Hemerocallis fulva preparation for inducing diuresis and treating stranguria and preparation method thereof
Through the combination of medicinal materials such as Yizhihuanghua and chitosan and mannan peptides, the problems of high loss rate of effective ingredients and poor antibacterial effects in the treatment of urinary tract infections have been solved, effectively inhibiting bacteria and relieving urinary tract inflammation of Gram-negative bacteria, and suitable for industrial production.
Patent Information
- Application Number
- CN202510573565.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-05-06
- Publication Date
- 2025-07-11
AI Technical Summary
In the treatment of urinary tract infection, existing traditional Chinese medicine preparations have problems such as high loss rate of active ingredient, short retention time of bladder mucosa, poor antibacterial effect on Gram-negative bacteria, and antibiotic resistance leads to poor treatment effect.
A yellow flower is used to combine verbena, white turtle root, plantain, gourd shell, white verbet, honeysuckle, Houttuynia cordata and other medicinal materials, combined with chitosan, mannan peptide and other ingredients, and through freeze-drying, dynamic countercurrent extraction and low-frequency ultrasonic treatment, a yellow flower preparation with broad-spectrum antibacterial effect is formed, extending the retention time of the active ingredient in urothelial cells.
It significantly improves the antibacterial effect on Gram-negative bacteria, reduces urinary tract mucosa inflammation, promotes Na+ excretion in the urine, relieves ureteral spasm, prolongs the efficacy of the drug, and is suitable for industrial production.
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Figure CN120285108A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of pharmaceutical preparations, and particularly relates to a Solidago virgaurea preparation for promoting diuresis and dredging strangury and a preparation method thereof. Background Art
[0002] Existing pets are prone to urinary tract infections due to external invasion of damp-heat, unclean lower genitals, invasion of filthy pathogenic factors from below, heat accumulating in the bladder, or improper diet, overeating fatty and thick foods, resulting in spleen dysfunction, dampness and heat accumulation, damp-heat pouring downward, and damp-heat accumulating in the bladder, leading to unfavorable bladder qi transformation.
[0003] Currently, the incidence of complicated urinary tract infections is increasing year by year, which is closely related to the abuse of antibiotics. The resistance rate of fluoroquinolones to Escherichia coli, the main pathogenic bacterium of urinary tract infections, has exceeded 60%. The third-generation cephalosporins (such as ceftriaxone) are still the first-line drugs for gonorrhea, but the resistance rate of Escherichia coli to them has increased significantly. The resistance rate of ceftriaxone to ESBL-producing Escherichia coli has increased from 5.3% in 2010 to 17.1% in 2023. Although traditional Chinese medicine has unique advantages in the treatment of urinary tract infections, experimental studies have confirmed that heat-clearing and detoxifying herbs such as honeysuckle and forsythia have a high in vitro antibacterial rate against Staphylococcus aureus (Gram-positive bacteria), but a low antibacterial effect against Neisseria gonorrhoeae (Gram-negative diplococcus). This difference is due to the low outer membrane permeability and high expression of the active efflux system of Neisseria gonorrhoeae.
[0004] At the same time, the traditional decoction process leads to a large loss of volatile antibacterial substances. Modern pharmacological research reveals that the traditional compatibility of Chinese herbs has a high loss rate of effective components due to the destruction of volatile antibacterial substances in the decoction process. Moreover, the existing preparations have a short retention time in the bladder mucosa and are difficult to penetrate the microcolony structure formed by pathogenic bacteria, resulting in unsatisfactory curative effects. Summary of the Invention
[0005] The purpose of the present invention is to solve the disadvantages existing in the prior art, and to provide a Solidago virgaurea preparation for promoting diuresis and dredging strangury and a preparation method thereof.
[0006] A Solidago virgaurea preparation for promoting diuresis and dredging strangury, characterized in that its raw materials by mass include: 500-600 parts of Solidago virgaurea, 50-150 parts of Verbena officinalis, 100-300 parts of Rhizoma Imperatae, 100-300 parts of Plantago asiatica, 50-200 parts of Fructus Lagenariae, 50-250 parts of Cynanchum glaucescens, 10-100 parts of honeysuckle, 10-100 parts of Houttuynia cordata, 10-20 parts of chitosan, 1-5 parts of sodium ascorbate, 5-15 parts of mannan oligosaccharide peptide, 10-20 parts of sodium benzoate, 1-10 parts of chondroitin sulfate, and 8000-12000 parts of water.
[0007] Preferably, the deacetylation degree of chitosan is 88-92%.
[0008] Preferably, in the mannan peptide, the mass percentage of the total sugar is 88-90%, and the mass percentage of the amino acid is 5-6%.
[0009] The preparation method of the above-mentioned yellow flower preparation for promoting diuresis and alleviating stranguria includes the following steps:
[0010] S1. Dissolve chitosan in the malic acid solution, add sodium ascorbate, and stir in the dark for 1-2 h to obtain pretreated chitosan.
