A lotion for clearing heat and drying dampness, a preparation method and a quality control method

Abstract

The application provides a lotion for clearing heat and drying dampness, a preparation method and a quality control method, which are prepared from the following components in parts by weight: honeysuckle 5-500 parts, Chinese corktree 5-500 parts, pig linden 5-500 parts, poria cocos 5-500 parts, Chinese pricklyash 5-500 parts, Chinese senna 5-500 parts, gallnut 5-500 parts. The lotion is provided with strict compatibility of monarch, minister, assistant and messenger, can directly reach the lesion when used externally, can quickly relieve the itching symptoms, can regulate the damp-heat pathogenesis and reduce the recurrence. The total effective rate of the lotion on the damp-heat type anorectal diseases reaches more than 93%, and the incidence of adverse reactions is less than 1%.

Description

Technical Field

[0001] This invention belongs to the field of traditional Chinese medicine preparations, specifically relating to a heat-clearing and dampness-drying lotion, its preparation method, and its quality control method. Background Technology

[0002] Anorectal diseases (such as hemorrhoids, anal fissures, and perianal abscesses) are common and frequently occurring clinical conditions, often manifesting as redness, swelling, heat, pain, exudation, and itching. In traditional Chinese medicine (TCM) theory, they are often categorized under "damp-heat accumulation" and "blood stasis." Therefore, in clinical practice, TCM herbs with heat-clearing, dampness-drying, swelling-reducing, pain-relieving, blood-activating, and stasis-removing effects are frequently used for local fumigation and sitz baths. This therapy allows the medication to act directly on the affected area, resulting in rapid efficacy and high patient acceptance. It is an important component of external treatment methods in TCM surgery.

[0003] Chinese patent CN112121077A discloses a traditional Chinese medicine wash for treating hemorrhoids, as follows: Preparation method: (1) Raw material processing: Prunella vulgaris, dandelion, three needles and Sophora japonica are crushed into coarse powder.

[0004] (2) Extraction: Boil the above coarse powder twice with water. The amount of water added each time is 10-11 times the total weight of the dry medicinal materials, and the boiling time each time is 1-1.5 hours.

[0005] (3) Concentration: Combine the filtrates from the two decoctions and concentrate them until the concentration of the concentrate reaches 1-1.5g of raw medicinal material per 1mL.

[0006] (4) Preparation: Add sodium benzoate to the concentrate as a preservative, and the amount added is 0.4-0.6% of the weight of the concentrate.

[0007] (5) Filtration and dilution: The above solution is filtered by pressure, and then diluted with distilled water of the same weight as the concentrate.

[0008] (6) Packaging: Mix the diluted medicine solution evenly and then package it to obtain the finished Chinese medicine wash.

[0009] Quality control methods: Indirect control of the final product quality is achieved by controlling the quality of the concentrate, a key intermediate in the preparation process. This involves controlling the relative density or concentration of the concentrate (i.e., "1-1.5g of raw drug per mL"). However, this single quality control method is insufficient to guarantee the product's efficacy or quality.

[0010] In hospital clinical practice, proven and effective in-house formulas, validated through long-term clinical trials, are based on classic prescriptions and adapted by departmental experts based on their clinical experience. Currently, the application model for these formulas is as follows: after a doctor prescribes the medicine, the hospital's decoction room uses traditional methods to boil the medicinal herbs with water, filters the liquid, and then mechanically packages it into disposable plastic bags or bottles for patients. Patients need to heat the liquid for fumigation or sitz baths.

[0011] While this model can meet basic clinical needs, it is essentially a rudimentary service model of "prescribing medicine according to prescription," and has obvious limitations: Primary form of preparation: The product is a liquid decoction with high water content, large volume and weight, and simple packaging, which is inconvenient for patients (especially those who need to travel for business or leisure) to carry and transport.

[0012] Poor stability: The decoction is rich in nutrients such as sugars and proteins, making it extremely susceptible to mold and fermentation. It has a very short shelf life (usually 3-14 days under refrigeration) and requires strict storage conditions, which limits the distribution and use of the medicine.

[0013] Inconsistent quality: The preparation of medicines in hospital decoction rooms follows a "front shop, back factory" model. The decoction process is greatly affected by human and objective factors such as batches of medicinal materials, decoction time, heat, water volume, and differences in decoction equipment. This makes it difficult to maintain consistent quality attributes such as the content of effective ingredients and clarity between different batches, and even different bags of the same batch. The stability and reproducibility of clinical efficacy cannot be scientifically guaranteed. At the same time, the lack of systematic and quantifiable quality control methods makes it difficult to effectively monitor and evaluate the quality of the finished product. Unable to be industrialized: This model relies heavily on manual or semi-mechanized operations in hospital decoction rooms, resulting in low production efficiency and high costs. It cannot achieve standardized and large-scale commercial production, which greatly limits the promotion, application, and market value transformation of this effective prescription.

[0014] Against this backdrop, developing clinically effective hospital prescriptions into modern external Chinese medicine preparations that are stable in quality, easy to use, convenient to store and transport, and industrialized has become a technical problem with clear clinical demand. Summary of the Invention

[0015] This invention provides a heat-clearing and dampness-drying lotion for treating external hemorrhoids, mixed hemorrhoids, prolapsed and incarcerated internal hemorrhoids, anal fissures, perianal abscesses, and acute exacerbations of anal fistulas, with significant clinical efficacy. This lotion is convenient to use, storage-stable, quality-controllable, and suitable for industrial production. A matching preparation process and quality control method have been established to ensure its quality uniformity and effectiveness.

[0016] A heat-clearing and dampness-drying wash is prepared from the following components in parts by weight: honeysuckle 5-500 parts, phellodendron bark 5-500 parts, polyporus umbellatus 5-500 parts, poria cocos 5-500 parts, and Sichuan pepper 5-500 parts.

