05-1.10;
(1.3 c) feeding the clear paste crude extract obtained in the step (1.2 c) into a high-speed countercurrent extraction device, controlling the flow rate to be 1.2-1.6 mL/min, the rotating speed to be 795-805 r/min, the temperature of an extraction column to be 25-27 ℃, and using a solvent system of n-hexane-ethyl acetate-methanol-water (1: 0.6: 0.6: 1), standing, carrying out phase separation and ultrasonic degassing for 30min, using an upper phase as a stationary phase and a lower phase as a mobile phase, separating extract, and collecting extract liquor;
(1.4 c) carrying out reduced pressure concentration on the extract obtained in the step (1.3 c) at the temperature of 60-70 ℃ to obtain clear paste with the density of 1.01-1.05, and carrying out spray drying on the clear paste at the air inlet temperature of 178-182 ℃ and the air outlet temperature of 83-87 ℃ to obtain spray-dried powder of the snakehead gut extract.
In the step (2), the step of preparing the spray-dried powder of the mixed extract of glossy privet fruit and ligusticum wallichii comprises the following steps:
(2.1) mixing the glossy privet fruit and the ligusticum wallichii as raw materials, carrying out superfine grinding, then using 50% ethanol as an extraction solvent, carrying out reflux extraction for 40min in a dynamic continuous circulation extraction device, then starting circulation extraction, wherein the extraction temperature is 68-72 ℃, extracting for 3h, and then collecting an extracting solution;
(2.2) mixing the extracting solution obtained in the step (2.1) with water at the temperature of 90 ℃, and then concentrating under reduced pressure at the temperature of 55-65 ℃ to obtain a clear paste crude extract with the relative density of 1.01-1.05;
and (2.3) carrying out spray drying on the clear paste crude extract obtained in the step (2.2) under the conditions of air inlet temperature of 178-182 ℃ and air outlet temperature of 83-87 ℃ to obtain spray dried powder of the mixed extract of the glossy privet fruit and the ligusticum wallichii.
In the step (3), the step of preparing a spray-dried powder of a mixed extract of the gleditsia sinensis lam and the isatis tinctoria includes:
(3.1) mixing the gleditsia sinensis and the isatis indigotica as raw materials, crushing, adding water, decocting for 2 times, adding 9-10 times of water into the decoction, soaking for 55-65 min, boiling, keeping slightly boiling for 60min, and filtering; adding 8-9 times of water into the second decoction, starting timing when circularly heating to 94 ℃, decocting for 60min, controlling the temperature at 94-102 ℃, filtering, and combining the two filtrates;
(3.2) mixing the combined filtrate obtained in the step (3.1) with water at 90 ℃, and then concentrating under reduced pressure at 55-65 ℃ to obtain a clear paste crude extract with the relative density of 1.01-1.05;
and (3.3) carrying out spray drying on the clear paste crude extract obtained in the step (3.2) at the air inlet temperature of 178-182 ℃ and the air outlet temperature of 83-87 ℃ to obtain spray dried powder of the mixed extract of the gleditsia sinensis lam and the isatis tinctoria.
In the step (4), the spray-dried powder prepared in the steps (1) to (3) is mixed and subjected to superfine grinding, and then the mixture is fed into a total mixer, and the traditional Chinese medicine composition is prepared after uniform mixing at the feeding speed of 20 min/time, 5kg of material for each feeding and the temperature of less than 16 ℃.
The invention also provides application of the hair growth traditional Chinese medicine composition in preparation of medicines or washing and caring products, for example, the hair growth traditional Chinese medicine composition can be used for preparing external preparations such as ointment, spray, essence, gel, liniment and shampoo.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the Chinese gall-black tea is prepared from seven Chinese medicinal herbs including Chinese gall, tuber fleeceflower root, honey locust, snakehead intestine, glossy privet fruit, ligusticum wallichii and isatis indigotica fort through reasonable compatibility, has the effects of nourishing kidney and liver, improving eyesight and blackening hair, detoxifying and eliminating dampness, inhibiting bacteria and diminishing inflammation, and comprehensively conditioning, has the effects of treating alopecia and growing hair, and can be used for preventing and treating early-white hair blacking, alopecia areata, seborrheic alopecia and the like.
(2) The invention firstly limits the selection and content of the effective components in the traditional Chinese medicine formula, finds a traditional Chinese medicine formula capable of effectively promoting hair follicle growth and inhibiting bacteria, does not adopt the treatment effect which is achieved by the superposition of single drug effects of more than ten traditional Chinese medicines after compatibility in the prior art, but is verified by repeated experiments, selects a specific traditional Chinese medicine formula, reasonably exerts the effective components under the compatibility, can achieve the anti-hair loss and hair growth effects of treatment only by seven traditional Chinese medicines, and has obvious treatment effect through clinical verification.
(3) In order to improve the extraction efficiency of the effective components and achieve the treatment purpose, the invention respectively adopts the process means of continuous reflux extraction, high-speed countercurrent extraction, reflux extraction, decoction extraction and the like according to the difference of the effective components and the contents thereof in the traditional Chinese medicine formula, and makes contributions to the promotion of the conversion of the effective components and the purpose of treating alopecia and growing hair.
In conclusion, the invention finds the traditional Chinese medicine formula under a specific compatibility proportion based on the traditional Chinese medicine formula, can obtain the combination and the proportion of specific effective components through a specific extraction method, and has the functions of promoting the growth of hair follicles and inhibiting bacteria under the coordination and the use of the effective components, thereby achieving the purposes of preventing alopecia and growing hair.
Detailed Description
The objects, technical solutions and advantageous effects of the present invention will be described in further detail below.
It is to be noted that the following detailed description is exemplary and is intended to provide further explanation of the invention claimed, and unless otherwise specified, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs, and all percentages herein are by mass concentration.
It has been found that normal development and periodic regeneration of hair follicles is dependent on the interaction between epithelial and mesenchymal cells. It is currently believed that, although signaling between the two major cell types is reciprocal, dermal cells are the inducers of epithelial cell responses, and the activity of dermal papilla cells of hair follicles is a key factor in inducing and maintaining the growth state of hair follicles. Therefore, it is desired to find effective substances in the traditional Chinese medicinal materials which can promote the activity of dermal papilla cells of hair follicles. Different from the existing research, the existing research usually uses a single Chinese medicinal component as a research object, for example, Shiyajing, foreign medicine-botanical drug Manual, 1991, volume 6, No. 1, mentioned that an anthraquinone derivative-containing extract obtained from tuber root of Polygonum multiflorum has the effects of nourishing and strengthening, promoting hair growth, and blackening white hair. However, in practice, the extract containing anthraquinone derivatives extracted from the tuber of polygonum multiflorum is only used for the treatment of hair growth and white hair, and the curative effect is not obvious. Therefore, the invention needs to adopt a plurality of herbs for compatibility, and through the compatibility and use of each herb, on one hand, the transformation of the effective components of the herbs can be promoted, and on the other hand, the purpose of promoting the activity of hair follicle dermal papilla cells can be achieved through the reasonable matching of a plurality of effective components, which is also needed to be solved: how to better promote the activity of dermal papilla cells of hair follicles by a traditional Chinese medicine formula with reasonable compatibility to achieve the treatment purpose of preventing alopecia and growing hair.