[0011] S2. Crush and mix solidago virgaurea, verbena officinalis, rhizoma lmperatae, plantain herb, bottle gourd peel, cynanchum stauntonii, honeysuckle flower, and houttuynia cordata evenly, perform freeze-drying, then microwave-treat for 2-6 min, and perform liquid nitrogen freeze-crushing to obtain a premixed raw material; perform dynamic countercurrent extraction on the premixed raw material for 1-2 h; then perform pressurized extraction for 1-2 h, and perform pressure filtration to obtain an extract.
[0012] S4. Concentrate the extract under reduced pressure, add the pretreated chitosan and mannan peptide, stir at 40-50 °C for 10-30 min, add sodium benzoate, chondroitin sulfate, and water, adjust the pH value of the system to 5.8-6, and perform low-frequency ultrasonic treatment for 10-20 min.
[0013] Solidago virgaurea is yellow in color, has a delicate fragrance, is pungent and bitter in taste, and is of mild nature. It enters the liver and gallbladder meridians. It dispels wind and clears heat, reduces swelling and detoxicates. It is used to treat headache due to common cold, sore throat, jaundice, whooping cough, infantile convulsion, traumatic injury, carbuncle and sore back, and tinea manus.
[0014] Verbena officinalis is bitter in taste and of cool nature. It belongs to the liver and spleen meridians. It promotes blood circulation to remove stasis, arrests malaria, detoxifies, and promotes diuresis to alleviate edema. It is used for mass in the abdomen, amenorrhea and dysmenorrhea, malaria, sore throat, carbuncle and sore, edema, and stranguria with heat syndrome.
[0015] Rhizoma lmperatae is sweet in taste and of cold nature. It belongs to the stomach, lung, and bladder meridians. It cools blood for hemostasis, clears heat and promotes diuresis. It is used for hematemesis due to blood heat, epistaxis, hematuria, fever and restlessness due to febrile disease, jaundice, edema, stranguria with pain and heat syndrome; acute nephritis with edema.
[0016] Plantain herb is sweet in taste and of cold nature. It belongs to the liver, kidney, and bladder meridians. It clears heat and promotes diuresis, reduces phlegm, cools blood, and detoxifies. It is used for oliguria with edema, stranguria with pain and heat syndrome, diarrhea due to summer heat and dampness, cough with phlegm-heat, hematemesis and epistaxis, carbuncle and sore.
[0017] Bottle gourd peel is sweet in taste and of mild nature. It belongs to the heart and small intestine meridians. It promotes diuresis to alleviate edema. It is used for edema and ascites, swelling and pain of beriberi, etc.
[0018] Cynanchum stauntonii is pungent and sweet in taste and of warm nature. It belongs to the lung meridian. It lowers qi, eliminates phlegm, and relieves cough. It is used for excessive qi in the lung, profuse sputum, cough, chest fullness and dyspnea.
[0019] Honeysuckle flower is sweet in taste and of cold nature. It belongs to the stomach and lung meridians. It clears heat and detoxifies. It is mainly used for fever due to warm disease, dysentery with heat-toxic blood, carbuncle, sore, furuncle, sore throat, and various infectious diseases.
[0020] Houttuynia cordata Thunb., pungent in taste and cold in nature, attributing to the lung meridian, clearing heat and detoxifying, expelling pus and resolving carbuncles, inducing diuresis for treating stranguria. It is mainly used for lung abscess with expectoration, cough due to phlegm-heat, sore throat, dysentery, carbuncles and sores, heat stranguria.
[0021] Preferably, in S1, the mass fraction of the malic acid solution is 0.1 - 0.5%.
[0022] Preferably, in S1, the temperature for stirring in the dark is 40 - 50°C.
[0023] Preferably, in S2, the power of the microwave treatment is 600 - 700 W, and the microwave temperature is 40 - 50°C.
[0024] Preferably, in S2, during the dynamic countercurrent extraction process, the solid-liquid ratio is 1:10 - 12, the extraction temperature is 40 - 50°C, and the dynamic countercurrent circulation flow rate is 6 - 8 L / min.
[0025] Preferably, in S2, the temperature for pressurized extraction is 70 - 80°C; the pressure for pressure filtration is 0.1 - 0.3 MPa.
[0026] Preferably, in S3, it is concentrated under reduced pressure to a relative density of 1.1 - 1.2, the temperature for concentration under reduced pressure is 55 - 65°C, and the vacuum degree is -0.06 to -0.08 MPa.
[0027] Preferably, in S3, the frequency of the low-frequency ultrasonic treatment is 20 - 25 kHz, and the ultrasonic power is 100 - 150 W.
[0028] Beneficial effects:
[0029] The present invention uses Solidago virgaurea, Verbena officinalis, Imperata cylindrica, Plantago asiatica, Lagenaria siceraria, Cynanchum stans, Lonicera japonica, and Houttuynia cordata Thunb. in combination, which not only has a broad-spectrum antibacterial effect, inhibits the adhesion and proliferation of pathogenic microorganisms, but also can reduce the release of inflammatory factors, alleviate the inflammation of the urinary tract mucosa, and enhance the local immune response; the combination of Plantago asiatica, Imperata cylindrica, and Lagenaria siceraria can not only inhibit the reabsorption of Na + by renal tubules, significantly promote the excretion of Na + in urine and reduce the loss of K + , but also relieve the spasm of ureteral smooth muscle and improve the problem of unsmooth urination.