[0017] With Phellodendron bark as the core ingredient, it is combined with honeysuckle to clear heat and detoxify, and disperse wind-heat, which helps Phellodendron bark to enhance its heat-clearing and detoxifying power and prevent heat toxins from accumulating on the skin and causing sores. Polyporus umbellatus and Poria cocos promote diuresis and eliminate dampness, and strengthen the spleen and replenish qi. The two complement each other and can not only drain damp-heat in the lower jiao, but also strengthen the spleen to eliminate the source of dampness, thus treating both the symptoms and the root cause. Sichuan pepper dispels wind, kills parasites, dries dampness and relieves itching. Its pungent and warm properties can restrain the bitter and cold nature of Phellodendron bark and honeysuckle, and prevent cold and dampness from damaging the spleen.

[0018] Furthermore, a heat-clearing and dampness-drying wash is prepared from the following components in parts by weight: honeysuckle 5-500 parts, phellodendron bark 5-500 parts, polyporus umbellatus 5-500 parts, poria cocos 5-500 parts, Sichuan pepper 5-500 parts, and soapberry thorns 5-500 parts.

[0019] Further research revealed that adding soapberry thorns to reduce swelling and promote detoxification, and to penetrate the meridians, can guide the medicinal power directly to the affected area, enhance the clearing effect on deep damp toxins, and solve the problem of poor local ventilation and difficulty in healing in some damp-heat type anorectal diseases.

[0020] Furthermore, a heat-clearing and dampness-drying wash is prepared from the following components in parts by weight: honeysuckle 5-500 parts, phellodendron bark 5-500 parts, polyporus umbellatus 5-500 parts, poria cocos 5-500 parts, Sichuan pepper 5-500 parts, soapberry thorns 5-500 parts, and gallnut 5-500 parts.

[0021] Further research revealed that gallnut has a sour and astringent taste, is cold in nature, and enters the lung, large intestine, and kidney meridians. It has astringent and consolidating properties, can heal sores and relieve itching, and is effective in treating skin oozing and itching that is difficult to cure, as it astringes without leaving any pathogens.

[0022] In some embodiments of the present invention, a heat-clearing and dampness-drying wash is prepared from the following components in parts by weight: 10-300 parts honeysuckle, 10-300 parts phellodendron bark, 10-300 parts polyporus umbellatus, 10-300 parts poria cocos, 10-300 parts Sichuan pepper, 10-300 parts soapberry thorns, and 10-300 parts gallnut.

[0023] In some embodiments of the present invention, a heat-clearing and dampness-drying wash is prepared from the following components in parts by weight: 30-200 parts of honeysuckle, 30-200 parts of phellodendron bark, 30-200 parts of polyporus umbellatus, 30-200 parts of poria cocos, 30-200 parts of Sichuan pepper, 30-200 parts of soapberry thorns, and 30-200 parts of gallnut.

[0024] In some embodiments of the present invention, a heat-clearing and dampness-drying wash is prepared from the following components in parts by weight: 30-100 parts of honeysuckle, 30-100 parts of phellodendron bark, 30-100 parts of polyporus umbellatus, 30-100 parts of poria cocos, 30-100 parts of Sichuan pepper, 30-100 parts of soapberry thorns, and 30-100 parts of gallnut.

[0025] In some embodiments of the present invention, a heat-clearing and dampness-drying wash is prepared from the following components in parts by weight: 40-80 parts of honeysuckle, 40-80 parts of phellodendron bark, 40-80 parts of poria cocos, 40-80 parts of poria cocos, 40-80 parts of Sichuan pepper, 40-80 parts of soapberry thorns, and 40-80 parts of gallnut.

[0026] In some embodiments of the present invention, a heat-clearing and dampness-drying wash is prepared from the following components in parts by weight: 50 parts honeysuckle, 50 parts phellodendron bark, 50 parts polyporus umbellatus, 50 parts poria cocos, 50 parts Sichuan pepper, 50 parts soapberry thorns, and 50 parts gallnut.

[0027] Phellodendron bark: It is cold in nature and bitter in taste, and mainly contains alkaloids such as berberine and phellodendron alkaloid. Modern pharmacological studies show that it has significant anti-inflammatory, antibacterial and anti-allergic effects. Berberine can inhibit the release of inflammatory factors such as TNF-α and IL-6, and has a strong inhibitory effect on pathogenic bacteria such as Staphylococcus aureus and Candida albicans.

[0028] Honeysuckle: It is cold in nature and sweet in taste. It mainly contains chlorogenic acid, luteolin and other components, which have anti-inflammatory, antibacterial and antiviral effects. Chlorogenic acid can reduce skin inflammation, inhibit the release of sensitizing substances and relieve itching symptoms.

[0029] Polyporus umbellatus and Poria cocos: Both contain polysaccharide components. Polyporus umbellatus polysaccharide and Poria cocos polysaccharide have the effects of regulating immunity and promoting diuresis and dampness removal. They can improve skin microcirculation, reduce tissue fluid exudation, and enhance the body's ability to clear pathogens.

[0030] Sichuan pepper: It is warm in nature and pungent in taste. It mainly contains volatile oil, alkaloids and other components, and has antibacterial, insecticidal and antipruritic effects. Its volatile oil can inhibit the growth of dermatophytes, relieve local itching, and promote local blood circulation and improve the skin's nutritional status.

[0031] Gleditsia sinensis thorns: warm in nature and pungent in taste, mainly containing flavonoids and triterpenoids, with anti-inflammatory, antibacterial and immunomodulatory effects, can enhance the transdermal absorption of drugs, help clear deep damp toxins, and have good efficacy for sores, carbuncles and skin diseases.

