Preparation method of colon powder for external use
By optimizing the raw materials and preparation process of the colon powder, and employing enzymatic pretreatment, ultrasound-assisted water extraction, spray drying, and irradiation sterilization, the problems of single composition and stability of existing external colon powders have been solved, achieving a highly efficient and uniform colon treatment effect.
Patent Information
- Application Number
- CN202511444904.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-10-10
- Publication Date
- 2026-01-20
AI Technical Summary
Existing topical powders for colonic use suffer from limitations such as single drug components, low extraction rate, uneven particle size distribution, and poor flowability, making it difficult to simultaneously achieve anti-inflammatory and colonic mucosal repair effects. Furthermore, high-temperature sterilization destroys active ingredients, affecting therapeutic efficacy and safety.
Using Astragalus membranaceus, Pulsatilla chinensis, Astragalus membranaceus, and Lithospermum erythrorhizon as the main raw materials, combined with Portulaca oleracea and Fraxinus chinensis, the extraction solvent dosage, temperature, and time are optimized through enzymatic pretreatment, ultrasonic-assisted water extraction, spray drying, and irradiation sterilization processes to ensure efficient extraction and stability of active ingredients. Three-dimensional mixing and low-temperature drying technologies are used to ensure product uniformity and safety.
It significantly improves the extraction rate and stability of active ingredients, enhances the anti-inflammatory and colonic mucosal repair effects, ensures product uniformity and safety, and meets the targeted treatment needs of colon diseases.
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Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of medicine preparation, in particular to a preparation method of a colon powder for external use. BACKGROUND
[0002] Colonic diseases are common digestive system diseases in clinic, which have long course and are prone to recurrence, seriously affecting the quality of life of patients. At present, oral drugs or enema administration are mostly used in clinical treatment. Oral drugs need to be absorbed by the gastrointestinal tract and then act on the colon, which is easy to be destroyed by gastric acid and digestive enzymes, has low bioavailability, and may cause systemic side effects. Traditional enema preparations are mostly in liquid dosage form, which has the problems of short retention time of drugs in the colon after enema, uneven distribution, slow relief of effective components, and poor quality and effect.
[0003] The existing colon powder for external use has obvious defects in raw material compatibility and preparation process. Most of the existing formulas only use the efficacy of a single medicinal material, and do not form a multi-component action system. For example, although Huangqi can enhance immunity, it lacks targeted inhibitory components for colonic inflammation, and it is difficult to meet the dual needs of anti-inflammatory and repair of colonic mucosa. In addition, the preparation process mostly uses traditional decoction extraction method, which has low extraction rate of effective components and easy degradation of components during drying process. The sterilization process mostly uses high-temperature sterilization, which further destroys active components. At the same time, the product has uneven particle size distribution and poor flowability, which affects the uniformity and safety of drug administration during clinical use.
[0004] Therefore, the present application provides a preparation method of a colon powder for external use. SUMMARY
[0005] The present application aims to provide a preparation method of a colon powder for external use to solve the problems in the background art.
[0006] To achieve the above-mentioned purpose, the present application provides the following technical solution: a preparation method of a colon powder for external use, which is composed of the following raw materials by weight: 15-25 parts of Radix Astragali, 10-20 parts of Radix Pulsatillae, 8-18 parts of Radix Astragali, 6-16 parts of Radix Baphlantis, and 3-8 parts of auxiliary materials. The preparation method comprises the steps of raw material pretreatment, extraction, drying, mixing, and sterilization.
[0007] The raw materials further comprise 5-15 parts of Portulaca oleracea and 4-12 parts of Cortex Fraxini by weight, and the weight ratio of Portulaca oleracea to Cortex Fraxini is 1:0.8-1.2.
[0008] The auxiliary materials are at least two of microcrystalline cellulose, sodium carboxymethyl starch, and magnesium stearate, and the weight ratio of microcrystalline cellulose to sodium carboxymethyl starch is 2:1-1.5.
[0009] As a specific scheme of the technical scheme of the present application, the raw material pretreatment step is specifically: after removing impurities from Radix Astragali, Radix Paeoniae Alba, Radix Paeoniae Rubra and Radix Lithospermi, they are then placed in a blast drying oven at 60-70℃ to dry the moisture content to ≤8%, and then ground to 80-100 mesh particles.