[0030] The present invention uses vacuum freezing treatment in combination with cryogenic freezing ultrafine grinding, which can cause micropores to be formed in the cell structure due to ice crystal formation, improve the dissolution rate during subsequent extraction, and at the same time significantly increase the specific surface area of the system. In combination with the subsequent dynamic countercurrent extraction, the extraction efficiency is significantly improved; the various operations in S2 of the present invention are coordinated to avoid the loss of volatile oil caused by high temperature and significantly reduce the loss rate of active ingredients.
[0031] Medicinal-grade chitosan forms a cationic complex in malic acid solution, synergistically plays an antioxidant stabilizing role with sodium ascorbate, and produces intermolecular association with mannan peptide through hydrogen bonding and hydrophobic interaction. This associative structure can prolong the residence time of the active ingredient in urothelial cells and has excellent sustained-release effect.
[0032] The present invention has good effects of clearing heat and detoxifying, and promoting diuresis and relieving stranguria. It not only has obvious antibacterial and anti-inflammatory effects, but also can significantly increase urine volume, promote the excretion of Na + in urine, reduce the loss of K + , and at the same time has high stability and good reproducibility, and is more suitable for industrial production. Description of the Drawings
[0033] Figure 1 It is a comparison chart of the antibacterial diameters of the Flos Chrysanthemi Indici preparations obtained in Example 5 and Comparative Examples 1-3.
[0034] Figure 2 It is a comparison chart of the writhing times of the groups of Example 5, Comparative Example 1, Comparative Example 2, Comparative Example 3 and the blank control group.
[0035] Figure 3 It is a graph of the urine volume changes within 4 h after administration of the groups of Example 5, Comparative Example 1, Comparative Example 2, Comparative Example 3 and the model group.
[0036] Figure 4 It is a comparison chart of the contents of K + , Na + in urine within 4 h after administration of the groups of Example 5, Comparative Example 1, Comparative Example 2, Comparative Example 3 and the model group. Detailed Embodiments
[0037] The present invention will be further explained below in conjunction with specific embodiments.
[0038] Example 1
[0039] A Flos Chrysanthemi Indici preparation for promoting diuresis and relieving stranguria, the raw materials thereof include: 500 g of Solidago virgaurea, 50 g of Verbena officinalis, 100 g of Rhizoma Imperatae, 100 g of Plantago asiatica, 50 g of Lagenaria siceraria shell, 50 g of Cynanchum stauntonii, 10 g of Lonicera japonica, 10 g of Houttuynia cordata, 10 g of medicinal-grade chitosan with a deacetylation degree of 90%, 1 g of sodium ascorbate, 5 g of mannan peptide, 10 g of sodium benzoate, 1 g of chondroitin sulfate, and 8000 g of water.
[0040] The preparation method of the above-mentioned Flos Chrysanthemi Indici preparation for promoting diuresis and relieving stranguria includes the following steps:
[0041] S1. Dissolve medicinal-grade chitosan in 100 g of malic acid solution with a mass fraction of 0.1%, add sodium ascorbate and stir in the dark for 1 h, and the stirring temperature is 40°C to obtain pretreated chitosan;
[0042] S2. Grind and mix Goldenrod, Verbena, Imperata root, Plantain, Cucurbita urticaria, Rhizoma Cibotii, Flos Lonicerae, and Houttuynia cordata evenly, freeze-dry in vacuum, and microwave for 2 min, with the microwave temperature at 40°C and the microwave power at 600 W, and freeze-crush with liquid nitrogen until the average particle size is ≤10 μm to obtain a premixed raw material; subject the premixed raw material to dynamic countercurrent extraction for 1 h, with purified water as the solvent, a solid-liquid ratio of 1:10, an extraction temperature of 40°C, and a dynamic countercurrent circulation flow rate of 6 L / min; and then perform pressurized extraction for 1 h, with the pressurized extraction temperature at 70°C, and filter at 0.1 MPa to obtain an extract;
[0043] S3. Concentrate the extract under reduced pressure to a relative density of 1.1, the temperature of reduced pressure concentration is 55°C, the vacuum degree is -0.06MPa, add pretreated chitosan and mannan peptide, stir at 40°C for 10 minutes, add sodium benzoate, chondroitin sulfate, and deionized water, adjust the pH value of the system to 5.8-6, and perform low-frequency ultrasonic treatment for 10 minutes, the ultrasonic frequency is 20kHz, and the ultrasonic power is 100W.