[0032] Gallnut: It is cold in nature and sour and astringent in taste. It mainly contains tannins, gallic acid and other components. It has astringent, antibacterial and anti-inflammatory effects, which can reduce skin exudation, promote wound healing, inhibit various pathogens, and relieve itching symptoms.

[0033] This lotion uses Phellodendron bark as the core ingredient for clearing heat and drying dampness, and honeysuckle is added to enhance its detoxifying power, inspired by the Huanglian Jiedu Decoction in "Collection of Experiences in Ulcer Treatment". It follows the method of Wuling Powder in "Treatise on Febrile Diseases" to promote diuresis and eliminate dampness, and is optimized by combining the clinical experience of modern proctologist Gao Yuehong.

[0034] The principal herb: Phellodendron bark is bitter and cold in nature, entering the kidney, bladder, and large intestine meridians. It excels at clearing heat and drying dampness, purging fire and detoxifying, especially effective in clearing damp-heat in the lower burner. The *Compendium of Materia Medica* states that it "treats hematochezia, dysentery, various types of weakness and paralysis, and eliminates damp-heat in the lower burner," making it an essential herb for treating anorectal and genital diseases caused by damp-heat. Honeysuckle is sweet and cold in nature, entering the lung, heart, and stomach meridians. It clears heat and detoxifies, disperses wind-heat, and assists Phellodendron bark in enhancing its heat-clearing and detoxifying power, preventing the accumulation of heat toxins on the skin and the formation of sores.

[0035] The assistant herbs are: Polyporus umbellatus and Poria cocos. They are sweet and bland in taste, neutral in nature, and enter the spleen, kidney, and bladder meridians. They promote diuresis and eliminate dampness, strengthen the spleen and replenish qi. The two herbs complement each other and can both drain damp heat in the lower jiao and strengthen the spleen to eliminate the source of dampness, thus treating both the symptoms and the root cause.

[0036] The adjuvant herbs are: Sichuan pepper, which is pungent and warm in nature, and enters the spleen, stomach and kidney meridians. It dispels wind, kills parasites, dries dampness and relieves itching. Its pungent and warm nature can restrain the bitter and cold nature of Phellodendron bark and honeysuckle, and prevent cold and dampness from damaging the spleen; Gleditsia sinensis thorns, which are pungent and warm in nature, enter the liver and stomach meridians. They reduce swelling and promote detoxification, penetrate the meridians, and can guide the medicinal power directly to the disease site, enhancing the effect of clearing deep damp toxins. The herb used is gallnut, which has a sour and astringent taste and is cold in nature. It enters the lung, large intestine, and kidney meridians. It has astringent and consolidating properties, and can help heal sores and stop itching. It is effective for skin oozing and itching that is difficult to cure, as it astringes without leaving any pathogens.

[0037] Secondly, the present invention provides a customized and optimized process for preparing the above-mentioned lotion, optimizing the extraction process parameters to maximize the extraction and retention of multiple effective components in the formula, thereby improving extraction efficiency and product yield.

[0038] A method for preparing a heat-clearing and dampness-drying wash includes the following steps: Step 1: Add 8-12 times the amount of water to the remaining ingredients except for the Sichuan peppercorns and simmer for 0.5-4 hours. Add the Sichuan peppercorns 0.1-0.5 hours before the end of the simmering process. Step 2: Add Sichuan peppercorns and simmer for 0.1 to 0.5 hours, then filter and separate to obtain herbal extract 1 and herbal residue 1; Step 3: Add 6-10 times the amount of water to the dregs 1 and decoct for 0.5-4 hours. Filter and separate to obtain the herbal extract 2. Step 4: Combine herbal extract 1 and herbal extract 2, concentrate under reduced pressure, add preservative, stir to dissolve and mix well, adjust the volume of the liquid to 1000ml, filter, and dispense to obtain the final product.

[0039] In some embodiments of the present invention, in step 1, 9-11 times the amount of water is added and decocted for 0.8-3 hours, preferably 10 times the amount of water is added and decocted for 1-2 hours, more preferably 10 times the amount of water is added and decocted for 1.5 hours.

[0040] In some embodiments of the present invention, in step 1, Sichuan peppercorns are added 0.3 to 0.4 hours before the end of simmering; preferably, Sichuan peppercorns are added 20 minutes before the end of simmering.

[0041] In some embodiments of the present invention, in step 2, Sichuan peppercorns are added and then simmered for 0.3 to 0.4 hours; preferably, Sichuan peppercorns are added and then simmered for 20 minutes.

[0042] In some embodiments of the present invention, in step 3, 7-9 times the amount of water is added to the dregs 1 and decocted for 0.8-3 hours, preferably 8 times the amount of water is added to the dregs 1 and decocted for 1-2 hours, more preferably 8 times the amount of water is added to the dregs 1 and decocted for 1.5 hours.

[0043] The preservative is selected from one or more preservatives such as potassium sorbate, sodium benzoate, and parabens.

[0044] Thirdly, this invention provides a precise, comprehensive, and quantifiable quality control method for the aforementioned lotion, enabling direct and precise control of the content of key active pharmaceutical ingredients in the prescription and achieving qualitative determination of multiple components. By setting clear content limits, the chemical equivalence of each batch of product is ensured, thereby guaranteeing the stability and reliability of clinical efficacy.

[0045] A quality control method for a heat-clearing and drying lotion, characterized in that the method includes HPLC determination and TLC determination.

[0046] The TLC determination method includes one or more of the following: Phellodendron bark qualitative determination method, Gallnut qualitative determination method, and Gleditsia sinensis thorn qualitative determination method.