[0010] As a specific scheme of the technical scheme of the present application, the extraction step adopts an ultrasonic-assisted water extraction process, with the following specific parameters: the extraction solvent is 6-10 times the weight of the raw materials of purified water, the ultrasonic power is 300-500W, the extraction temperature is 50-65℃, the extraction time is 1.5-2.5 hours, the extraction times is 2-3 times, and the combined extraction liquid is filtered to be clear.
[0011] As a specific scheme of the technical scheme of the present application, the clear extraction liquid is concentrated under reduced pressure, with the following concentration conditions: vacuum degree -0.08 to -0.06 MPa, temperature 60-75℃, and concentrated to a relative density of 1.20-1.30 of the extract.
[0012] As a specific scheme of the technical scheme of the present application, the drying step adopts a spray drying process, with the following spray drying parameters: inlet air temperature 160-180℃, outlet air temperature 70-85℃, feed rate 20-30mL / min, atomization pressure 0.2-0.3MPa, and after drying, dry extract powder is obtained, with a moisture content of ≤5%.
[0013] As a specific scheme of the technical scheme of the present application, the mixing step is: placing the dry extract powder and excipients in a three-dimensional motion mixer, with a mixing speed of 15-25r / min and a mixing time of 20-30 minutes, and stopping every 5-8 minutes during the mixing process to check the uniformity of mixing, to ensure that the content variation coefficient is ≤3%.
[0014] As a specific scheme of the technical scheme of the present application, the sterilization step adopts an irradiation sterilization process, with an irradiation dose of 5-8kGy, and after sterilization, the colon powder is subjected to microbial limit detection, to ensure that the total number of bacteria is ≤100cfu / g, the total number of molds and yeasts is ≤10cfu / g, and Escherichia coli and Staphylococcus aureus are not detected.
[0015] As a specific scheme of the technical scheme of the present application, the purslane and cortex fraxini need to be subjected to enzymatic hydrolysis treatment before extraction, with the following enzymatic hydrolysis process: adding 0.5-1% of the weight of the raw materials of cellulase, enzymatic hydrolysis temperature 10-50℃, enzymatic hydrolysis pH value 4.5-5.5, enzymatic hydrolysis time 1-1.5 hours, and after enzymatic hydrolysis, the temperature is raised to 80-90℃ to inactivate the enzyme for 10-15 minutes.
[0016] As a specific scheme of the technical scheme of the present application, inert gas is introduced into the extraction system every 30-40 minutes during the ultrasonic-assisted water extraction process, the inert gas is nitrogen, and the aeration rate is 0.5-1 L / min, so as to prevent the oxidation degradation of the effective components.
[0017] Compared with the prior art, the present application has the following beneficial effects:
[0018] The present application realizes multiple effects of anti-inflammation, repair of colon mucosa and enhancement of the resistance of the body by taking radix astragali, radix pulsatillae, radix astragali and porphyra as raw materials, radix astragali tonifying the spleen and replenishing qi, radix pulsatillae clearing heat and detoxifying, radix astragali enhancing immunity, and radix baphlami cooling blood and activating blood, and further adding spilanthes and cortex fraxini, the antibacterial and anti-inflammatory effects can be strengthened, the treatment of diseases such as ulcerative colitis can be significantly improved, and the problems of single formula and limited efficacy of the prior art are solved.
[0019] Meanwhile, the ultrasonic-assisted water extraction process is adopted, the extraction solvent dosage, ultrasonic power, temperature and time parameters are optimized, compared with the traditional decoction method, the extraction rate of the effective components is increased by more than 30%; nitrogen is introduced during the extraction process to prevent the oxidation degradation of the components, the vacuum concentration and spray drying process are combined, rapid drying is realized in a low-temperature environment, the damage of high temperature to the active components is avoided, the content of the effective components (such as astragaloside A and shikonin) in the dry extract powder is increased by 25%-40% compared with the traditional process, and the stability of the product efficacy is ensured. DETAILED DESCRIPTION
[0020] Example 1: Preparation of a base formula for a colon powder for external use
[0021] Raw material ratio: 20 parts of radix astragali, 15 parts of radix pulsatillae, 13 parts of radix astragali, 11 parts of radix baphlami, 10 parts of spilanthes, 9 parts of cortex fraxini (weight ratio of spilanthes to cortex fraxini 1:0.9), and 5 parts of auxiliary materials (3.2 parts of microcrystalline cellulose and 1.8 parts of sodium carboxymethyl starch, weight ratio 2:1.125).
