A dandruff-removing traditional Chinese medicine rich extract, a preparation method and application thereof

Abstract

This invention belongs to the field of scalp care technology, specifically relating to a concentrated extract of traditional Chinese medicine for dandruff removal, its preparation method, and its application. The concentrated extract is prepared from the following raw materials: chrysanthemum, honeysuckle, *Hosta plantago-aquatica*, gentian, *Smilax glabra*, and perilla. The preparation method includes water extraction, alcohol precipitation, macroporous resin purification, and concentration and drying steps. This invention also includes a no-rinse dandruff spray containing the concentrated extract. The concentrated extract and no-rinse spray prepared by this invention exhibit excellent inhibitory effects against *Malaisetta* and can significantly improve dandruff and scalp itching symptoms, demonstrating clear application value.

Description

Technical Field

[0001] This invention belongs to the field of scalp care technology, specifically relating to a traditional Chinese medicine extract for dandruff removal, its preparation method, and its application. Background Technology

[0002] Dandruff is one of the most common sub-health / mild scalp problems, typically manifesting as excessive shedding of the stratum corneum, forming white or grayish-white scales, often accompanied by varying degrees of itching, tightness, oiliness, odor, and recurring flare-ups. It and seborrheic dermatitis (SD) are often considered different severity stages of the same disease spectrum: dandruff is primarily characterized by "scalping without significant erythema or inflammation," while seborrheic dermatitis presents with more pronounced erythema, inflammation, and oily scales. This problem has a high incidence and recurrence rate in the adult population, affecting approximately 50% of adults globally, resulting in a significant socio-psychological burden and long-term care needs.

[0003] Current research generally agrees that the occurrence of dandruff and seborrheic dermatitis is closely related to three key factors: ① abnormal sebum secretion and its composition; ② imbalance of microbial metabolism and flora, with Malassezia as the core; and ③ individual susceptibility and abnormal skin barrier function. Malassezia is lipid-dependent; its secreted lipases can break down sebum triglycerides, producing free fatty acids. In susceptible individuals, this can induce a stimuli response and disrupt the skin barrier function, thereby triggering dandruff and itching.

[0004] Currently, the mainstream products for dandruff are mainly rinse-out shampoos, with commonly used active ingredients including antifungal drugs (such as ketoconazole and piroctone olamine) and keratolytic agents (such as salicylic acid). However, rinse-out products have significant drawbacks: the active ingredients only stay on the scalp for a short time during shampooing, making it difficult to maintain their effect; some dandruff-reducing products may cause dryness, stinging, and color fading after dyeing, affecting long-term adherence to use; and the relapse rate after discontinuation is relatively high.

[0005] In the field of dandruff treatment derived from traditional Chinese medicine, existing technologies mostly focus on preparing anti-dandruff shampoos or topical washes, with relatively insufficient systematic solutions for leave-on products. Chinese patents CN102670735A and CN103202786A disclose various traditional Chinese medicine anti-dandruff compositions, but most are rinse-off formulations. Leave-on sprays place higher demands on the clarity, low viscosity, low pigment content, storage stability, and smooth spraying of extracts, while the direct application of traditional Chinese medicine aqueous extracts often suffers from problems such as dark color, colloidal precipitation, and nozzle clogging.

[0006] Therefore, developing a traditional Chinese medicine enrichment extract that can effectively inhibit Malassezia and relieve scalp itching, and is also suitable for no-rinse spray formulations, as well as its preparation method, has important practical significance and clinical application value. Summary of the Invention

[0007] The purpose of this invention is to overcome the shortcomings of the prior art and provide a Chinese herbal medicine enrichment extract with good antibacterial effect, high clarity, and suitable for no-rinse spray, as well as its preparation method and application, to solve the problems of easy clogging of nozzles, storage precipitation, excessively dark color, and short residence time and easy recurrence of rinse-off products when using existing Chinese herbal medicine extracts for no-rinse spray.

[0008] This invention provides a method for preparing a concentrated extract of traditional Chinese medicine for dandruff removal. The concentrated extract is prepared from the following raw materials: chrysanthemum, honeysuckle, Gentiana scabra, Smilax glabra, and Perilla frutescens. The preparation method includes: extracting the raw materials with water to obtain an aqueous extract; subjecting the aqueous extract to alcohol precipitation, loading the supernatant onto a macroporous adsorption resin column, eluting sequentially with water and ethanol solutions, collecting the ethanol eluent, concentrating and drying it to obtain the final product.