[0047] The qualitative determination method for Phellodendron amurense includes the following steps: Take 5 ml of sample, add 30 ml of 1% acetic acid methanol, shake well, filter, evaporate the filtrate to dryness, dissolve the residue in 2 ml of 1% acetic acid methanol to obtain the test solution. Separately, take 0.1 g of Phellodendron amurense reference material, add 20 ml of 1% acetic acid methanol, sonicate for 20 minutes, filter, evaporate the filtrate to dryness, dissolve the residue in 2 ml of 1% acetic acid methanol to obtain the reference material solution. Take 2-4 μl of each of the above two solutions and spot them separately on the same silica gel G thin-layer plate. Use toluene-ethyl acetate-isopropanol-methanol-water (6:3:1.5:1.5:0.3) as the developing solvent, place in a developing tank saturated with ammonia vapor, develop, remove, air dry, and examine under ultraviolet light at 365 nm. In the chromatogram of the test sample, a fluorescent main spot of the same color should appear at the corresponding position as in the chromatogram of the reference material.

[0048] The qualitative determination method for gallnut includes the following steps: Take 10 ml of the sample, add 25 ml of 50% methanol solution containing 10% hydrochloric acid, heat under reflux for 2 hours, cool, filter, and extract the filtrate twice with 20 ml of hydrochloric acid-saturated ether each time. Combine the ether extracts, evaporate to dryness, and dissolve the residue in 1 ml of methanol to obtain the test solution. Separately, take 0.5 g of gallnut reference material and prepare a reference material solution using the same method. Apply 3-6 μl of each solution to the same silica gel GF plate. 254 On a thin-layer plate, toluene (saturated with water)-ethyl acetate-formic acid (6:3:1) was used as the developing solvent. The plate was then removed, dried, and examined under ultraviolet light at 254 nm. The test sample chromatogram showed a fluorescent main spot of the same color at the corresponding position as the reference medicinal material chromatogram.

[0049] The qualitative determination method for Gleditsia sinensis thorns includes the following steps: Take 20 ml of this product, extract twice with 15 ml of ethyl acetate each time, combine the ethyl acetate solutions, evaporate to dryness, dissolve the residue in 1 ml of methanol to obtain the test solution. Separately, take 1 g of Gleditsia sinensis thorns reference material, add 15 ml of methanol, sonicate for 30 minutes, filter, evaporate the filtrate to dryness, dissolve the residue in 10 ml of water, add 15 ml of ethyl acetate, shake to extract, separate the ethyl acetate solution, evaporate to dryness, dissolve the residue in 1 ml of methanol to obtain the reference material solution. Take 4-8 μl of each solution and spot them separately on the same silica gel G thin-layer plate, develop with dichloromethane-methanol-concentrated ammonia (9:1:0.2) as the developing solvent, remove, air dry, and examine under ultraviolet light at 365 nm. In the chromatogram of the test sample, a fluorescent main spot of the same color appears at the corresponding position as in the chromatogram of the reference material.

[0050] The HPLC determination includes the method for determining the content of berberine hydrochloride.

[0051] The method for determining the content of berberine hydrochloride includes the following steps: Chromatographic conditions and system suitability test: Octadecylsilane-bonded silica gel was used as the stationary phase; acetonitrile-0.05 mol / L potassium dihydrogen phosphate solution (45:55) (0.4 g sodium dodecyl sulfate was added per 100 ml, and the pH was adjusted to 4.0 with phosphoric acid) was used as the mobile phase; the detection wavelength was 345 nm. Preferably, the theoretical plate number calculated based on the berberine hydrochloride peak should be no less than 5000.

[0052] To prepare the reference solution, accurately weigh an appropriate amount of berberine hydrochloride reference standard, add methanol to prepare a solution containing 40 μg per ml.

[0053] To prepare the test solution, take the sample, shake well, accurately pipette 10 ml into a 50 ml volumetric flask, add a methanol-hydrochloric acid (100:1) mixture to dilute, and bring the volume to the mark. Shake well, centrifuge, and take the supernatant to obtain the test solution.

[0054] The assay involves accurately injecting 10 μl each of the reference solution and the test solution into a liquid chromatograph and determining the concentration. Each ml of this product contains berberine hydrochloride (C...). 20 H 18 The amount of ClNO4 (calculated) shall not be less than 0.08 mg.

[0055] Technical effects of the present invention: (1) The lotion provided by this invention has a strict combination of principal, assistant, adjuvant, and guide herbs. When applied externally, it directly targets the affected area, quickly relieving itching symptoms while regulating the damp-heat pathogenesis and reducing recurrence. It has been verified that the overall effective rate for damp-heat type anorectal diseases is over 93%, and the incidence of adverse reactions is <1%.

[0056] (2) This invention provides a traditional Chinese medicine external wash. At the process level, a standardized, scalable, and industrializable preparation process is designed to replace the traditional manual decoction. At the dosage form and stability level, through process optimization and pharmacological research, the prescription is transformed into a wash dosage form with smaller volume, significantly improved stability, and easy portability and storage. At the quality controllability level, a scientific, systematic, and quantifiable quality control method is established to ensure high batch-to-batch quality uniformity and stable and reliable efficacy. Ultimately, the hospital clinical prescription is successfully transformed into a new traditional Chinese medicine product that meets modern pharmaceutical standards and has market competitiveness. Detailed Implementation

[0057] This invention discloses a heat-clearing and dampness-drying lotion, its preparation method, and its quality control method. Those skilled in the art can refer to the content of this invention and, in conjunction with the relevant principles of traditional Chinese medicine, pharmaceutical preparations, and pharmaceutical analysis, appropriately modify the process parameters to achieve the desired result. It is particularly important to note that all similar substitutions and modifications are obvious to those skilled in the art and are considered to be included within the scope of this invention. The application of this invention has been described through preferred embodiments, and those skilled in the art can clearly modify or appropriately change and combine the methods and applications described herein without departing from the content, spirit, and scope of this invention to realize and apply the technology of this invention.