[0044] Example 2
[0045] The invention discloses a goldenrod preparation for promoting diuresis and relieving stranguria. The raw materials thereof include: 600g of goldenrod, 150g of verbena, 300g of Imperata root, 300g of Plantain, 200g of Cucurbita urticaria shell, 250g of Rhizoma Dioscoreae, 100g of Honeysuckle, 100g of Houttuynia cordata, 20g of medicinal-grade chitosan with a deacetylation degree of 90%, 5g of sodium ascorbate, 15g of mannan peptide, 20g of sodium benzoate, 10g of chondroitin sulfate and 12000g of water.
[0046] The method for preparing the above-mentioned Huanghua preparation for promoting diuresis and relieving stranguria comprises the following steps:
[0047] S1. Dissolve pharmaceutical grade chitosan in 200 g of 0.5% malic acid solution, add sodium ascorbate and stir for 2 h in dark at 50° C. to obtain pretreated chitosan;
[0048] S2. Grind and mix Goldenrod, Verbena, Imperata root, Plantain, Cucurbita urticaria, Ligusticum chuanxiong, Honeysuckle and Houttuynia cordata evenly, freeze-dry in vacuum, and microwave for 6 min, with the microwave temperature at 50°C and the microwave power at 700 W, and freeze-crush with liquid nitrogen until the average particle size is ≤10 μm to obtain a premixed raw material; subject the premixed raw material to dynamic countercurrent extraction for 2 h, with purified water as the solvent, a solid-liquid ratio of 1:12, an extraction temperature of 50°C, and a dynamic countercurrent circulation flow rate of 8 L / min; then perform pressurized extraction for 2 h, with the pressurized extraction temperature at 80°C, and filter at 0.3 MPa to obtain an extract;
[0049] S3. Concentrate the extract under reduced pressure to a relative density of 1.2 at a reduced pressure concentration temperature of 65°C and a vacuum degree of -0.08 MPa. Add pretreated chitosan and mannan peptide, stir at 50°C for 30 min, add sodium benzoate, chondroitin sulfate, and deionized water, adjust the pH value of the system to 5.8 - 6, and perform low-frequency ultrasonic treatment for 20 min at an ultrasonic frequency of 25 kHz and an ultrasonic power of 150 W.
[0050] Example 3
[0051] A kind of Solidago virgaurea preparation for promoting diuresis and relieving stranguria, the raw materials thereof include: 520 g of Solidago virgaurea, 120 g of Verbena officinalis, 150 g of Rhizoma Imperatae, 250 g of Plantago asiatica, 80 g of Lagenaria siceraria shell, 200 g of Cynanchum stauntonii, 40 g of Lonicera japonica, 80 g of Houttuynia cordata, 12 g of medicinal chitosan with a deacetylation degree of 90%, 4 g of sodium ascorbate, 8 g of mannan peptide, 18 g of sodium benzoate, 3 g of chondroitin sulfate, and 11000 g of water.
[0052] The preparation method of the above-mentioned Solidago virgaurea preparation for promoting diuresis and relieving stranguria includes the following steps:
[0053] S1. Dissolve the medicinal chitosan in 120 g of malic acid solution with a mass fraction of 0.4%, add sodium ascorbate, and stir in the dark for 80 min at a stirring temperature of 48°C to obtain pretreated chitosan.
[0054] S2. Crush and mix Solidago virgaurea, Verbena officinalis, Rhizoma Imperatae, Plantago asiatica, Lagenaria siceraria shell, Cynanchum stauntonii, Lonicera japonica, and Houttuynia cordata evenly, perform vacuum freeze-drying and then microwave treatment for 3 min at a microwave temperature of 48°C and a microwave power of 620 W, and use liquid nitrogen to freeze and crush to an average particle size ≤ 10 μm to obtain a premixed raw material; perform dynamic countercurrent extraction on the premixed raw material for 100 min with purified water as the solvent, a material-liquid ratio of 1:10.5, an extraction temperature of 48°C, and a dynamic countercurrent circulation flow rate of 6.5 L / min; then perform pressurized extraction for 100 min at a pressurized extraction temperature of 73°C, and filter under a pressure of 0.25 MPa to obtain an extract.
[0055] S3. Concentrate the extract under reduced pressure to a relative density of 1.15 at a reduced pressure concentration temperature of 58°C and a vacuum degree of -0.07 MPa. Add pretreated chitosan and mannan peptide, stir at 48°C for 15 min, add sodium benzoate, chondroitin sulfate, and deionized water, adjust the pH value of the system to 5.8 - 6, and perform low-frequency ultrasonic treatment for 18 min at an ultrasonic frequency of 21 kHz and an ultrasonic power of 130 W.
[0056] Example 4
[0057] A kind of Solidago virgaurea preparation for promoting diuresis and relieving stranguria, the raw materials of which include: 580 g of Solidago virgaurea, 80 g of Verbena officinalis, 250 g of Rhizoma Imperatae, 150 g of Plantago asiatica, 180 g of Lagenaria siceraria shell, 100 g of Cynanchum stauntonii, 80 g of Lonicera japonica, 40 g of Houttuynia cordata, 18 g of medicinal chitosan with a deacetylation degree of 90%, 2 g of sodium ascorbate, 12 g of mannan peptide, 12 g of sodium benzoate, 7 g of chondroitin sulfate, and 9000 g of water.