[0009] In this invention, the raw materials are as follows by weight: 5-30 parts of chrysanthemum, 5-30 parts of honeysuckle, 2-20 parts of gentian and blue gentian, 5-40 parts of smilax glabra, and 2-20 parts of perilla.

[0010] In some embodiments, the raw materials are in the following proportions by weight: 10-25 parts chrysanthemum, 10-25 parts honeysuckle, 5-15 parts gentian and blue gentian, 10-35 parts smilax and 5-15 parts perilla.

[0011] In some implementations, the raw materials are in the following proportions by weight: 20 parts chrysanthemum, 20 parts honeysuckle, 10 parts gentian and blue gentian, 25 parts smilax and 10 parts perilla.

[0012] In this invention, the mass ratio of raw material to water in the water extraction step can be 1:(6-20), for example 1:8, 1:10, 1:12 or 1:15, etc.

[0013] In some implementations, the mass ratio of the raw material to water is 1:10.

[0014] In this invention, the water extraction can be performed by methods such as heating extraction, decoction extraction, reflux extraction, maceration extraction, or percolation extraction. The extraction temperature can range from room temperature to 100°C, preferably 60–100°C; for example, 70°C, 80°C, 90°C, or 100°C; the number of extractions can be 1–3 times, and the extraction time for each extraction can be 0.5–3 hours, for example, 1 hour, 1.5 hours, or 2 hours.

[0015] In this invention, the ethanol volume fraction in the alcohol precipitation step can be 60% to 90%, for example, 60%, 65%, 70%, 75%, 80%, or 85%. In some preferred embodiments, the ethanol volume fraction is 70%. The settling time can be 0.5 to 24 hours, for example, 1 hour, 4 hours, 8 hours, 12 hours, or 24 hours. The methods for separating the precipitate include, but are not limited to, centrifugation, filtration, or combinations thereof.

[0016] In this invention, the macroporous adsorption resin includes, but is not limited to, one or more of AB-8, D101, HPD-100, and HPD-600. In the elution step, elution is first performed with water, followed by elution with an ethanol solution; wherein the water elution volume can be 2 to 10 column volumes, for example, 2, 4, 5, 6, 8, or 10 column volumes; and the ethanol solution elution volume can be 1 to 8 column volumes, for example, 1, 2, 4, 5, 6, or 8 column volumes. The volume fraction of the ethanol solution can be 60% to 80%, preferably 70%.

[0017] In this invention, the preparation method may further include the following steps: combining the precipitate obtained by alcohol precipitation with the water eluent from the resin purification process to recover the residual effective components therein; and / or concentrating and drying the water eluent after resin purification to recover and reuse it as a byproduct.

[0018] In this invention, the concentration and drying step includes, but is not limited to, one or more of spray drying, vacuum drying, and freeze drying.

[0019] This invention provides a traditional Chinese medicine enrichment extract for dandruff removal, which is prepared by the above-described preparation method.

[0020] This invention provides a no-rinse anti-dandruff spray, which includes a concentrated extract of the traditional Chinese medicine for dandruff removal.

[0021] In this invention, the amount of the dandruff-removing herbal extract added is 0.05 to 5.0 wt% by weight of the finished product, for example, 0.1 wt%, 0.5 wt%, 1.0 wt%, 2.0 wt%, or 5.0 wt%.

[0022] In this invention, the spray further includes 0.02 to 0.30 wt% chlorhexidine acetate, for example, 0.05 wt%, 0.10 wt%, 0.15 wt%, or 0.20 wt%.

[0023] In this invention, the no-rinse anti-dandruff spray further comprises a cosmetically acceptable carrier. The carrier includes, but is not limited to, an aqueous phase and a moisturizing / solubilizing system. The moisturizing / solubilizing system is selected from one or more of glycerin, propylene glycol, 1,3-propanediol, and butylene glycol, and its addition amount can be 1–20 wt%, for example, 2 wt%, 5 wt%, 8 wt%, 10 wt%, 15 wt%, or 20 wt%.

[0024] In this invention, the spray may also contain one or more excipients selected from pH adjuster, chelating agent, antioxidant, and fragrance. For example, the chelating agent may be selected from at least one of disodium EDTA and tetrasodium EDTA, and the amount added may be 0.01 to 0.05 wt%.