[0058] To better understand the invention and not to limit its scope, all figures indicating amounts, percentages, and other numerical values ​​used in this application should, in all cases, be understood to be modified by the word "approximately." Each numerical parameter should at least be considered as obtained based on reported significant figures and through conventional rounding methods.

[0059] The present invention will be further illustrated by the following examples, but the examples do not limit the present invention in any way.

[0060] Example 1: A lotion for clearing heat and drying dampness Ingredients: 50g honeysuckle, 50g phellodendron bark, 50g polyporus umbellatus, 50g poria cocos, 50g Sichuan pepper, 50g gleditsia sinensis thorns, 50g gallnut.

[0061] Preparation method: Step 1: Add 10 times the amount of water to the remaining ingredients except for the Sichuan peppercorns and simmer for 1.5 hours. Add the Sichuan peppercorns 20 minutes before the end of the simmering process. Step 2: Add Sichuan peppercorns and simmer for another 20 minutes, then filter and separate to obtain herbal extract 1 and herbal residue 1; Step 3: Add 8 times the amount of water to the dregs 1 and decoct for 1.5 hours. Filter and separate to obtain medicinal extract 2. Step 4: Combine herbal extract 1 and herbal extract 2, concentrate under reduced pressure, add 1g of potassium sorbate, stir to dissolve and mix well, adjust the volume of the liquid to 1000ml, filter, and dispense into bottles, 100ml per bottle, to obtain the wash.

[0062] Qualitative determination of Phellodendron bark: Take 5 ml of the prepared lotion, add 30 ml of 1% acetic acid methanol, shake well, filter, evaporate the filtrate to dryness, dissolve the residue in 2 ml of 1% acetic acid methanol to obtain the test solution. Separately, take 0.1 g of Phellodendron bark reference material, add 20 ml of 1% acetic acid methanol, sonicate for 20 minutes, filter, evaporate the filtrate to dryness, dissolve the residue in 2 ml of 1% acetic acid methanol to obtain the reference material solution. Take 2-4 μl of each of the above two solutions and spot them separately on the same silica gel G thin-layer plate. Use toluene-ethyl acetate-isopropanol-methanol-water (6:3:1.5:1.5:0.3) as the developing solvent, place in a developing tank saturated with ammonia vapor, develop, remove, air dry, and examine under ultraviolet light at 365 nm. In the chromatogram of the test sample, a fluorescent main spot of the same color appears at the corresponding position as in the chromatogram of the reference material.

[0063] Qualitative determination of Gallnut: Take 10 ml of the prepared lotion, add 25 ml of 50% methanol solution of 10% hydrochloric acid, heat under reflux for 2 hours, cool, filter, and extract the filtrate twice with 20 ml of hydrochloric acid-saturated ether each time. Combine the ether extracts, evaporate to dryness, and dissolve the residue in 1 ml of methanol to obtain the test solution. Separately, take 0.5 g of Gallnut reference material and prepare a reference material solution using the same method. Apply 3-6 μl of each solution to the same silica gel GF254 thin-layer plate, develop using toluene (water-saturated)-ethyl acetate-formic acid (6:3:1) as the developing solvent, remove, air dry, and examine under ultraviolet light at 254 nm. In the chromatogram of the test sample, a fluorescent main spot of the same color appears at the corresponding position as in the chromatogram of the reference material.

[0064] Qualitative determination of Gleditsia sinensis thorns: Take 20 ml of the prepared lotion, extract twice with 15 ml of ethyl acetate each time, combine the ethyl acetate solutions, evaporate to dryness, dissolve the residue in 1 ml of methanol to obtain the test solution. Separately, take 1 g of Gleditsia sinensis thorns reference material, add 15 ml of methanol, sonicate for 30 minutes, filter, evaporate the filtrate to dryness, dissolve the residue in 10 ml of water, add 15 ml of ethyl acetate, shake and extract, separate the ethyl acetate solution, evaporate to dryness, dissolve the residue in 1 ml of methanol to obtain the reference material solution. Take 4-8 μl of each solution and spot them separately on the same silica gel G thin-layer plate, develop with dichloromethane-methanol-concentrated ammonia (9:1:0.2) as the developing solvent, remove, air dry, and examine under ultraviolet light at 365 nm. In the chromatogram of the test sample, a fluorescent main spot of the same color appears at the corresponding position as in the chromatogram of the reference material.

[0065] Method for determining berberine hydrochloride content: Chromatographic conditions and system suitability test: Octadecylsilane-bonded silica gel was used as the stationary phase; acetonitrile-0.05 mol / L potassium dihydrogen phosphate solution (45:55) (0.4 g sodium dodecyl sulfate was added per 100 ml, and the pH was adjusted to 4.0 with phosphoric acid) was used as the mobile phase; the detection wavelength was 345 nm. The theoretical plate number, calculated based on the berberine hydrochloride peak, should not be less than 5000.

[0066] To prepare the reference solution, accurately weigh an appropriate amount of berberine hydrochloride reference standard, add methanol to prepare a solution containing 40 μg per ml.

[0067] To prepare the test solution, take the sample, shake well, accurately pipette 10 ml into a 50 ml volumetric flask, add a methanol-hydrochloric acid (100:1) mixture to dilute, and bring the volume to the mark. Shake well, centrifuge, and take the supernatant to obtain the test solution.

[0068] The assay involves accurately injecting 10 μl each of the reference solution and the test solution into a liquid chromatograph and determining the concentration. Each ml of this product contains berberine hydrochloride (C...). 20 H 18 The result, calculated as ClNO4, was 0.11 mg.

[0069] Example 2: A lotion for clearing heat and drying dampness Ingredients: 50g honeysuckle, 50g phellodendron bark, 50g polyporus, 50g poria cocos, 50g Sichuan pepper.