[0058] The preparation method of the above Solidago virgaurea preparation for promoting diuresis and relieving stranguria includes the following steps:
[0059] S1. Dissolve the medicinal chitosan in 180 g of malic acid solution with a mass fraction of 0.2%, add sodium ascorbate and stir in the dark for 100 min, the stirring temperature is 42 °C, to obtain pretreated chitosan;
[0060] S2. Crush and mix Solidago virgaurea, Verbena officinalis, Rhizoma Imperatae, Plantago asiatica, Lagenaria siceraria shell, Cynanchum stauntonii, Lonicera japonica, and Houttuynia cordata evenly, vacuum freeze-dry and then microwave-treat for 5 min, the microwave temperature is 42 °C, the microwave power is 680 W, and use liquid nitrogen to freeze and crush to an average particle size ≤ 10 μm to obtain a premixed raw material; perform dynamic countercurrent extraction on the premixed raw material for 80 min, using purified water as the solvent, the solid-liquid ratio is 1:11.5, the extraction temperature is 42 °C, and the dynamic countercurrent circulation flow rate is 7.5 L / min; then perform pressurized extraction for 80 min, the pressurized extraction temperature is 77 °C, and filter under a pressure of 0.15 MPa to obtain an extract;
[0061] S3. Concentrate the extract under reduced pressure to a relative density of 1.15, the reduced pressure concentration temperature is 62 °C, the vacuum degree is -0.07 MPa, add the pretreated chitosan and mannan peptide, stir at a temperature of 42 °C for 25 min, add sodium benzoate, chondroitin sulfate, and deionized water, adjust the pH value of the system to 5.8 - 6, and perform low-frequency ultrasonic treatment for 12 min, the ultrasonic frequency is 24 kHz, and the ultrasonic power is 110 W.
[0062] Example 5
[0063] A kind of Solidago virgaurea preparation for promoting diuresis and relieving stranguria, the raw materials of which include: 550 g of Solidago virgaurea, 100 g of Verbena officinalis, 200 g of Rhizoma Imperatae, 200 g of Plantago asiatica, 130 g of Lagenaria siceraria shell, 150 g of Cynanchum stauntonii, 60 g of Lonicera japonica, 60 g of Houttuynia cordata, 15 g of medicinal chitosan with a deacetylation degree of 90%, 3 g of sodium ascorbate, 10 g of mannan peptide, 15 g of sodium benzoate, 5 g of chondroitin sulfate, and 10000 g of water.
[0064] The preparation method of the above Solidago virgaurea preparation for promoting diuresis and relieving stranguria includes the following steps:
[0065] S1. Dissolve pharmaceutical-grade chitosan in 150 g of malic acid solution with a mass fraction of 0.3%, add sodium ascorbate, stir in the dark for 90 min at a stirring temperature of 45 °C to obtain pretreated chitosan;
[0066] S2. Crush and mix Solidago virgaurea, Verbena officinalis, Rhizoma Imperatae, Plantago asiatica, Fructus Trichosanthis, Cynanchum stauntonii, Lonicera japonica, and Houttuynia cordata evenly, vacuum freeze-dry and then microwave-treat for 4 min at a microwave temperature of 45 °C and a microwave power of 650 W. Use liquid nitrogen to freeze-crush to an average particle size of ≤10 μm to obtain a premixed raw material; perform dynamic countercurrent extraction on the premixed raw material for 90 min with purified water as the solvent, a material-liquid ratio of 1:11, an extraction temperature of 45 °C, and a dynamic countercurrent circulation flow rate of 7 L / min; then perform pressurized extraction for 90 min at a pressurized extraction temperature of 75 °C, and filter under 0.2 MPa pressure to obtain an extract;
[0067] S3. Concentrate the extract under reduced pressure to a relative density of 1.15 at a reduced pressure concentration temperature of 60 °C and a vacuum degree of -0.07 MPa. Add pretreated chitosan and mannan peptide, stir at a temperature of 45 °C for 20 min, add sodium benzoate, chondroitin sulfate, and deionized water, adjust the pH value of the system to 5.8 - 6, and perform low-frequency ultrasonic treatment for 15 min at an ultrasonic frequency of 22.5 kHz and an ultrasonic power of 120 W.
[0068] Comparative Example 1
[0069] A Solidago virgaurea preparation for promoting diuresis and alleviating stranguria, the raw materials of which include: 550 g of Solidago virgaurea, 100 g of Verbena officinalis, 330 g of Rhizoma Imperatae, 200 g of Plantago asiatica, 150 g of Cynanchum stauntonii, 60 g of Lonicera japonica, 60 g of Houttuynia cordata, 15 g of pharmaceutical-grade chitosan with a deacetylation degree of 90%, 3 g of sodium ascorbate, 10 g of mannan peptide, 15 g of sodium benzoate, 5 g of chondroitin sulfate, and 10000 g of water.