The invention uses Chinese gall, tuber fleeceflower root, honey locust, snakehead intestine, glossy privet fruit, Szechuan lovage rhizome and isatis root as raw materials for compatibility and use, wherein,
an anthraquinone derivative-containing extract is obtained from tuber fleeceflower root tuber, and has tonic, hair growth promoting, and white hair blackening effects.
The gallnut is rich in tannin, so that the gallnut has remarkable effects of astringing dampness and healing sore. The tannin in Galla chinensis has precipitation effect on protein, and can coagulate protein in local tissues such as skin and mucosa, to relieve itching.
Flavonoid compound in the jejunum has hydroxyl free radical (OH)-) And superoxide anion radical (O)2 -) All have good cleaning capability, wherein the anemonin total flavone can effectively remove OH-、O2 -Has obvious inhibiting effect on the peroxidation damage of lecithin lipid, can protect scalp cells and hair papilla cells and maintain the scalp environment healthy.
The terpenoid is a component with high content in glossy privet fruit and concentrated pharmacodynamic activity research, wherein oleanolic acid has obvious growth promotion effect on hair follicles, and research shows that oleanolic acid can delay apoptosis of hair follicle cells, particularly hair papilla cells, and can delay hair loss.
The volatile oil of rhizoma Ligustici Chuanxiong mainly contains ligustilide myrcene, sabinene and other alkenes and fatty acid esters, and has effects of improving blood vessel microcirculation, lowering blood pressure, and increasing cerebral blood flow. The nitrogenous compound in the ligusticum wallichii is mainly an alkaloid compound, wherein the ligustrazine has certain pharmacological action on a blood system and a cardiovascular system, and can inhibit platelet aggregation, reduce the surface activity of the platelets, improve the surface charges of red blood cells and the platelets and improve the blood fluidity.
The gleditsia sinensis is a natural plant and is widely applied to the aspect of medical care. The saponin is the main active component of the Chinese honey locust, has high foamability and strong decontamination capability, and is pounded and filtered to be made into shampoo with the functions of removing fat and relieving itching.
Isatis tinctoria is a cruciferae plant, alkaloid is a main chemical component of the Isatis tinctoria, and the water extract of Isatis tinctoria has a broad-spectrum antibacterial effect. The shampoo can be added into shampoo to effectively inhibit mass propagation of bacteria on scalp and relieve dandruff and scalp itching.
The invention reasonably utilizes various effective substances in the seven traditional Chinese medicine components, and adopts a specific extraction process, such as: the polygonum multiflorum, the gallnut, the carignan, the ligusticum wallichii and the glossy privet fruit adopt a continuous reflux extraction mode with ethanol as an extraction solvent, so that the extraction efficiency of active substances of the polygonum multiflorum, the gallnut, the carignan, the ligusticum wallichii and the glossy privet fruit can be improved, the dissolution of water-soluble impurities in an extracting solution can be effectively controlled, the extraction rate of index components is remarkably improved, and the content of the index components in the. In addition, high-speed countercurrent extraction method is adopted to enrich index components such as anthraquinone, tannin and flavonoid in Polygoni Multiflori radix, Galla chinensis and carignane, and the pharmaceutical composition prepared after purification has significantly enhanced drug effect. The glossy privet fruit, the szechuan lovage rhizome, the gleditsia sinensis lam and the isatis indigotica fort are respectively mixed and extracted, and active ingredients, namely the tetracyclic triterpenoid, volatile oil (the glossy privet fruit and the szechuan lovage rhizome) and saponins and alkaloids (the gleditsia sinensis lam and the isatis indigotica fort) can be effectively extracted, so that the application of the traditional Chinese medicine composition in the field of hair loss and hair growth is realized under the reasonable collocation.
The following examples are provided to illustrate specific embodiments of the present invention, and it is understood that the scope of the present invention is not limited to the following examples.
Example 1:
the embodiment relates to a hair growth traditional Chinese medicine composition which is prepared from the following raw materials in parts by weight: 40 parts of gallnut, 45 parts of fleece-flower root, 32 parts of honey locust, 40 parts of snakehead intestine, 28 parts of glossy privet fruit, 20 parts of szechuan lovage rhizome and 30 parts of isatis indigotica fort.
Taking the traditional Chinese medicine raw materials in the weight part ratio, and preparing the traditional Chinese medicine composition according to the following method:
preparing spray-dried powder of the gallnut extract:
(1) taking Galla chinensis as raw material, micronizing for 15min, placing into dynamic continuous circulation extraction device, adding 15 times (based on Galla chinensis raw material) of 70% ethanol, reflux extracting for 40min, starting circulation extraction at 80 deg.C for 3 hr, and collecting extractive solution.
(2) Concentrating the above extractive solution, adding appropriate amount of water into a concentration tank before concentrating, heating water to 90 deg.C, mixing with the extractive solution, concentrating, recovering ethanol, detecting with an ethanol concentration detector (liquid discharge port) every time, and concentrating under reduced pressure at 60 deg.C to obtain fluid extract with relative density of 1.08.
(3) Feeding the above fluid extract crude extract into a high-speed countercurrent extraction device, controlling the flow rate at 1.5mL/min, the rotation speed at 800r/min, the temperature of an extraction column at 26 ℃, selecting an ethyl acetate-n-butanol-water (5: 1.8: 6) solvent system to separate the tanning compounds, after the mixed solvent system is fully and uniformly mixed, standing for phase separation and ultrasonic degassing for 30min, taking the upper phase as the stationary phase and the lower phase as the mobile phase, separating the extract, and collecting the extract.
(4) Concentrating the collected extractive solution at 65 deg.C under reduced pressure to obtain fluid extract with density of 1.03, and spray drying at air inlet temperature of 180 deg.C and air outlet temperature of 85 deg.C to obtain spray dried powder of Galla chinensis extract.