[0025] In this invention, the pH of the no-rinse dandruff spray is 4.5 to 6.5, for example, 4.5, 5.0, 5.5, 6.0 or 6.5.

[0026] In this invention, the preparation method of the no-rinse anti-dandruff spray includes, but is not limited to: dissolving or dispersing the above-mentioned enriched extract of traditional Chinese medicine in a carrier, adding chlorhexidine acetate (0.18% to 0.22% in the final solution) and other optional excipients, adjusting the pH to 4.5 to 6.5, and filling it into a spray bottle to obtain the product.

[0027] The present invention also provides the use of the dandruff-removing herbal extract or the spray in the preparation of scalp care products for improving dandruff and / or scalp itching.

[0028] In this invention, the scalp care products include, but are not limited to, dry shampoo sprays, scalp serums, scalp care solutions, and scalp ointments.

[0029] The present invention also provides a topical pharmaceutical composition prepared from the following components in parts by weight:

[0030] Chrysanthemum 5-30 parts, honeysuckle 5-30 parts, blue hosta and gentian 2-20 parts, smilax glabra 5-40 parts, perilla 2-20 parts.

[0031] In this invention:

[0032] The principal herbs are chrysanthemum and honeysuckle, which clear heat and detoxify, dispel wind and heat, and directly relieve heat stagnation in the scalp.

[0033] Assistant herbs: Gentiana scabra, Gentiana scabra, clear heat and dry dampness, assisting the principal herbs in clearing away damp-heat pathogens;

[0034] Adjuvant herb: Smilax glabra, which detoxifies and removes dampness, and also promotes urination;

[0035] The guiding herb is Perilla frutescens, which regulates Qi and nourishes the blood, guides the medicine upwards, and harmonizes the effects of other herbs.

[0036] The term "direct treatment" refers to using cold-natured medicines to directly clear away heat pathogens, much like extinguishing a flame with cold water—a direct treatment method of "treating heat with cold." Chrysanthemum and honeysuckle are used as the principal herbs, their cold properties directly clearing away accumulated heat pathogens in the scalp.

[0037] The present invention has the following beneficial effects:

[0038] (1) This invention uses a compound of five Chinese herbal medicines: chrysanthemum, honeysuckle, blue gentian, smilax, and perilla. It works synergistically from multiple dimensions, including antibacterial, anti-inflammatory, antipruritic, and conditioning of the scalp microenvironment. In vitro antibacterial experiments showed that the MIC value against Malassezia reached 2 mg / mL, which was significantly better than the water extract group (8 mg / mL) and the water extract + alcohol precipitation group (4 mg / mL). Human efficacy verification showed that the dandruff score and pruritus VAS score decreased significantly after use, and it has a good dandruff removal and itch relief effect.

[0039] (2) The present invention significantly reduces the content of pigments and macromolecular impurities in the extract through the preparation process of "water extraction-alcohol precipitation-macroporous resin purification-concentration and drying", and obtains a Chinese herbal enrichment extract with low color and low viscosity. It effectively solves the engineering problems of traditional Chinese herbal extracts being easy to clog nozzles, precipitation during storage, and excessive color when used in no-rinse sprays, and improves the manufacturability and shelf stability of no-rinse sprays.

[0040] (3) The present invention combines the above-mentioned Chinese herbal enrichment extract with chlorhexidine acetate to form an antiseptic and antibacterial system suitable for residence-type products. It can provide effective antibacterial support at a low dosage. At the same time, the purification process reduces the impurity load, significantly improving the stability and safety of the preparation. Moreover, the preparation process facilitates the establishment of quality control indicators and is suitable for industrial scale-up. Attached Figure Description

[0041] Figure 1 Comparison of the appearance of the enriched extracts of traditional Chinese medicine prepared in Comparative Examples 1 and 2 with those prepared in Example 1;

[0042] Figure 2 Comparison of the antibacterial effects of each example and comparative example against Malassezia (1: blank control; 2: positive control; 3: comparative example 1; 4: comparative example 2; 5: example 1).

[0043] Figure 3 Comparison photos of the scalp before and after using the no-rinse spray of this invention in typical cases (left image is before use, right image is after use). Detailed Implementation

[0044] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to embodiments. It should be understood that the specific embodiments described herein are merely illustrative and not intended to limit the invention. All features disclosed in this specification, or steps in all disclosed methods or processes, except for mutually exclusive features and / or steps, can be combined in any way.