[0070] The preparation method of the above Solidago virgaurea preparation for promoting diuresis and alleviating stranguria includes the following steps:
[0071] S1. Dissolve pharmaceutical-grade chitosan in 150 g of malic acid solution with a mass fraction of 0.3%, add sodium ascorbate, stir in the dark for 90 min at a stirring temperature of 45 °C to obtain pretreated chitosan;
[0072] S2. Grind and mix Goldenrod, Verbena, Plantain, Imperata cylindrica, Rhizoma Cibotii, Flos Lonicerae, and Houttuynia cordata evenly, freeze-dry in vacuum, and microwave-treat for 4 min, with the microwave temperature at 45°C and the microwave power at 650W, and freeze-crush with liquid nitrogen until the average particle size is ≤10 μm to obtain a premixed raw material; subject the premixed raw material to dynamic countercurrent extraction for 90 min, with purified water as the solvent, a solid-liquid ratio of 1:11, an extraction temperature of 45°C, and a dynamic countercurrent circulation flow rate of 7 L / min; and then perform pressurized extraction for 90 min, with the pressurized extraction temperature at 75°C, and filter at 0.2 MPa to obtain an extract;
[0073] S3. Concentrate the extract under reduced pressure to a relative density of 1.15 at a temperature of 60°C and a vacuum degree of -0.07 MPa. Add pretreated chitosan and mannan peptide, stir at 45°C for 20 min, add sodium benzoate, chondroitin sulfate and deionized water, adjust the pH value of the system to 5.8-6, and perform low-frequency ultrasonic treatment for 15 min at a frequency of 22.5 kHz and a power of 120 W.
[0074] Comparative Example 2
[0075] A diuretic and stranguria-relieving goldenrod preparation comprises the following raw materials: 550g goldenrod, 100g verbena, 200g Imperata root, 200g Plantain, 130g Cucurbita urticaria, 150g Rhizoma Dioscoreae, 60g Honeysuckle, 60g Houttuynia cordata, 18g medicinal-grade chitosan with a deacetylation degree of 90%, 10g mannan peptide, 15g sodium benzoate, 5g chondroitin sulfate and 10000g water.
[0076] The method for preparing the above-mentioned Huanghua preparation for promoting diuresis and relieving stranguria comprises the following steps:
[0077] S1. Grind and mix goldenrod, verbena, Imperata root, plantain, gourd shell, radix scutellariae, honeysuckle and houttuynia cordata evenly, freeze-dry in vacuum, and microwave for 4 min, with the microwave temperature at 45°C and the microwave power at 650W, and freeze-crush with liquid nitrogen until the average particle size is ≤10 μm to obtain a premixed raw material; subject the premixed raw material to dynamic countercurrent extraction for 90 min, with purified water as the solvent, a solid-liquid ratio of 1:11, an extraction temperature of 45°C, and a dynamic countercurrent circulation flow rate of 7 L / min; then perform pressurized extraction for 90 min, with the pressurized extraction temperature at 75°C, and filter at 0.2 MPa to obtain an extract;
[0078] S2. Concentrate the extract under reduced pressure to a relative density of 1.15 at a temperature of 60°C and a vacuum degree of -0.07 MPa. Add pharmaceutical grade chitosan and mannan peptide, stir at 45°C for 20 min, add sodium benzoate, chondroitin sulfate and deionized water, adjust the pH value of the system to 5.8-6, and perform low-frequency ultrasonic treatment for 15 min at a frequency of 22.5 kHz and a power of 120 W.
[0079] Comparative Example 3
[0080] A Solidago virgaurea preparation for promoting diuresis and removing stranguria, the raw materials of which include: 550 g of Solidago virgaurea, 100 g of Verbena officinalis, 200 g of Imperata cylindrica, 200 g of Plantago asiatica, 130 g of Lagenaria siceraria, 150 g of Cynanchum stauntonii, 60 g of Lonicera japonica, 60 g of Houttuynia cordata, 15 g of pharmaceutical-grade chitosan with a degree of deacetylation of 90%, 3 g of sodium ascorbate, 10 g of mannan peptide, 15 g of sodium benzoate, 5 g of chondroitin sulfate, and 10000 g of water.
[0081] The preparation method of the above-mentioned Solidago virgaurea preparation for promoting diuresis and removing stranguria includes the following steps:
[0082] S1. Dissolve the pharmaceutical-grade chitosan in 150 g of a 0.3% malic acid solution, add sodium ascorbate, and stir in the dark for 90 min at a stirring temperature of 45 °C to obtain pretreated chitosan;
[0083] S2. Crush and mix Solidago virgaurea, Verbena officinalis, Imperata cylindrica, Plantago asiatica, Lagenaria siceraria, Cynanchum stauntonii, Lonicera japonica, and Houttuynia cordata evenly, perform vacuum freeze-drying and then microwave treatment for 4 min at a microwave temperature of 45 °C and a microwave power of 650 W, and mechanically crush to an average particle size ≤ 10 μm to obtain a premixed raw material; perform dynamic countercurrent extraction on the premixed raw material for 90 min with purified water as the solvent, a solid-to-liquid ratio of 1:11, an extraction temperature of 45 °C, and a dynamic countercurrent circulation flow rate of 7 L / min; then perform pressurized extraction for 90 min at a pressurized extraction temperature of 75 °C and filter under a pressure of 0.2 MPa to obtain an extract;
[0084] S3. Concentrate the extract under reduced pressure to a relative density of 1.15 at a reduced pressure concentration temperature of 60 °C and a vacuum degree of -0.07 MPa, add the pretreated chitosan and mannan peptide, stir at a temperature of 45 °C for 20 min, add sodium benzoate, chondroitin sulfate, and deionized water, adjust the pH value of the system to 5.8 - 6, and perform low-frequency ultrasonic treatment for 15 min at an ultrasonic frequency of 22.5 kHz and an ultrasonic power of 120 W.