[0070] Preparation method: Same as in Example 1.

[0071] Qualitative determination of Phellodendron bark: Same as in Example 1, showing the same color fluorescent main spot.

[0072] Berberine hydrochloride content determination method: Same as in Example 1, each 1 ml of Phellodendron bark contains berberine hydrochloride (C20 H 18 The result, calculated as ClNO4, was 0.11 mg.

[0073] Example 3: A lotion for clearing heat and drying dampness Ingredients: 50g honeysuckle, 50g phellodendron bark, 50g polyporus umbellatus, 50g poria cocos, 50g Sichuan pepper, 50g soapberry thorns.

[0074] Preparation method: Same as in Example 1.

[0075] Qualitative determination of Phellodendron bark: Same as in Example 1, showing the same color fluorescent main spot.

[0076] Qualitative determination of soapberry thorns: Same as in Example 1, showing fluorescent main spots of the same color.

[0077] Berberine hydrochloride content determination method: Same as in Example 1, each 1 ml of Phellodendron bark contains berberine hydrochloride (C 20 H 18 The result, calculated as ClNO4, was 0.11 mg.

[0078] Example 4: A lotion for clearing heat and drying dampness Ingredients: Honeysuckle 60g, Phellodendron bark 60g, Polyporus umbellatus 60g, Poria cocos 60g, Sichuan pepper 60g, Gleditsia sinensis thorns 40g, Gallnut 40g.

[0079] Preparation method: Same as in Example 1.

[0080] Qualitative determination of Phellodendron bark: Same as in Example 1, showing the same color fluorescent main spot.

[0081] Qualitative determination of soapberry thorns: Same as in Example 1, showing fluorescent main spots of the same color.

[0082] Qualitative determination of gallnut: Same as in Example 1, showing the same color fluorescent main spot.

[0083] Berberine hydrochloride content determination method: Same as in Example 1, each 1 ml of Phellodendron bark contains berberine hydrochloride (C 20 H 18 The concentration of ClNO4 was 0.14 mg.

[0084] Comparative Examples 1-4: Washes for clearing heat and drying dampness Comparative Example 1: Honeysuckle 50g, Polyporus umbellatus 50g, Poria cocos 50g, Sichuan pepper 50g, Gleditsia sinensis thorns 50g, Gallnut 50g Comparative Example 2: 50g each of Phellodendron bark, Polyporus umbellatus, Poria cocos, Zanthoxylum bungeanum, Gleditsia sinensis thorns, and Galla chinensis. Comparative Example 3: Honeysuckle 50g, Phellodendron bark 50g, Sichuan pepper 50g, Gleditsia sinensis thorns 50g, Gallnut 50g Comparative Example 4 Components: Honeysuckle 50g, Phellodendron bark 50g, Polyporus umbellatus 50g, Poria cocos 50g, Gallnut 50g Preparation method of Comparative Examples 1-3: Same as Example 1; The preparation method of Comparative Example 4 is as follows: Step 1: Take all components, add 10 times the amount of water and decoct for 2.0 hours, filter and separate to obtain medicinal extract 1 and dregs 1; Step 2: Add 8 times the amount of water to the dregs 1 and decoct for 1.5 hours. Filter and separate to obtain medicinal extract 2. Step 3: Combine herbal extract 1 and herbal extract 2, concentrate under reduced pressure, add 1g of potassium sorbate, stir to dissolve and mix well, adjust the volume of the liquid to 1000ml, filter, and dispense into bottles, 100ml per bottle, to obtain the wash.

[0085] Example 5: Effect Evaluation For patients with external hemorrhoids, mixed hemorrhoids, or acute prolapsed and incarcerated internal hemorrhoids, take one bottle twice a day for two weeks.

[0086] Efficacy evaluation criteria: Cure: No pain, swelling, or congestion around the anus; anal swelling and rectal bleeding disappear. Effective: The above symptoms are controlled and show significant improvement; Ineffective: Symptoms do not improve significantly, or even worsen.

[0087]

[0088] Typical Case 1 Ms. Liu, female, 24 years old, presented with a chief complaint of a perianal mass accompanied by pain for six months. The patient noticed the mass perianal without any obvious cause six months prior. The mass protruded during defecation, and became swollen and painful during diarrhea or constipation. She also experienced intermittent rectal bleeding, with small amounts of bright red blood appearing in the stool, in relatively large quantities. She had no feeling of pressure or tightness in the anus, no anal dampness, no itching, and no stool leakage. She typically had one bowel movement per day, the first part of which was dry, followed by a soft, formed stool without mucus or pus. The amount of stool was adequate, but defecation was difficult. She had previously used hemorrhoid suppositories, but her condition did not improve. The patient had poor sleep, a normal appetite, yellow urine, and constipation. Her tongue was dark with a yellow, greasy coating, and her pulse was slippery. Traditional Chinese medicine diagnosis indicated damp-heat accumulation in the lower jiao (lower burner). Treatment principle: clear heat and dry dampness.

[0089] The herbal wash prepared in Example 1 was administered once, one bottle (100ml) twice a day. After 7 days, the bleeding stopped, the hemorrhoids shrank, and the pain was relieved. Continued use for another 7 days resulted in no pain during bowel movements, the anal swelling disappeared, and sleep improved.

[0090] Typical Case 2 Mr. Wang, male, 19 years old, presented with a chief complaint of swelling, pain, and discomfort in the perianal region for 7 days. Seven days prior, the patient developed swelling and pain in the perianal region without any obvious cause. The swelling and pain were more pronounced during defecation or after prolonged squatting, accompanied by intermittent rectal bleeding, mostly bright red blood on toilet paper, in small amounts, and a foreign body sensation in the anus. There was no feeling of pressure or tightness in the anus, no anal dampness, no itching, and no leakage of stool. He typically had one bowel movement daily, with dry stool, no mucus or pus, and normal stool volume, but difficulty in defecation. His condition did not improve without treatment. The patient also experienced poor sleep, normal appetite, yellow urine, and constipation. His tongue was dark with a yellow, greasy coating, and his pulse was slippery. Traditional Chinese medicine diagnosis indicated damp-heat accumulation in the lower jiao (lower burner), and the treatment principle was to clear heat and dry dampness.