[0045] Unless otherwise defined, 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 pertains. The terminology used in this specification is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.

[0046] Example 1: Spray of water-extracted alcohol-precipitated resin-enriched extract

[0047] (1) Preparation of water-extracted, alcohol-precipitated, resin-enriched extract

[0048] Weigh out 20 parts by weight of chrysanthemum, 20 parts by weight of honeysuckle, 10 parts by weight of gentian root, 25 parts by weight of smilax glabra, and 10 parts by weight of perilla. Mix them and add 10 times the amount of water. Extract twice, combine the extracts, filter, concentrate the filtrate, add ethanol to a volume fraction of 70%, evaporate the ethanol, let stand for 24 hours, and centrifuge to collect the supernatant. Load the supernatant onto a macroporous adsorption resin column, first elute with water to remove hydrophilic impurities / some pigments and ineffective components, then elute with 70% ethanol, collect the ethanol eluent, and obtain the water-extracted, alcohol-precipitated, resin-enriched extract.

[0049] (2) Preparation of spray

[0050] Chlorhexidine acetate (0.18%–0.22% in the final solution) is added to the water-extracted, alcohol-precipitated, resin-enriched extract, the pH is adjusted to 4.5–6.5, and the extract is then filled into spray bottles.

[0051] Comparative Example 1: Ethanol Extract Spray

[0052] (1) Preparation of ethanol extract

[0053] Weigh out 20 parts of chrysanthemum, 20 parts of honeysuckle, 10 parts of gentian root, 25 parts of smilax glabra, and 10 parts of perilla according to the specified weight ratios. Add 8 times the amount of ethanol, extract twice, combine the extracts, filter, and obtain the ethanol extract.

[0054] (2) Preparation of spray

[0055] Add chlorhexidine acetate (0.18%–0.22% in the final solution) to the ethanol extract, adjust the pH to 4.5–6.5, and fill into spray bottles to obtain the final product.

[0056] Comparative Example 2: Water-extracted and alcohol-precipitated extract spray

[0057] (1) Water-extracted and alcohol-precipitated extract

[0058] Weigh out 20 parts of chrysanthemum, 20 parts of honeysuckle, 10 parts of gentian root, 25 parts of smilax glabra, and 10 parts of perilla according to the specified weight ratio. Add 10 times the amount of water, extract twice, combine the extracts, filter, concentrate the filtrate, precipitate with alcohol to an ethanol concentration of 70%, filter again, and take the supernatant to obtain the water-extracted alcohol-precipitated extract.

[0059] (2) Preparation of spray

[0060] Add chlorhexidine acetate (0.18%–0.22% in the final solution) to the water-extracted alcohol-precipitated extract, adjust the pH to 4.5–6.5, and fill into spray bottles to obtain the final product.

[0061] Experimental Example 1: Anti-Malassezia Activity Test

[0062] This experiment aimed to evaluate the in vitro inhibitory activity of enriched extracts of traditional Chinese medicine against Malassezia. The standard strain of Malassezia was used, and modified Dixon (mDixon) liquid medium was used. The culture conditions were 32℃. Ketoconazole was used as the positive control, and DMSO was used as the negative control. The results are shown in Table 1.

[0063] Table 1. MIC results against Malassezia

[0064]

[0065] From Table 1 and Figure 2 It can be seen that the Chinese herbal enrichment extract prepared in Example 1 of the present invention has a significant inhibitory effect on Malassezia, with a MIC value of 2 mg / mL, which is significantly lower than that of Comparative Example 1 (8 mg / mL) and Comparative Example 2 (4 mg / mL). This indicates that the extraction and purification process of the present invention effectively enriches the active ingredients and significantly improves the antibacterial effect.

[0066] Experimental Example 2

[0067] A randomized, controlled, parallel design was used to recruit 120 participants with mild to moderate dandruff, who were randomly assigned to an experimental group and a control group, with 60 participants in each group. The experimental group used the no-rinse spray prepared in the example, sprayed onto the scalp and gently massaged 1-2 times daily, without rinsing; the control group used a commercially available shampoo containing regular anti-dandruff ingredients. The trial lasted for 2 weeks. Dandruff scores (0-100 points, higher scores indicating more severe dandruff) and pruritus VAS scores (0-10 points, higher scores indicating more severe pruritus) were assessed before use, and at weeks 1 and 2 after use. Adverse reactions were also recorded.