[0085] Perform in vitro antibacterial tests on the Solidago virgaurea preparations obtained in Example 5 and Comparative Examples 1 - 3 as follows: Inoculate Staphylococcus aureus, Streptococcus faecalis, Escherichia coli, and Proteus vulgaris on nutrient agar plates respectively, Neisseria gonorrhoeae on chocolate agar plates, and Candida albicans on Sabouraud agar plates; punch holes with a diameter of 5 mm on each agar plate, dilute the Solidago virgaurea preparations obtained in Example 5 and Comparative Examples 1 - 3 to 100 times respectively and add them into the holes of each agar plate, place them in an incubator at 37 °C for 24 h, and place Neisseria gonorrhoeae in a CO2 incubator at 37 °C for 24 h, and count the drug inhibition diameters on each agar plate of each group.
[0086] As Figure 1As shown in the figure, the yellow flower preparations obtained in Example 5 and Comparative Examples 1-3 have antibacterial effects to varying degrees against Staphylococcus aureus, Streptococcus faecalis, Escherichia coli, Proteus vulgaris, Neisseria gonorrhoeae, and Candida albicans. Among them, the antibacterial effects against Staphylococcus aureus and Neisseria gonorrhoeae are the strongest; and the antibacterial effect of the yellow flower preparation obtained in Example 5 against each strain is the strongest, superior to that of Comparative Examples 1-3 (P < 0.05).
[0087] Taking Kunming mice as the experimental subjects, the yellow flower preparations obtained in Example 5 and Comparative Examples 1-3 were used for the analgesic test in mice. The specific steps are as follows: 50 male mice (body weight 20 ± 2 g) were randomly divided into 5 groups (10 mice in each group), namely the Example 5 group, the Comparative Example 1 group, the Comparative Example 2 group, the Comparative Example 3 group, and the blank control group. They were successively given the yellow flower preparation obtained in Example 5 (dose: 5 g / kg bw), the yellow flower preparation obtained in Comparative Example 1 (dose: 5 g / kg bw), the yellow flower preparation obtained in Comparative Example 2 (dose: 5 g / kg bw), the yellow flower preparation obtained in Comparative Example 2 (dose: 5 g / kg bw), and intragastrically administered with an equal volume of distilled water; 1 h after administration, each mouse was intraperitoneally injected with 0.2 mL / mouse of 0.6% glacial acetic acid solution to cause pain, and the writhing times of the mice within 20 min were immediately observed and recorded.
[0088] As Figure 2 shown, the yellow flower preparations obtained in Example 5 and Comparative Examples 1-3 can significantly reduce the writhing times of mice caused by acetic acid; and the number of writhing times of the mice in the Example 5 group is the least, significantly less than that of the Comparative Examples 1-3 groups (P < 0.05), indicating that the yellow flower preparation obtained by the present invention can significantly relieve pain.
[0089] Using Kunming mice as experimental subjects, the diuretic tests on mice were conducted with the yellow flower preparations obtained in Example 5 and Comparative Examples 1-3 as follows: Male mice (body weight 20±2 g) were fed conventionally and allowed to drink water freely. 50 mice with urine output reaching more than 40% of the infused volume within 2 h were selected and randomly divided into 5 groups (10 mice in each group), namely the Example 5 group, the Comparative Example 1 group, the Comparative Example 2 group, the Comparative Example 3 group and the model group. They were successively administered the yellow flower preparation obtained in Example 5 (dose: 5 g / kg bw), the yellow flower preparation obtained in Comparative Example 1 (dose: 5 g / kg bw), the yellow flower preparation obtained in Comparative Example 2 (dose: 5 g / kg bw), the yellow flower preparation obtained in Comparative Example 2 (dose: 5 g / kg bw), and an equal volume of distilled water by gavage. Subsequently, they were fasted for 16-18 h and allowed to drink water freely. For each test, 1 mouse was taken, the lower abdomen of the animal was gently pressed to drain the remaining urine, a load of normal saline was given by gavage at 0.4 mL / 10 g, and then the administration by gavage was continued. The mice were randomly placed in a simple metabolic cage, with 1 mouse in each cage. The urine of each mouse was collected at 1, 2, 3, and 4 h after administration, and the urine output per 10 g body weight of the mouse was calculated. The collected urine was sealed and stored at 0 °C in a refrigerator. Before measurement, the urine was dissolved in a 37 °C water bath, shaken well, sampled and diluted 10 times with deionized water, and the contents of K + , Na + in the urine were measured using an electrolyte analyzer.