[0091] The herbal wash prepared in Example 1 was administered, one bottle at a time, twice a day. After 5 days, the bleeding stopped, the hemorrhoids shrank, and the pain was relieved. Continued use for another 5 days resulted in no pain during bowel movements, the anal swelling disappeared, and sleep improved.

[0092] Typical Case 3 Ms. Fan, 41 years old, presented with a chief complaint of a perianal mass four years prior. She reported noticing the mass approximately four years ago without any apparent cause. The mass protruded during bowel movements, making it difficult to clean the anus afterward. She experienced pain and discomfort after consuming spicy or irritating foods, intermittent rectal bleeding, blood on toilet paper, and in severe cases, small, bright red, copious amounts of blood. She reported no rectal pressure, dampness, itching, or leakage of stool. She typically had one bowel movement daily, with soft, formed stools, free of mucus and pus, and a normal stool volume. She experienced intermittent difficulty in defecation and occasional feelings of incomplete evacuation. She had previously treated with topical hemorrhoid cream, but her condition did not improve. She also reported poor sleep, normal appetite, yellow urine, and constipation. Her tongue was dark with a yellow, greasy coating, and her pulse was slippery. Traditional Chinese medicine diagnosis indicated damp-heat accumulation in the lower jiao (lower burner). Treatment principle: clear heat and dry dampness.

[0093] The herbal wash prepared in Example 1 was administered, one bottle at a time, twice a day. After 6 days, the rectal bleeding stopped, the hemorrhoids shrank, and the pain was relieved. Continued use for another 6 days resulted in no pain during bowel movements, the anal swelling disappeared, and sleep improved.

[0094] Typical Case 4 Ms. Li, 35 years old, presented with a one-year chief complaint of rectal prolapse accompanied by swelling during defecation or squatting. One year prior, without any obvious cause, she experienced multiple prolapsed masses in her anus during defecation or squatting. These masses required slow reduction after defecation. She experienced discomfort and swelling from the prolapsed masses, a foreign body sensation in the anus, a feeling of heaviness in the anus, and intermittent anal dampness. There was no anal itching, leakage of stool, or other bowel movements. She typically had one bowel movement daily, with soft, formed stools, no blood, mucus, or pus, and a normal stool volume without difficulty in defecation. She had previously used hemorrhoid suppositories, but her condition did not improve. She also experienced poor sleep, normal appetite, yellow urine, and constipation. Her tongue was dark with a yellow, greasy coating, and her pulse was slippery. Traditional Chinese medicine diagnosis indicated damp-heat accumulation in the lower jiao (lower burner). Treatment principle: clear heat and dry dampness.

[0095] The herbal wash prepared in Example 1 was administered, one bottle at a time, twice a day. After 10 days, the prolapsed hemorrhoids in the anus decreased in size, and the pain was relieved. Continued application for another 10 days resulted in no swelling of the prolapsed mass in the anus, no foreign body sensation in the anus, no feeling of heaviness in the anus, no anal dampness, and improved sleep.

[0096] Typical Case 5 Mr. Li, male, 37 years old, presented with a chief complaint of rectal prolapse accompanied by anal dampness during defecation for six months. The patient reported experiencing rectal prolapse without any obvious cause six months prior. The prolapsed mass would spontaneously reduce after defecation, but caused swelling and discomfort, intermittent rectal bleeding, and small, bright red, copious drops of stool during defecation. There was no feeling of fullness, dampness, itching, or leakage of stool from the anus. He typically had bowel movements once every two days, with dry stools, no mucus or pus, and moderate stool volume, but difficulty in defecation. He had previously used topical hemorrhoid cream without improvement. The patient also experienced poor sleep, normal appetite, yellow urine, and constipation. His tongue was dark with a yellow, greasy coating, and his pulse was slippery. Traditional Chinese medicine diagnosis indicated damp-heat accumulation in the lower jiao (lower burner), and the treatment principle was to clear heat and dry dampness.

[0097] The herbal wash prepared in Example 1 was administered, one bottle at a time, twice a day. After 7 days, the prolapsed mass inside the anus decreased in size and frequency, and the rectal bleeding stopped. Continued use for another 7 days resulted in a further reduction in the frequency of prolapsed mass inside the anus, no discomfort after the mass prolapsed, and improved sleep.

[0098] The detergent provided by this invention has an overall effectiveness of over 93%, with each component working synergistically, significantly better than comparative examples 1-4.

[0099] Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A heat-clearing and dampness-drying wash, prepared from the following components in parts by weight: honeysuckle 5-500 parts, phellodendron bark 5-500 parts, polyporus umbellatus 5-500 parts, poria cocos 5-500 parts, Sichuan pepper 5-500 parts, soapberry thorns 5-500 parts, gallnut 5-500 parts.

2. The heat-clearing and dampness-drying washing agent as described in claim 1, characterized in that, It was prepared from the following components by weight: honeysuckle 30-100 parts, phellodendron bark 30-100 parts, polyporus umbellatus 30-100 parts, poria cocos 30-100 parts, Sichuan pepper 30-100 parts, gleditsia sinensis thorns 30-100 parts, and gallnut 30-100 parts.

3. The heat-clearing and dampness-drying washing agent as described in claim 1, characterized in that, It was prepared from the following components by weight: 50 parts honeysuckle, 50 parts phellodendron bark, 50 parts polyporus umbellatus, 50 parts poria cocos, 50 parts Sichuan pepper, 50 parts gleditsia sinensis thorns, and 50 parts gallnut.