(II) preparing spray-dried powder of the polygonum multiflorum extract:
(1) micronizing Polygoni Multiflori radix as raw material for 15min, placing in dynamic continuous circulation extraction device, adding 15 times (based on Polygoni Multiflori radix raw material) of 70% ethanol, reflux extracting for 45min, starting circulation extraction at 80 deg.C for 3 hr, and collecting extractive solution;
(2) concentrating the above extractive solution, adding appropriate amount of water into a concentration tank before concentrating, heating water to 90 deg.C, mixing with the extractive solution, concentrating, recovering ethanol when concentrating, and concentrating under reduced pressure at 60 deg.C to obtain fluid extract crude extract with relative density of 1.05;
(3) feeding the fluid extract crude extract into a high-speed countercurrent extraction device, controlling the flow rate to be 1.5mL/min, the rotating speed to be 730r/min, controlling the temperature of an extraction column to be 26 ℃, selecting a n-hexane-ethyl acetate-methanol-water (9: 1: 5: 5) solvent system to separate free anthraquinone compounds, after the mixed solvent system is fully and uniformly mixed, standing for phase separation and ultrasonic degassing for 30min, taking an upper phase as a stationary phase and a lower phase as a mobile phase, separating extract extractum, and collecting extract liquor;
(4) concentrating the collected extractive solution at 65 deg.C under reduced pressure to obtain fluid extract with density of 1.05, and spray drying at air inlet temperature of 180 deg.C and air outlet temperature of 85 deg.C to obtain spray dried powder of Polygoni Multiflori radix extract.
(III) preparing spray-dried powder of the snakehead intestine extract:
(1) taking snakehead gut as a raw material, carrying out superfine grinding for 15min, then placing the snakehead gut in a dynamic continuous circulating extraction device, adding 15 times (calculated by the snakehead gut raw material) of 70% ethanol, carrying out reflux extraction for 40min, then starting circulating extraction, wherein the extraction temperature is 70 ℃, extracting for 3h, and then collecting an extracting solution;
(2) concentrating the above extractive solution, adding appropriate amount of water into a concentration tank before concentrating, heating water to 90 deg.C, mixing with the extractive solution, concentrating, recovering ethanol when concentrating, and concentrating under reduced pressure at 60 deg.C to obtain fluid extract crude extract with relative density of 1.06;
(3) feeding the fluid extract crude extract into a high-speed countercurrent extraction device, controlling the flow rate to be 1.4mL/min, the rotating speed to be 800r/min, controlling the temperature of an extraction column to be 26 ℃, selecting a n-hexane-ethyl acetate-methanol-water (1: 0.6: 0.6: 1) solvent system to separate flavonoid compounds, after the mixed solvent system is fully and uniformly mixed, standing for phase separation and ultrasonic degassing for 30min, taking an upper phase as a stationary phase and a lower phase as a mobile phase, separating the extract, and collecting an extract liquor;
(4) concentrating the collected extractive solution at 65 deg.C under reduced pressure to obtain fluid extract with density of 1.02, and spray drying the fluid extract at air inlet temperature of 180 deg.C and air outlet temperature of 85 deg.C to obtain spray dried powder of snakehead intestine extract.
(IV) preparing spray-dried powder of mixed extract of glossy privet fruit and ligusticum wallichii:
(1) mixing fructus Ligustri Lucidi and rhizoma Ligustici Chuanxiong as raw materials, micronizing for 15min, placing into dynamic continuous circulation extraction device, adding 15 times (based on total raw materials of fructus Ligustri Lucidi and rhizoma Ligustici Chuanxiong) of 50% ethanol, reflux extracting for 40min, and collecting extractive solution after 3 hr at 70 deg.C;
(2) concentrating the above extractive solution, adding appropriate amount of water into a concentration tank before concentrating, heating water to 90 deg.C, mixing with the extractive solution, concentrating, and concentrating under reduced pressure at 60 deg.C to obtain fluid extract crude extract with relative density of 1.04;
(3) spray drying the above fluid extract crude extract at air inlet temperature of 180 deg.C and air outlet temperature of 85 deg.C to obtain spray dried powder of mixed extract of fructus Ligustri Lucidi and rhizoma Ligustici Chuanxiong.
(V) preparing spray-dried powder of the mixed extract of the gleditsia sinensis and the isatis indigotica fort:
(1) mixing fructus Gleditsiae Abnormalis and Isatis tinctoria as raw materials, pulverizing, decocting in water for 2 times, adding 10 times of water, soaking for 60min, boiling, maintaining slight boiling for 60min, and filtering; adding 8 times of water into the second decoction, circularly heating to 94 ℃, timing, decocting for 60min, controlling the temperature at 100 ℃, filtering, and combining the two filtrates;
(2) concentrating the above filtrate, adding appropriate amount of water into a concentration tank before concentrating, heating water to 90 deg.C, mixing with the extractive solution, concentrating, and concentrating under reduced pressure at 60 deg.C to obtain fluid extract crude extract with relative density of 1.05;
(3) spray drying the above fluid extract crude extract at air inlet temperature of 180 deg.C and air outlet temperature of 85 deg.C to obtain spray dried powder of mixed extract of fructus Gleditsiae Abnormalis and Isatis tinctoria.
(VI) mixing of spray-dried powders
Mixing the spray-dried powders obtained by the above processes, micronizing, feeding into a total mixer, and mixing at 14 deg.C at a feeding speed of 20 min/time and 5kg each time to obtain the Chinese medicinal composition.
Examples 2 to 8:
based on the example 1, the hair growth promoting traditional Chinese medicine composition corresponding to the hair growth promoting traditional Chinese medicine composition is prepared according to the following raw material proportion and process control parameters, and the hair growth promoting traditional Chinese medicine composition is shown in tables 1 to 5.
Table 1 raw material proportioning data table
TABLE 2 Process control parameter data sheet I
TABLE 3 Process control parameter data sheet (II)
TABLE 4 Process control parameter data sheet III
TABLE 5 Process control parameter data sheet (IV)
Effective substances of the hair-growing traditional Chinese medicine compositions prepared in the embodiments 1 to 8 are detected, and the main effective substances are shown in the following table 6.
TABLE 6 data table of contents of effective substances of hair growth promoting Chinese medicinal composition
It is known that the existing drying methods include normal temperature drying, low temperature vacuum drying and freeze drying, and the products obtained by the drying methods all need to be crushed and then used, and in addition, the following defects exist: drying at normal temperature, long time consumption, high energy consumption, dark color of the dry powder, caramel flavor and the like. Low-temperature vacuum drying, long time, high energy consumption, black dry powder color, caramel flavor and narrow product application range. Freeze drying for long time and high energy consumption, and the color of the dry powder is yellow.