[0022] Preparation steps:
[0023] Raw material pretreatment: after removing impurities from radix astragali, radix pulsatillae, radix astragali and radix baphlami, and removing impurities from spilanthes and cortex fraxini, 0.8% of cellulase based on the weight of the raw materials is added, and enzymolysis is carried out at 45°C and pH 5.0 for 1.2 hours, then the temperature is increased to 85°C for 12 minutes to inactivate the enzyme, and all the raw materials are dried in a 65°C air-drying oven to a moisture content of 6%, and then pulverized to 90 mesh particles.
[0024] Extraction: the pretreated raw materials are put into an extraction tank, 8 times the total mass of the raw materials of purified water is added, the ultrasonic power is set to 400 W, and the extraction temperature is set to 58°C, nitrogen is introduced every 35 minutes during the extraction process (aeration rate 0.8 L / min), extraction is carried out twice, each time for 2 hours, the extraction liquids are combined and filtered through a 0.22 um microporous filter membrane to be clear.
[0025] Concentration under reduced pressure: The clarified extract was placed in a rotary evaporator and concentrated under the conditions of vacuum degree -0.07 MPa and temperature 70℃ until the extract paste with a relative density of 1.25 at 60℃ was obtained.
[0026] Spray drying: The extract paste was dried by a spray dryer with the inlet air temperature of 170℃, the outlet air temperature of 78℃, the feeding rate of 25 mL / min and the atomization pressure of 0.25 MPa, and the dry extract powder was obtained with the moisture content of 4.2%.
[0027] Mixing: The dry extract powder and the excipients were put into a three-dimensional motion mixer with the rotation speed of 20 r / min, and mixed for 25 minutes. The mixture uniformity was detected every 6 minutes during the mixing process by high performance liquid chromatography, and the final content variation coefficient was 2.3%.
[0028] Sterilization: The sterilization was performed by irradiation with the dose of 6 kGy, and the microbial limit was detected after the sterilization.
[0029] Example 2 Preparation of a high-portulaca oleracea ratio of a topical colon powder
[0030] Raw material ratio: 25 parts of radix astragali, 20 parts of radix anemarrhena, 18 parts of radix astragali, 16 parts of radix lithospermi, 15 parts of portulaca oleracea, 12 parts of cortex fraxini (weight ratio of portulaca oleracea to cortex fraxini 1:0.8), and 8 parts of excipients (5.2 parts of microcrystalline cellulose and 2.8 parts of sodium carboxymethyl starch, weight ratio 2:1.08).
[0031] Preparation steps:
[0032] Raw material pretreatment: The enzymolysis process of portulaca oleracea and cortex fraxini was 1% cellulase based on the weight of raw materials, and the enzymolysis was performed at 48℃ and pH 5.2 for 1.5 hours. The enzyme inactivation temperature was 88℃, and the time was 15 minutes. All the raw materials were dried at 68℃ until the moisture content was 5%, and then pulverized to 100 mesh.
[0033] Extraction: The extraction solvent was 10 times the total weight of the raw materials of purified water. The ultrasonic power was 500 W, and the temperature was 65℃. Nitrogen was passed every 40 minutes (1 L / min), and the extraction was performed for 3 times, each for 2.5 hours. The clarity after filtration met the requirements.
[0034] Concentration under reduced pressure: The vacuum degree was -0.08 MPa, and the temperature was 75℃. The extract paste with a relative density of 1.30 was obtained.
[0035] Spray drying: The inlet air temperature was 180℃, the outlet air temperature was 85℃, the feeding rate was 30 mL / min, and the atomization pressure was 0.3 MPa. The moisture content of the dry extract powder was 3.8%.
[0036] Mixing: The rotation speed was 25 r / min, and the mixing was performed for 30 minutes. The uniformity was detected every 8 minutes, and the variation coefficient was 2.1%.
[0037] Sterilization: 8kGy irradiation sterilization, subsequent microbial indicators testing.
[0038] Example 3 Preparation of external use colon powder with low proportion of auxiliary materials
[0039] Raw material proportioning: 15 parts of earthy astragalus, 10 parts of white peony, 8 parts of astragalus, 6 parts of Chinese columbine, 5 parts of betony, 4 parts of cortex fraxini (weight ratio of betony to cortex fraxini 1:0.8), 3 parts of auxiliary materials (1.8 parts of microcrystalline cellulose, 1.2 parts of magnesium stearate).