[0090] As Figure 3 and Figure 4 shown, the urine output of the mice in the Example 5 group was always the highest after administration, superior to the other groups (P < 0.05); moreover, the content of Na + in the urine of the mice in the Example 5 group was the highest, and the content of K + was the lowest, superior to the other groups (P < 0.05).
[0091] The above are only the preferred specific embodiments of the present invention, but the protection scope of the present invention is not limited thereto. Any person skilled in the art within the technical scope disclosed by the present invention, according to the technical solution and inventive concept of the present invention, makes equivalent substitutions or changes, and should be covered by the protection scope of the present invention.
Claims
1. A preparation of Flos Chrysanthemi for promoting diuresis and alleviating stranguria, characterized in that, Its raw materials by mass parts include: 500 - 600 parts of Solidago virgaurea, 50 - 150 parts of Verbena officinalis, 100 - 300 parts of Rhizoma Imperatae, 100 - 300 parts of Plantago asiatica, 50 - 200 parts of Lagenaria siceraria (Molina) Standl., 50 - 250 parts of Cynanchum glaucescens (Decne.) Hand.-Mazz., 10 - 100 parts of Lonicera japonica Thunb., 10 - 100 parts of Houttuynia cordata Thunb., 10 - 20 parts of chitosan, 1 - 5 parts of sodium ascorbate, 5 - 15 parts of mannan oligosaccharide peptide, 10 - 20 parts of sodium benzoate, 1 - 10 parts of chondroitin sulfate, and 8000 - 12000 parts of water.
2. The Huanghua preparation for promoting diuresis and alleviating stranguria according to claim 1, wherein The degree of deacetylation of chitosan is 88 - 92%.
3. The huanghua preparation for promoting diuresis and relieving stranguria according to claim 1, characterized in that, In mannan oligosaccharide peptide, the mass percentage of total sugar is 88 - 90%, and the mass percentage of amino acid is 5 - 6%.
4. A preparation method of a Hemerocallis flower preparation for promoting diuresis and dredging strangury as described in any one of claims 1-3, characterized in that, It includes the following steps: S1. Dissolve chitosan in malic acid solution, add sodium ascorbate and stir in the dark for 1 - 2 h to obtain pretreated chitosan. S2. Crush and mix Solidago virgaurea, Verbena officinalis, Rhizoma Imperatae, Plantago asiatica, Lagenaria siceraria (Molina) Standl., Cynanchum glaucescens (Decne.) Hand.-Mazz., Lonicera japonica Thunb., and Houttuynia cordata Thunb. evenly, freeze-dry and then microwave-treat for 2 - 6 min, and freeze-crush with liquid nitrogen to obtain a premixed raw material; perform dynamic countercurrent extraction on the premixed raw material for 1 - 2 h; then perform pressurized extraction for 1 - 2 h, and filter press to obtain an extract. S4. Concentrate the extract under reduced pressure, add the pretreated chitosan and mannan oligosaccharide peptide, stir at 40 - 50 °C for 10 - 30 min, add sodium benzoate, chondroitin sulfate, and water, adjust the pH value of the system to 5.8 - 6, and perform low-frequency ultrasonic treatment for 10 - 20 min.
5. The preparation method of the Coreopsis tinctoria preparation for promoting diuresis and alleviating stranguria according to claim 4, wherein, In S1, the mass fraction of the malic acid solution is 0.1 - 0.5%.
6. The preparation method of the Coreopsis tinctoria preparation for promoting diuresis and draining stranguria according to claim 4, characterized in that, In S1, the temperature of stirring in the dark is 40 - 50 °C.
7. The preparation method of the Hemerocallis flower preparation for promoting diuresis and alleviating stranguria according to claim 4, characterized in that, In S2, the power of the microwave treatment is 600 - 700 W, and the microwave temperature is 40 - 50 °C.
8. The preparation method of the Coreopsis tinctoria preparation for promoting diuresis and relieving stranguria according to claim 4, characterized in that, In S2, during the dynamic countercurrent extraction process, the solid-liquid ratio is 1:10 - 12, the extraction temperature is 40 - 50 °C, and the dynamic countercurrent circulation flow rate is 6 - 8 L / min.
9. The preparation method of the coreopsis preparation for promoting diuresis and alleviating stranguria according to claim 4, characterized in that, In S2, the temperature of the pressurized extraction is 70 - 80 °C; the pressure of the filter press is 0.1 - 0.3 MPa.
10. The preparation method of the Hemerocallis flower preparation for promoting diuresis and relieving stranguria according to claim 4, wherein, In S3, concentrate under reduced pressure to a relative density of 1.1 - 1.2, the temperature of the reduced pressure concentration is 55 - 65 °C, and the vacuum degree is -0.06~-0.08 MPa.