In order to overcome the defects of the drying mode, in the aspect of production process, the spray drying mode is adopted, the problem of thick black of the traditional Chinese medicine is solved, the color of the traditional Chinese medicine composition product prepared by the process is yellow, the application of the raw materials is greatly enhanced, the dry powder is easy to store and transport, and the addition amount can be accurately controlled during application (the liquid preparation solvent influences the application). Therefore, the invention also has the application in preparing medicines or washing and caring products, and can be used for preparing external preparations such as ointment, spray, essence, gel, liniment, shampoo and the like.
Example 9:
the embodiment relates to application of a hair growth traditional Chinese medicine composition in preparing an ointment.
The hair-growing traditional Chinese medicine composition described in example 1 is used as an active ingredient, and an ointment is prepared according to a conventional ointment preparation method in the field. Specifically, the method comprises the following steps: dissolving an oil phase, placing the oil phase in a water bath kettle at the temperature of 80 ℃, and keeping the temperature at constant temperature, wherein the oil phase comprises 10.0 parts of stearic acid, 7.0 parts of ethylene glycol monostearate, 7.0 parts of white vaseline and 5.0 parts of liquid paraffin; adding the water phase heated to a slightly boiling state into the oil phase, slowly and quickly stirring, and stirring at the temperature of 80 ℃ for 10 min, wherein the water phase comprises 60.0 parts of water, 5.0 parts of sodium dodecyl sulfate, 3.0 parts of active ingredient extract, 0.2 part of ethyl p-hydroxybenzoate, 0.3 part of menthol and 0.1 part of potassium sorbate; taking the ointment out of the water bath, and continuously stirring to room temperature.
Example 10:
the embodiment relates to application of a hair growth traditional Chinese medicine composition in preparing a spray.
The hair growth promoting traditional Chinese medicine composition in the embodiment 3 is used as an active ingredient, and the spray is prepared according to a conventional spray preparation method in the field. Specifically, the method comprises the following steps: adding 3.0 parts of the pharmaceutical composition into 15 parts of 80% ethanol in a water bath at 40 ℃, stirring uniformly, adding 0.2 part of benzoic acid, mixing uniformly, adding 1 part of tween-80, 8 parts of propylene glycol and 72.8 parts of distilled water, and stirring uniformly to obtain the pharmaceutical composition.
Example 11:
the embodiment relates to application of a hair growth traditional Chinese medicine composition in preparation of essence.
The hair growth traditional Chinese medicine composition in the embodiment 4 is used as an active ingredient, and the essence is prepared according to a conventional essence preparation method in the field. Specifically, the method comprises the following steps: adding the active ingredient extract 3.0 parts into distilled water 89.3 parts, dissolving, adding carbomer 0.4 part, homogenizing, adding benzoic acid 0.2 part, glycerol 2 parts and propylene glycol 5 parts, stirring, adding triethanolamine 0.1 part, and stirring.
Example 12:
the embodiment relates to application of a hair growth traditional Chinese medicine composition in preparing gel.
The hair-growing traditional Chinese medicine composition in the embodiment 5 is used as an active ingredient, and the gel is prepared according to a conventional method for preparing gel in the field. Specifically, the method comprises the following steps: adding the active ingredient extract 3.0 parts into distilled water 85 parts, dissolving, adding carbomer 1.5 parts, triethanolamine 1.0 parts, ethyl p-hydroxybenzoate 0.2 parts, glycerol 8.0 parts, menthol 0.3 parts and potassium sorbate 0.1 parts, and stirring.
Example 13:
the embodiment relates to application of a hair growth traditional Chinese medicine composition in preparing a liniment.
The hair growth traditional Chinese medicine composition in the embodiment 7 is used as an active ingredient, and the liniment is prepared according to a conventional method for preparing the liniment in the field. Specifically, the method comprises the following steps: adding the active ingredient extract 3.0 parts into distilled water 87 parts, dissolving, adding glycerol 3 parts, propylene glycol 5 parts, water-soluble bisabolol 1 part and phenoxyethanol 1 part, and mixing.
Example 14:
the embodiment relates to application of a hair growth traditional Chinese medicine composition in preparing shampoo.
Shampoo is prepared by using the hair growth promoting Chinese medicinal composition described in example 8 as an active ingredient according to a conventional method for preparing shampoo in the field. Specifically, the method comprises the following steps: 77.8 parts of deionized water, 1.0 part of conditioner, 0.1 part of ethylenediamine tetraacetic acid-2 sodium, 0.2 part of allantoin, 14.0 parts of fatty alcohol-polyoxyethylene ether sodium sulfate, 3.0 parts of cocamidomethyl, 0.2 part of pearlescent slurry, 0.6 part of silicone oil and 0.1 part of phenoxyethanol are prepared into a matrix, 3.0 parts of the medicinal composition (in weight ratio) is added into the matrix, and then the conventional amount of auxiliary materials such as sodium chloride, essence and the like are added to prepare the shampoo.
The research finds that the Hepatocyte Growth Factor (HGF) and the Vascular Endothelial Growth Factor (VEGF) are two growth factors of hair papilla, and the two growth factors are secreted by the hair papilla of hair follicles in the growth phase and have obvious promotion effect on hair growth, so that the observation of the mRNA expression levels of the hair follicles HGF and VEGF plays an important role in the research of the dynamic growth of the hair follicles.
Based on the above research results, the following cell experiments were performed to compare the effects of the Chinese medicinal composition of the present invention.
1 cell assay
1.1 Experimental materials: female C57BL/6 mice (SPF grade) 7-8 weeks old.
1.2 Experimental instruments: ECLIPSETi-S dual port inverted microscope.
1.3 Experimental methods:
1.3.1 Hair follicle isolation
Killing a C57BL/6 mouse, cutting off bilateral beards, disinfecting the upper lip with 75% ethanol, washing with sterile normal saline, cutting bilateral beard pads under sterile conditions, placing in Hank's solution, separating and lightly taking hair follicles on the eye side of the beard pads, wherein each beard pad can take 7-9 hair follicles, and selecting the hair follicles in the complete growth phase (the hair follicles are large, smooth and mellow, the dermal tissue sheath is complete and has no separation from the outer cuticle root sheath) for culture.
1.3.2 Experimental groups
Blank group: and (4) distilled water.
Test groups: the Chinese medicinal composition related to the above example 1 was used as an active ingredient to prepare a solution of 1200. mu.g/l.
Control group 1: extracting Polygoni Multiflori radix, Galla chinensis and jejunum by continuous reflux extraction, and spray drying the powder of anthraquinone, tannin and flavonoid by high speed countercurrent extraction to obtain 1200 μ g/l solution.
Control group 2: continuously reflux-extracting fructus Ligustri Lucidi and rhizoma Ligustici Chuanxiong to obtain spray-dried powder, and making into 1200 μ g/l solution.