4. A method for preparing any one of the heat-clearing and drying washing agents as described in claims 1 to 3, comprising the following steps: Step 1: Add 8-12 times the amount of water to the remaining ingredients except for the Sichuan peppercorns and simmer for 0.5-4 hours. Add the Sichuan peppercorns 0.1-0.5 hours before the end of the simmering process. Step 2: Add Sichuan peppercorns and simmer for 0.1 to 0.5 hours, then filter and separate to obtain herbal extract 1 and herbal residue 1; Step 3: Add 6-10 times the amount of water to the dregs 1 and decoct for 0.5-4 hours. Filter and separate to obtain the herbal extract 2. Step 4: Combine herbal extract 1 and herbal extract 2, concentrate under reduced pressure, add preservative, stir to dissolve and mix well, adjust the volume of the liquid to 1000ml, filter, and dispense to obtain the final product.

5. A quality control method for any of the heat-clearing and drying washing agents as described in claims 1 to 3, characterized in that, The methods include HPLC determination and TLC determination.

6. The quality control method as described in claim 5, characterized in that, The TLC determination method includes one or more of the following: Phellodendron bark qualitative determination method, Gallnut qualitative determination method, and Gleditsia sinensis thorn qualitative determination method.

7. The quality control method as described in claim 6, characterized in that, The qualitative determination method for Phellodendron bark includes the following steps: Take 5 ml of sample, add 30 ml of 1% acetic acid methanol, shake well, filter, evaporate the filtrate to dryness, dissolve the residue in 2 ml of 1% acetic acid methanol to obtain the test solution; Take 0.1 g of Phellodendron bark reference material, add 20 ml of 1% acetic acid methanol, sonicate for 20 minutes, filter, evaporate the filtrate to dryness, dissolve the residue in 2 ml of 1% acetic acid methanol to obtain the reference material solution; Take 2-4 μl of each of the above two solutions and spot them separately on the same silica gel G thin-layer plate, using toluene-ethyl acetate-isopropanol-methanol-water (6:3:1.5:1.5:0.3) as the developing solvent, place in a developing tank saturated with ammonia vapor, develop, remove, air dry, and examine under ultraviolet light at 365 nm. In the chromatogram of the test sample, a fluorescent main spot of the same color should appear at the corresponding position as in the chromatogram of the reference material.

8. The quality control method as described in claim 6, characterized in that, The qualitative determination method for gallnut includes the following steps: Take 10 ml of the sample, add 25 ml of 50% methanol solution containing 10% hydrochloric acid, heat under reflux for 2 hours, cool, filter, and extract the filtrate twice with 20 ml of hydrochloric acid-saturated ether each time. Combine the ether extracts, evaporate to dryness, and dissolve the residue in 1 ml of methanol to obtain the test solution; separately, take 0.5 g of gallnut reference material and prepare a reference material solution using the same method; apply 3-6 μl of each of the two solutions separately to the same silica gel GF. 254 On a thin-layer plate, toluene (saturated with water)-ethyl acetate-formic acid (6:3:1) was used as the developing solvent. The plate was then removed, dried, and examined under ultraviolet light at 254 nm. The test sample chromatogram showed a fluorescent main spot of the same color at the corresponding position as the reference medicinal material chromatogram.

9. The quality control method as described in claim 6, characterized in that, The qualitative determination method for Gleditsia sinensis thorns includes the following steps: Take 20 ml of this product, extract twice with 15 ml of ethyl acetate each time, combine the ethyl acetate solutions, evaporate to dryness, dissolve the residue in 1 ml of methanol to obtain the test solution; Take 1 g of Gleditsia sinensis thorns reference material, add 15 ml of methanol, sonicate for 30 minutes, filter, evaporate the filtrate to dryness, dissolve the residue in 10 ml of water, add 15 ml of ethyl acetate, shake and extract, separate the ethyl acetate solution, evaporate to dryness, dissolve the residue in 1 ml of methanol to obtain the reference material solution; Take 4-8 μl of each of the two solutions and spot them separately on the same silica gel G thin-layer plate, develop with dichloromethane-methanol-concentrated ammonia (9:1:0.2) as the developing solvent, remove, air dry, and examine under ultraviolet light at 365 nm. In the chromatogram of the test sample, a fluorescent main spot of the same color appears at the corresponding position as in the chromatogram of the reference material.

10. The quality control method according to claim 5, wherein the HPLC determination includes the berberine hydrochloride content determination method; The method for determining the content of berberine hydrochloride includes the following steps: Chromatographic conditions and system suitability test: Octadecylsilane-bonded silica gel was used as the stationary phase; acetonitrile-0.05 mol / L potassium dihydrogen phosphate solution (45:55) (0.4 g sodium dodecyl sulfate was added per 100 ml, and the pH was adjusted to 4.0 with phosphoric acid) was used as the mobile phase; the detection wavelength was 345 nm; the theoretical plate number calculated based on the berberine hydrochloride peak should not be less than 5000; To prepare the reference solution, take an appropriate amount of berberine hydrochloride reference standard, accurately weigh it, and add methanol to prepare a solution containing 40 μg per ml. To prepare the test solution, take this product, shake well, accurately pipette 10 ml into a 50 ml volumetric flask, add a methanol-hydrochloric acid (100:1) mixture to dilute, and bring to volume. Shake well, centrifuge, and take the supernatant to obtain the test solution. Assay: Accurately pipette 10 μl each of the reference solution and the test solution into the liquid chromatograph and determine the concentration. The content of berberine hydrochloride (C) per 1 ml of this product is obtained. 20 H 18 The amount of ClNO4 (calculated) shall not be less than 0.08 mg.

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