[0068] Table 2 Evaluation results of dandruff and antipruritic efficacy

[0069]

[0070] As shown in Table 2, the initial dandruff scores of the experimental group and the control group were 87.5 and 88, respectively. The baseline levels of the two groups were basically the same and comparable. In terms of dandruff removal effect, the dandruff score of the spray group of the present invention gradually decreased after 3 days, 1 week and 2 weeks, which was significantly lower than that of the control group, showing a faster onset of action and a more thorough dandruff removal effect. In terms of antipruritic effect, it was also significantly better than the control group, indicating that its itch relief effect was more prominent. Overall, the spray of the present invention is significantly better than the control product in terms of dandruff removal and antipruritic efficacy.

[0071] Typical Case: Subject, male, 53 years old, with a 30-year history of dandruff, presenting with significant itching. Before use, his dandruff score was 87 and his VAS score for itching was 10. He used the no-rinse spray prepared in Example 2 twice daily, spraying it onto his scalp and gently massaging it in. On the third day of use, his dandruff score decreased to 35 and his VAS score for itching decreased to 2. No itching or other adverse reactions occurred during use. Scalp photos are available. Figure 3 .

[0072] The above description is merely a preferred embodiment of the present invention and is not intended to limit the invention. Various modifications and variations can be made to the present invention by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.

Claims

1. A method for preparing an enriched extract of traditional Chinese medicine for dandruff removal, characterized in that, The dandruff-removing herbal extract is prepared from the following raw materials: chrysanthemum, honeysuckle, gentian, smilax, and perilla; the preparation method includes: extracting the raw materials with water to obtain an aqueous extract; treating the aqueous extract with alcohol, loading the supernatant onto a macroporous adsorption resin column, eluting with water and ethanol solutions sequentially, collecting the ethanol eluent, concentrating and drying to obtain the final product.

2. The preparation method according to claim 1, characterized in that, The raw materials, by weight, are: 5-30 parts chrysanthemum, 5-30 parts honeysuckle, 2-20 parts gentian and blue hosta, 5-40 parts smilax glabra, and 2-20 parts perilla; further, the raw materials, by weight, are: 10-25 parts chrysanthemum, 10-25 parts honeysuckle, 5-15 parts gentian and blue hosta, 10-35 parts smilax glabra, and 5-15 parts perilla; even further, the raw materials, by weight, are: 20 parts chrysanthemum, 20 parts honeysuckle, 10 parts gentian and blue hosta, 25 parts smilax glabra, and 10 parts perilla.

3. The preparation method according to claim 1, characterized in that, The mass ratio of the raw material to water is 1:(6-20); further, the mass ratio of the raw material to water is 1:

10.

4. The preparation method according to claim 1, characterized in that, The volume fraction of the ethanol solution used for alcohol precipitation and / or elution is 60-90%; further, the volume fraction of the ethanol is 70%.

5. A concentrated extract of traditional Chinese medicine for dandruff removal, characterized in that, It is prepared by the preparation method according to any one of claims 1 to 5.

6. A no-rinse anti-dandruff spray, characterized in that, The no-rinse dandruff spray comprises the dandruff-removing herbal extract as described in claim 7.

7. The no-rinse dandruff spray according to claim 6, characterized in that, In the no-rinse anti-dandruff spray, the amount of the anti-dandruff herbal extract added is 0.05-5.0 wt% by weight of the finished product; further, the no-rinse anti-dandruff spray also includes chlorhexidine acetate; even further, the amount of chlorhexidine acetate added is 0.02-0.30 wt%.

8. The no-rinse dandruff spray according to claim 6, characterized in that, The pH of the no-rinse dandruff spray is 4.5–6.

5.

9. The use of the dandruff-reducing herbal extract of claim 5 or the spray of any one of claims 6 to 9 in the preparation of a scalp care product for improving dandruff and / or scalp itching.

10. A topical pharmaceutical composition, characterized in that, It is prepared from the following components in parts by weight: Chrysanthemum 5-30 parts, honeysuckle 5-30 parts, gentian 2-20 parts, smilax glabra 5-40 parts, perilla 2-20 parts; further: Principal herbs: Chrysanthemum, Honeysuckle; The main ingredients: Blue Jade Hairpin and Gentian; Adjuvant herb: Smilax glabra; Used medicinal ingredient: Perilla frutescens.

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