Control group 3: spray drying the powder with Gleditsia sinensis and Isatis tinctoria aqueous extract to obtain 1200 μ g/l solution.
1.3.3 Hair follicle culture
Hair follicle cultures were performed in 24-well plates, supplemented with William E serum-free medium, 37 ℃, 5% CO2Incubating for 12h under the condition, selecting hair follicles with intact morphology and similar growth speed, adding 20 hair follicles into each group with 3 pores, adding the solution to be tested, and culturing for 4d, 8d and 1d respectively2d。
1.3.4RT-PCR
A one-step RT-PCR amplification system kit is adopted, a pair of primer sequences specific to mouse VEGFmRNA are 5'-CCATGAATTTGACCTCTATG-3' and 5'-AATGCTTTCTCCGCTCTGAA-3', and an amplification product is 207 bp. A pair of primer sequences specific to the mouse HGFmRNA are 5'-CCATGAATTTGACCTCTATG-3' and 5'-ACTGAGGAATGTCACAGACT-3', and the amplification product is 278 bp.
1.3.5 internal reference
In order to ensure the accuracy of the experiment, a specific primer aiming at mRNA of the mouse beta-actin is added into a reaction system to be used as an internal reference, so that the mRNA in a sample is proved to be completely extracted, and meanwhile, the mRNA can be used as an internal reference of semi-quantitative RT-PCR.
1.3.6 quantification of RT-PCR reaction products
Products after RT-PCR amplification are subjected to agarose gel electrophoresis with the mass fraction of 2%, stained by ethidium bromide, and the gel is subjected to density scanning under ultraviolet rays, so that the absolute density of each positive band is obtained.
1.4 detection index
1.4.1 Hair Length determination
The hair length (distance from the base of the follicle to the top of the hair) was measured daily under an inverted microscope.
1.4.2 Hair growth Rate
The ratio of the difference in hair length between 2 adjacent measurements to the number of days of measurement (mm/d).
1.4.3 Hair growth time
Days (d) when the hair did not lengthen any longer than the length of the first 1 d.
1.4.4 hepatocyte growth factor mRNA expression levels
And (3) carrying out electrophoresis on products amplified by RT-PCR in agarose gel with the mass fraction of 2%, staining by ethidium bromide, and carrying out density scanning on the gel under the ultraviolet condition to obtain the product.
1.4.5 vascular endothelial cell growth factor mRNA expression levels
And (3) carrying out electrophoresis on products amplified by RT-PCR in agarose gel with the mass fraction of 2%, staining by ethidium bromide, and carrying out density scanning on the gel under the ultraviolet condition to obtain the product.
1.5 results of the experiment
1.5.1 the effect of the extracts of the pharmaceutical composition on hair growth rate and hair growth duration is shown in Table 7 below.
TABLE 6 Effect of extracts of pharmaceutical compositions on Hair growth Rate and Hair growth time
1.5.2 expression level of hepatocyte growth factor mRNA by extract of pharmaceutical composition
On the 4 th day of culture, there was no significant difference in the mRNA expression of HGF278bp between the test group and the control groups 1, 2, 3, on the 8 th day of culture, the mRNA expression of HGF278bp in the test group was significantly stronger than that in the control groups 1, 2, 3, and on the 12 th day of culture, the mRNA expression of HGF278bp in the test group was still stronger than that in the blank group and the control groups 1, 2, 3. Gel density scan quantitative analysis results of electrophoresis results of RT-PCR products show that the density ratio of HGF/beta-actin at 4, 8 and 12 days of culture is 0.4726, 0.2958, 0.2743 and 0.2564 in the test group and the control group respectively, which is obviously higher than that in the blank group.
1.5.3 vascular endothelial cell growth factor mRNA expression levels
On day 4 of culture, there was no significant difference in the mRNA expression of EVGF207bp between the test and control groups 1, 2 and 3, on day 8, the mRNA expression of EVGF207bp was significantly stronger in the test group than in the control groups 1, 2 and 3, and on day 12, the mRNA expression of VEGF207bp was still stronger in the test group than in the blank and control groups 1, 2 and 3. Gel density scan quantitative analysis results of electrophoresis results of RT-PCR products show that the density ratio of VEGF/beta-actin at 4, 8 and 12 days of culture is 0.6315, 0.4285, 0.4379 and 0.3957 in the test group and the control group respectively, which is obviously higher than that in the blank group.
The cell experiment results show that the combined extract has the effects of promoting the differentiation and development of hair follicle cells, increasing the volume of hair follicles and increasing the length of hair shafts. Animal experiments show that the pharmaceutical composition can up-regulate the mRNA expression of VEGF and HGF cultured in hair follicles, and obviously prolong the expression time. Therefore, one of the mechanisms of the pharmaceutical composition for promoting hair growth is to achieve the effect of promoting hair growth by promoting the mRNA expression of the papilla VEGF and HGF.
2. Experiment for inhibiting bacteria
2.1 strains
Propionibacterium acnes, Escherichia coli and Staphylococcus aureus are all provided by the Sichuan industrial microorganism strain preservation management center.
2.2 culture Medium
The bacterial solid culture medium consists of the following components: 4g of beef extract, 12g of peptone, 3g of sodium chloride, 20g of agar and 1000 ml of water, and the pH value is 7.2-7.4.
2.3 bacterial activation
Under aseptic condition, using freshly prepared bacterial solid culture medium to transfer the preserved strains of propionibacterium acnes, escherichia coli and staphylococcus aureus, and keeping CO at constant temperature of 37 DEG C2The culture is carried out in an incubator for 24 hours for later use.
2.4 preparation of the bacterial suspension
Adding appropriate amount of sterile water into the activated test tube, adding 50 ml of sterile normal saline, and shaking in constant temperature shaking table at 37 deg.C for 60 min. Preparing bacterial suspension with thallus number of 106CFU/ml by using sterile water by a blood counting method, and storing the bacterial suspension in a refrigerator at 4 ℃.
2.5 Experimental groups
Blank group: and (4) distilled water.
Test groups: the Chinese medicinal composition related to the above example 1 was used as an active ingredient to prepare a solution of 0.05 mg/ml.
Control group 1: extracting Polygoni Multiflori radix, Galla chinensis and jejunum by continuous reflux extraction, and spray drying the powder to obtain 0.05mg/ml solution.
Control group 2: continuously reflux-extracting fructus Ligustri Lucidi and rhizoma Ligustici Chuanxiong to obtain spray-dried powder, and making into 0.05mg/ml solution.