[0040] Preparation steps:
[0041] Raw material pretreatment: the enzymolysis process of betony and cortex fraxini is 0.5% cellulase of raw material weight, 40℃, pH value 4.5, enzymolysis for 1 hour, enzyme inactivation temperature 80℃, time 10 minutes. Dry all raw materials at 60℃ to a moisture content of 8% and crush to 80 mesh.
[0042] Extraction: the extraction solvent is 6 times the weight of the total raw materials of purified water, the ultrasonic power is 300W, the temperature is 50℃, nitrogen is introduced every 30 minutes (0.5L / min), extraction is carried out 2 times (1.5 hours each time), and filtration is carried out to clarify.
[0043] Reduced pressure concentration: vacuum degree -0.06MPa, temperature 60℃, concentrate to the relative density of 1.20 (60℃) of extract.
[0044] Spray drying: inlet air temperature 160℃, outlet air temperature 70℃, feed rate 20mL / min, atomization pressure 0.2MPa, moisture content of dry extract powder 4.8%.
[0045] Mixing: rotation speed 15r / min, mixing 20 minutes, check uniformity every 5 minutes, coefficient of variation 2.8%.
[0046] Sterilization: 5kGy irradiation sterilization, complete preparation.
[0047] Comparative example 1 preparation of colon powder without enzymolysis treatment
[0048] The same raw material proportioning and preparation steps as example 1 are adopted, only the enzymolysis treatment steps of betony and cortex fraxini are deleted, and the cleaning and drying are directly carried out before participating in the extraction.
[0049] Comparative example 2 preparation of colon powder by traditional decoction extraction
[0050] The same raw material proportioning and preparation steps as example 1 are adopted, the ultrasonic assisted water extraction is replaced by traditional decoction extraction (extraction temperature 100℃, extraction time 3 hours, extraction 2 times), and nitrogen is not introduced during the extraction process.
[0051] Experimental data detection and analysis
[0052] 1. Active ingredient content detection (high performance liquid chromatography)
[0053]
[0054] The active ingredient contents of Examples 1-3 are significantly higher than those of Comparative Examples 1 and 2. In Comparative Example 1, the cell wall structure of the purslane and cortex of the cortex is not destroyed by the cellulase due to insufficient enzymatic treatment, resulting in a decrease in the dissolution rate of the active ingredients. In Comparative Example 2, the traditional decoction method is used, which easily destroys the heat-sensitive components at high temperatures, and some components are oxidized and degraded due to the absence of nitrogen, further reducing the content.
[0055] 2. In vitro release rate detection (artificial colon environment)
[0056]
[0057] The active ingredient release rates of Examples 1-3 are all more than 80% within 1 hour and close to 100% within 4 hours, meeting the standard of 1 hour ≥ 80% and 4 hours ≥ 95%. The total release amount of Comparative Example 1 is insufficient due to the low active ingredient content of the raw material. The degradation of the components in Comparative Example 2 further affects the release effect, and the particle size of the powder prepared by the traditional process is not uniform, which also reduces the release rate.
[0058] 3. Microbial limit detection
[0059]
[0060] The microbial indicators of all examples and comparative examples meet the national standard, indicating that the irradiation sterilization process (5-8 kGy) used in the present application can effectively control microbial contamination, and different raw material ratios and process parameters have no significant effect on the sterilization effect.
[0061] 4. Product physical performance detection
[0062]
[0063] The physical properties of Examples 1-3 meet the quality requirements, the particle size distribution is uniform, the repose angle is small (good flowability), the bulk density is appropriate, and the uniformity coefficient of the mixture is ≤3%. The flowability and uniformity of Comparative Examples 1 and 2 are poor due to the uneven particle size of the raw materials and insufficient mixing time, which may affect the accuracy of clinical administration.
[0064] The application can significantly improve the dissolution rate and stability of effective components and the content of key components such as astragaloside B and baiyunoside by the combined process of "enzymatic pretreatment + ultrasonic-assisted water extraction (nitrogen flushing)".
[0065] The application of spray drying and three-dimensional mixing process ensures that the product has uniform particle size, good fluidity and excellent in-vitro release performance, and can quickly release effective components within 1 hour, meeting the demand of targeted treatment of colon diseases.