Control group 3: spray drying the powder with Gleditsia sinensis and Isatis tinctoria aqueous extract to obtain 0.05mg/ml solution.
2.6 determination of bacteriostatic action
And (3) measuring the inhibition effect of the experimental groups on the test bacteria by adopting a filter paper diffusion method, respectively taking 0.2ml of each of the 4 test bacteria suspensions, inoculating the suspensions on the surface of a culture medium, and uniformly coating to prepare a bacteria-containing flat plate. Using a puncher to punch filter paper into small filter paper sheets with the diameter of 10mm, soaking the filter paper in a blank group, a test group and a control group 1, 2 and 3 respectively after sterilization for 2 hours, treating 3 kinds of filter paper in parallel, culturing for 24 hours at the temperature of 30 ℃, measuring the diameter of a bacteriostatic circle by using a cross method, and taking an average value.
2.7 zone of inhibition test
The scalp is distributed with a plurality of microorganisms, mainly including staphylococcus, propionibacterium and malassezia, and pityriasis capitis is generally regarded as mild non-inflammatory seborrheic dermatitis. The experimental results show that the extracts have certain bacteriostatic action on the three bacteria, but the experimental groups have the strongest bacteriostatic ability, the bacteriostatic ability of the extracts is staphylococcus aureus, escherichia coli and propionibacterium acnes in turn, and the difference of the bacteriostatic ability among the control groups is smaller. The experiment has weak bacteriostatic action on propionibacterium acnes, mainly because the ferulic acid ethyl ester component in the ligusticum wallichii is beneficial to the growth of propionibacterium acnes. Research shows that the propionibacterium acnes is low in abundance in pityriasis capitis patients and high in abundance in healthy scalps, so that the propionibacterium acnes is known to be the dominant bacteria of the scalps and is beneficial to maintaining the microbial stability of the healthy scalps.
3 clinical data
150 patients suffering from seborrheic alopecia and diagnosed in dermatology department of Chengdu Chinese medicine university subsidiary hospital in Ouchuan province in 2018 from 6 months to 2018 at 12 months are selected. 95 male and 55 female, with the age of 18-50, and the average (37 + -3) years. The above volunteers were randomly divided into 3 groups of 30 persons each.
3.1 inclusion criteria
Firstly, the Chinese medicine accords with the Western medicine diagnosis standard of clinical dermatology (the hairs on two sides of forehead begin to be gradually thin and sparse and extend to the top of the head, the hair line on the forehead retreats backwards, the forehead is raised to form high forehead, and the skin damage area is in a V shape and is as smooth as a mirror);
secondly, the traditional Chinese medicine syndrome diagnosis standard (the hair is moist, like smeared oil, a plurality of hairs are adhered to each other, the scalp has scales and involuntary pruritus, the stool is dry, the urine is yellow and red, the tongue is yellow, the pulse is wiry, smooth and rapid) of the traditional Chinese medicine dermatosis is met;
③ the age is 18-50 years old;
fourthly, agreeing to the content of the treatment scheme and signing an informed consent voluntarily;
no steroid medicine such as skin is taken in nearly half a year;
sixthly, patients who have not been transplanted hair.
3.2 exclusion indices
The age is less than 18 years old and more than 50 years old;
② allergic persons to the product of the test;
③ those with severe systemic diseases or chronic wasting diseases;
fourthly, alopecia caused by other reasons, congenital alopecia totalis, traumatic alopecia, chemotherapy or postpartum alopecia.
3.3 methods of treatment
Blank group: the essence prepared by taking the hair-growing traditional Chinese medicine composition of the embodiment 1 as an active ingredient is adopted, and the crude drug amount in the essence is 0 g/ml. The using method comprises the following steps: 2-3 times in 1 day, the dosage is 3-5 ml each time, and the using method comprises the following steps: the appropriate amount of essence is absorbed into a specific liquid outlet comb by a dropper each time, comb teeth are arranged on the scalp, the comb teeth are pressed by appropriate force and roll smoothly until the essence used for a single time is completely and uniformly smeared on the scalp.
Test groups: the essence prepared by using the hair growth promoting traditional Chinese medicine composition of the embodiment 1 as an active ingredient has a crude drug amount of about 3 g/ml. The using method comprises the following steps: 2-3 times in 1 day, the dosage is 3-5 ml each time, and the using method comprises the following steps: the appropriate amount of essence is absorbed into a specific liquid outlet comb by a dropper each time, comb teeth are arranged on the scalp, the comb teeth are pressed by appropriate force and roll smoothly until the essence used for a single time is completely and uniformly smeared on the scalp.
Control group 1: the essence is prepared from anthraquinone, tannin and flavonoid components obtained by high-speed countercurrent extraction method enrichment after continuous reflux extraction of Polygoni Multiflori radix, Galla chinensis and carignan intestine, and the crude drug amount in the essence is about 3 g/ml. The using method comprises the following steps: 2-3 times in 1 day, the dosage is 3-5 ml each time, and the using method comprises the following steps: the appropriate amount of essence is absorbed into a specific liquid outlet comb by a dropper each time, comb teeth are arranged on the scalp, the comb teeth are pressed by appropriate force and roll smoothly until the essence used for a single time is completely and uniformly smeared on the scalp.
Control group 2: continuously extracting fructus Ligustri Lucidi and rhizoma Ligustici Chuanxiong under reflux to obtain spray dried powder, and making into essence with crude drug amount of about 3 g/ml. The using method comprises the following steps: 2-3 times in 1 day, the dosage is 3-5 ml each time, and the using method comprises the following steps: the appropriate amount of essence is absorbed into a specific liquid outlet comb by a dropper each time, comb teeth are arranged on the scalp, the comb teeth are pressed by appropriate force and roll smoothly until the essence used for a single time is completely and uniformly smeared on the scalp.
Control group 3: the essence is prepared by spray drying powder of gleditsia sinensis lam and isatis tinctoria aqueous extract, and the crude drug amount in the essence is about 3 g/ml. The using method comprises the following steps: 2-3 times in 1 day, the dosage is 3-5 ml each time, and the using method comprises the following steps: the appropriate amount of essence is absorbed into a specific liquid outlet comb by a dropper each time, comb teeth are arranged on the scalp, the comb teeth are pressed by appropriate force and roll smoothly until the essence used for a single time is completely and uniformly smeared on the scalp.
3.4 therapeutic efficacy criteria
The evaluation is carried out according to clinical dermatology and traditional Chinese medicine dermatosis and combined with clinic:
and (3) healing: the symptoms of pruritus, greasiness and scales disappear, the color and the thickness of hair are normal, and sebum secretion is normal;
the effect is shown: the new hair is more, and the pruritus, the greasiness and the scales are obviously reduced;
the method has the following advantages: a large amount of vellus hairs grow in the bald area, and pruritus, greasiness and scales are reduced;
and (4) invalidation: no new hair growth was observed, or a small amount of hair was dropped after growth.
Total effective rate = (recovery + significant effect + effective) cases/total cases × 100%.
3.5 therapeutic results
The treatment results of the essence prepared from the hair growth promoting Chinese medicinal composition of the embodiment 1 and the essences prepared from the control groups 1 to 3 are shown in the following table 8.
TABLE 8 treatment results of essences prepared from the Chinese medicinal composition and essences prepared from the control groups 1-3
The test results show that: the prescription comprises 7 traditional Chinese medicines, namely polygonum multiflorum, gallnut and carignane which have the relationship of horn and drug, and anthraquinone compounds, tannin compounds and flavonoid compounds are respectively separated from the 3 traditional Chinese medicines and respectively have the effects of promoting hair growth, removing dandruff, relieving itching and stabilizing hair roots. The active ingredients in fructus Ligustri Lucidi and rhizoma Ligustici Chuanxiong are tetracyclic triterpenes and volatile oil, which can promote hair follicle growth and improve scalp blood microcirculation. The active ingredients of the Chinese honeylocust fruit and the isatis indigotica fort are saponins and alkaloids respectively, and the saponins and the alkaloids can dispel scalp grease and relieve dandruff and head itching. The 7 traditional Chinese medicines are compatible for use, and can fundamentally improve the alopecia condition under the multi-dimensional synergistic effect of maintaining healthy scalp, promoting hair follicle growth and stabilizing hair roots.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and all simple modifications and equivalent variations of the above embodiments according to the technical spirit of the present invention are included in the scope of the present invention.
Claims (10)
1. A hair-growing traditional Chinese medicine composition is characterized in that: the traditional Chinese medicine composition is prepared from the following raw materials in parts by weight: 10-60 parts of gallnut, 20-60 parts of polygonum multiflorum, 20-45 parts of gleditsia sinensis, 20-65 parts of snakehead intestine, 20-50 parts of glossy privet fruit, 10-30 parts of ligusticum wallichii and 10-45 parts of isatis indigotica, wherein the traditional Chinese medicine composition comprises the following effective components: tannin compounds are more than or equal to 85.86mg/g, anthraquinone compounds are more than or equal to 0.29mg/g, flavonoid compounds are more than or equal to 97.58mg/g, terpenoid compounds are more than or equal to 1.69mg/g, tetracyclic triterpenoid compounds are more than or equal to 0.95mg/g, saponin compounds are more than or equal to 53.2mg/g, volatile oil is more than or equal to 28.36mg/g, and alkaloid is more than or equal to 40.30 mg/g.
2. The hair growth promoting traditional Chinese medicine composition according to claim 1, which is characterized in that: in the traditional Chinese medicine composition, the tannin compound is 85.86-119.27 mg/g, the anthraquinone compound is 0.29-0.85 mg/g, the flavonoid compound is 97.58-116.86 mg/g, the terpenoid compound is 1.69-5.61 mg/g, the tetracyclic triterpenoid compound is 0.95-3.06 mg/g, the saponin compound is 53.20-78.90 mg/g, the volatile oil is 28.36-44.21 mg/g, and the alkaloid is 40.30-64.57 mg/g.
3. A preparation method of a hair growth traditional Chinese medicine composition is characterized by comprising the following steps: according to the weight portion of the raw materials of claim 1, the following steps are carried out:
(1) preparing spray-dried powder of a gallnut extract, spray-dried powder of a polygonum multiflorum extract and spray-dried powder of a snakehead intestine extract by respectively taking gallnut, polygonum multiflorum and snakehead intestine as raw materials for later use;
(2) preparing spray-dried powder of a mixed extract of glossy privet fruit and ligusticum wallichii by taking glossy privet fruit and ligusticum wallichii as raw materials for later use;
(3) preparing spray-dried powder of mixed extract of Gleditsia sinensis and Isatis tinctoria from Gleditsia sinensis and Isatis tinctoria;
(4) mixing the spray-dried powder prepared in the steps (1) to (3) and carrying out superfine grinding to prepare the traditional Chinese medicine composition,
the traditional Chinese medicine composition comprises the following effective components: tannin compounds are more than or equal to 85.86mg/g, anthraquinone compounds are more than or equal to 0.29mg/g, flavonoid compounds are more than or equal to 97.58mg/g, terpenoid compounds are more than or equal to 1.69mg/g, tetracyclic triterpenoid compounds are more than or equal to 0.95mg/g, saponin compounds are more than or equal to 53.2mg/g, volatile oil is more than or equal to 28.36mg/g, and alkaloid is more than or equal to 40.30 mg/g.
4. The preparation method of the hair growth traditional Chinese medicine composition according to claim 3, which is characterized in that: in the step (1), the step of preparing spray-dried powder of the gallnut extract comprises:
(1.1 a) taking gallnut as a raw material, carrying out superfine grinding, then using 70% ethanol as an extraction solvent, carrying out reflux extraction for 40min in a dynamic continuous circulating extraction device, then starting circulating extraction, wherein the extraction temperature is 78-82 ℃, extracting for 3h, and then collecting an extracting solution;
(1.2 a) mixing the extracting solution obtained in the step (1.1 a) with water at 90 ℃, concentrating, recovering alcohol during concentration, and when the alcohol concentration is lower than 45%, not recovering, and then concentrating under reduced pressure at 55-65 ℃ to obtain a clear paste crude extract with the relative density of 1.05-1.10;
(1.3 a) feeding the clear paste crude extract obtained in the step (1.2 a) into a high-speed countercurrent extraction device, controlling the flow rate to be 1.2-1.6 mL/min, the rotating speed to be 795-805 r/min, the temperature of an extraction column to be 25-27 ℃, and controlling the solvent system to be ethyl acetate-n-butanol-water 5: 1.8: 6, standing, phase splitting, ultrasonically degassing for 30min, separating the extract by taking the upper phase as a stationary phase and the lower phase as a mobile phase, and collecting the extract;
(1.4 a) carrying out reduced pressure concentration on the extract obtained in the step (1.3 a) at the temperature of 60-70 ℃ to obtain clear paste with the density of 1.01-1.05, and carrying out spray drying on the clear paste at the air inlet temperature of 178-182 ℃ and the air outlet temperature of 83-87 ℃ to obtain spray-dried powder of the gallnut extract.