[0066] Although embodiments of the application have been shown and described, it is to be understood that the application is not limited to these embodiments. Since modifications, variations, replacements and changes can be made to these embodiments without departing from the principles and spirit of the application, the scope of the application is defined by the appended claims and their equivalents.
Claims
1. A method for preparing a topical colon powder, characterized by, The external use colon powder is composed of the following raw materials in parts by weight: 15-25 parts of Radix Astragali, 10-20 parts of Radix Pulsatillae, 8-18 parts of Radix Astragali, 6-16 parts of Radix Lithospermi, and 3-8 parts of auxiliary materials; the preparation method comprises the steps of raw material pretreatment, extraction, drying, mixing, and sterilization. The raw materials further comprise 5-15 parts by weight of Portulaca oleracea and 4-12 parts by weight of Cortex Fraxini, and the weight ratio of Portulaca oleracea to Cortex Fraxini is 1:0.8-1.
2. The auxiliary materials are at least two of microcrystalline cellulose, sodium carboxymethyl starch, and magnesium stearate, and the weight ratio of microcrystalline cellulose to sodium carboxymethyl starch is 2:1-1.
5.
2. The preparation method of the external use colon powder according to claim 1, characterized in that, The raw material pretreatment step specifically comprises the following steps: removing impurities from Radix Astragali, Radix Pulsatillae, Radix Astragali, and Radix Lithospermi, respectively, and then drying them in a blast drying oven at 60-70°C to a water content of ≤8%, and then crushing them to 80-100 mesh particles.
3. The preparation method of the external use colon powder according to claim 1, characterized in that, The extraction step adopts an ultrasonic-assisted water extraction process, and the specific parameters are as follows: the extraction solvent is 6-10 times the total weight of the raw materials of purified water, the ultrasonic power is 300-500 W, the extraction temperature is 50-65°C, the extraction time is 1.5-2.5 hours, the extraction is performed 2-3 times, and the extracted liquid is combined and filtered to be clear.
4. The method for preparing an external colonic powder according to claim 3, characterized in that, The clear extracted liquid is concentrated under reduced pressure, and the concentration conditions are as follows: vacuum degree -0.08 to -0.06 MPa, temperature 60-75°C, and concentration to a relative density of 1.20-1.30 of the extract.
5. The method for preparing an external colonic powder according to claim 1, characterized in that, The drying step adopts a spray drying process, and the spray drying parameters are as follows: inlet air temperature 160-180°C, outlet air temperature 70-85°C, feed rate 20-30 mL / min, and atomization pressure 0.2-0.3 MPa, and the dry extract powder is obtained after drying, and the moisture content of the dry extract powder is ≤5%.
6. The method for preparing an external colonic powder according to claim 5, characterized in that, The mixing step is as follows: placing the dry extract powder and the auxiliary materials in a three-dimensional motion mixer, mixing at a speed of 15-25 r / min for 20-30 minutes, and stopping every 5-8 minutes during the mixing process to check the uniformity of the mixture, and ensuring that the coefficient of variation of the contents is ≤3%.
7. The method of claim 1, wherein the colon powder is prepared by mixing the following ingredients: The sterilization step adopts an irradiation sterilization process, and the irradiation dose is 5-8 kGy, and after sterilization, the microbial limit of the colon powder is detected to ensure that the total number of bacteria is ≤100 cfu / g, the total number of molds and yeasts is ≤10 cfu / g, and Escherichia coli and Staphylococcus aureus are not detected. 8. The method for preparing an external colonic powder according to claim 1, characterized in that, Portulaca oleracea and Cortex Fraxini need to be subjected to enzymatic hydrolysis treatment before extraction, and the enzymatic hydrolysis process is as follows: adding 0.5-1% of cellulase based on the weight of the raw materials, enzymatic hydrolysis temperature 10-50°C, enzymatic hydrolysis pH value 4.5-5.5, and enzymatic hydrolysis time 1-1.5 hours, and after enzymatic hydrolysis, the temperature is raised to 80-90°C to inactivate the enzyme for 10-15 minutes.
9. A method for preparing an external colonic powder according to claim 3, characterized in that, During the ultrasonic-assisted water extraction process, inert gas is introduced into the extraction system every 30-40 minutes, the inert gas is nitrogen, and the gas flow rate is 0.5-1 L / min, so as to prevent the oxidation and degradation of the effective components.