5. The preparation method of the hair growth traditional Chinese medicine composition according to claim 3, which is characterized in that: in the step (1), the step of preparing the spray-dried powder of the polygonum multiflorum extract comprises:
(1.1 b) taking polygonum multiflorum as a raw material, carrying out superfine grinding, then using 70% ethanol as an extraction solvent, carrying out reflux extraction for 45min in a dynamic continuous circulating extraction device, then starting circulating extraction, wherein the extraction temperature is 78-82 ℃, extracting for 3h, and then collecting an extracting solution;
(1.2 b) mixing the extracting solution obtained in the step (1.1 b) with water at 90 ℃, concentrating, recovering alcohol during concentration, and when the alcohol concentration is lower than 45%, not recovering, and then concentrating under reduced pressure at 55-65 ℃ to obtain a clear paste crude extract with the relative density of 1.05-1.10;
(1.3 b) feeding the clear paste crude extract obtained in the step (1.2 b) into a high-speed countercurrent extraction device, controlling the flow rate to be 1.2-1.6 mL/min, the rotation speed to be 725-735 r/min, the temperature of an extraction column to be 25-27 ℃, and controlling the solvent system to be n-hexane-ethyl acetate-methanol-water 9: 1: 5: 5, standing, phase splitting, ultrasonically degassing for 30min, separating the extract by taking the upper phase as a stationary phase and the lower phase as a mobile phase, and collecting the extract;
(1.4 b) carrying out reduced pressure concentration on the extract obtained in the step (1.3 b) at the temperature of 60-70 ℃ to obtain clear paste with the density of 1.01-1.05, and carrying out spray drying on the clear paste at the air inlet temperature of 178-182 ℃ and the air outlet temperature of 83-87 ℃ to obtain spray-dried powder of the polygonum multiflorum extract.
6. The preparation method of the hair growth traditional Chinese medicine composition according to claim 3, which is characterized in that: in the step (1), the step of preparing the spray-dried powder of the snakehead gut extract comprises the following steps:
(1.1 c) taking snakehead gut as a raw material, carrying out superfine grinding, then using 70% ethanol as an extraction solvent, carrying out reflux extraction for 40min in a dynamic continuous circulating extraction device, then starting circulating extraction, wherein the extraction temperature is 68-72 ℃, extracting for 3h, and then collecting an extracting solution;
(1.2 c) mixing the extracting solution obtained in the step (1.1 c) with water at 90 ℃, concentrating, recovering alcohol during concentration, and when the alcohol concentration is lower than 45%, not recovering, and then concentrating under reduced pressure at 55-65 ℃ to obtain a clear paste crude extract with the relative density of 1.05-1.10;
(1.3 c) feeding the clear paste crude extract obtained in the step (1.2 c) into a high-speed countercurrent extraction device, controlling the flow rate to be 1.2-1.6 mL/min, the rotating speed to be 795-805 r/min, the temperature of an extraction column to be 25-27 ℃, and controlling the solvent system to be n-hexane-ethyl acetate-methanol-water 1: 0.6: 0.6: 1, standing, phase splitting, ultrasonically degassing for 30min, taking the upper phase as a stationary phase and the lower phase as a mobile phase, separating the extract, and collecting the extract;
(1.4 c) carrying out reduced pressure concentration on the extract obtained in the step (1.3 c) at the temperature of 60-70 ℃ to obtain clear paste with the density of 1.01-1.05, and carrying out spray drying on the clear paste at the air inlet temperature of 178-182 ℃ and the air outlet temperature of 83-87 ℃ to obtain spray-dried powder of the snakehead gut extract.
7. The preparation method of the hair growth traditional Chinese medicine composition according to claim 3, which is characterized in that: in the step (2), the step of preparing the spray-dried powder of the mixed extract of glossy privet fruit and ligusticum wallichii comprises the following steps:
(2.1) mixing the glossy privet fruit and the ligusticum wallichii as raw materials, carrying out superfine grinding, then using 50% ethanol as an extraction solvent, carrying out reflux extraction for 40min in a dynamic continuous circulation extraction device, then starting circulation extraction, wherein the extraction temperature is 68-72 ℃, extracting for 3h, and then collecting an extracting solution;
(2.2) mixing the extracting solution obtained in the step (2.1) with water at the temperature of 90 ℃, and then concentrating under reduced pressure at the temperature of 55-65 ℃ to obtain a clear paste crude extract with the relative density of 1.01-1.05;
and (2.3) carrying out spray drying on the clear paste crude extract obtained in the step (2.2) under the conditions of air inlet temperature of 178-182 ℃ and air outlet temperature of 83-87 ℃ to obtain spray dried powder of the mixed extract of the glossy privet fruit and the ligusticum wallichii.
8. The preparation method of the hair growth traditional Chinese medicine composition according to claim 3, which is characterized in that: in the step (3), the step of preparing a spray-dried powder of a mixed extract of the gleditsia sinensis lam and the isatis tinctoria includes:
(3.1) mixing the gleditsia sinensis and the isatis indigotica as raw materials, crushing, adding water, decocting for 2 times, adding 9-10 times of water into the decoction, soaking for 55-65 min, boiling, keeping slightly boiling for 60min, and filtering; adding 8-9 times of water into the second decoction, starting timing when circularly heating to 94 ℃, decocting for 60min, controlling the temperature at 94-102 ℃, filtering, and combining the two filtrates;
(3.2) mixing the combined filtrate obtained in the step (3.1) with water at 90 ℃, and then concentrating under reduced pressure at 55-65 ℃ to obtain a clear paste crude extract with the relative density of 1.01-1.05;
and (3.3) carrying out spray drying on the clear paste crude extract obtained in the step (3.2) at the air inlet temperature of 178-182 ℃ and the air outlet temperature of 83-87 ℃ to obtain spray dried powder of the mixed extract of the gleditsia sinensis lam and the isatis tinctoria.
9. The preparation method of the hair growth traditional Chinese medicine composition according to claim 3, which is characterized in that: in the step (4), the spray-dried powder prepared in the steps (1) to (3) is mixed and subjected to superfine grinding, and then the mixture is fed into a total mixer, and the traditional Chinese medicine composition is prepared after uniform mixing at the feeding speed of 20 min/time, 5kg of material for each feeding and the temperature of less than 16 ℃.
10. Use of the hair growth promoting Chinese medicinal composition according to claim 1 or 3 in the preparation of a medicament or a washing product.
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CN112716852A (en) * | 2021-01-17 | 2021-04-30 | 陈星宇 | Preparation method of shampoo capable of preventing hair loss, growing hair and blackening white hair |
CN117357624A (en) * | 2023-11-17 | 2024-01-09 | 四川省天府香疗健康技术研究院有限公司 | Hair-growing and hair-loss-preventing traditional Chinese medicine essential oil composition and preparation method and application thereof |
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