CN114931556B - Preparation method of cattail pollen charcoal formula particles - Google Patents
Preparation method of cattail pollen charcoal formula particles Download PDFInfo
- Publication number
- CN114931556B CN114931556B CN202210672342.2A CN202210672342A CN114931556B CN 114931556 B CN114931556 B CN 114931556B CN 202210672342 A CN202210672342 A CN 202210672342A CN 114931556 B CN114931556 B CN 114931556B
- Authority
- CN
- China
- Prior art keywords
- cattail pollen
- decoction
- charcoal
- pollen charcoal
- charcoal formula
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
- A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
- A61K9/1605—Excipients; Inactive ingredients
- A61K9/1629—Organic macromolecular compounds
- A61K9/1652—Polysaccharides, e.g. alginate, cellulose derivatives; Cyclodextrin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/88—Liliopsida (monocotyledons)
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Landscapes
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Life Sciences & Earth Sciences (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Chemical & Material Sciences (AREA)
- Epidemiology (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- Medicinal Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Pharmacology & Pharmacy (AREA)
- Alternative & Traditional Medicine (AREA)
- Mycology (AREA)
- Microbiology (AREA)
- Medical Informatics (AREA)
- Botany (AREA)
- Biotechnology (AREA)
- Carbon And Carbon Compounds (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses a preparation method of cattail pollen charcoal formula particles, which comprises the following steps: (1) decocting; (2) preliminary impurity removal: (3) centrifuging; (4) dynamic high pressure microfluidic treatment; (5) granulating. The formula particles prepared by the invention avoid the defects of overhigh plaster yield and low content of active ingredients of decoction pieces in the preparation process, and effectively improve the dissolution stability of the cattail pollen charcoal formula particles in water. The cattail pollen charcoal formula particles prepared by the invention have the characteristic of quick solubility, and the uniformity degree of the effective components in the cattail pollen charcoal formula particles is strong.
Description
Technical Field
The invention relates to the technical field of preparation of traditional Chinese medicine granules, in particular to a preparation method of cattail pollen charcoal formula granules.
Background
The pollen Typhae charcoal is prepared by parching dried pollen of Typhae (Typha angustifolia L.) belonging to Typhaceae. The main ingredients of the cattail pollen are typhin, isorhamnetin, fatty oil, yellow pigment and the like, and the cattail pollen has the effects of stopping bleeding, removing blood stasis and treating stranguria. Modern medical research shows that the cattail pollen charcoal has an inhibition effect on in vitro tumor cells. The cattail pollen charcoal water extract or 5% ethanol extract can obviously shorten the blood coagulation time of rabbits, and the cattail pollen charcoal powder can treat blood loss after being decocted.
The dynamic high-pressure micro-jet technology is an environment-friendly continuous physical modification method, and is a modern novel treatment technology integrating multiple unit operations such as conveying, mixing, high-pressure, high-speed impact, shearing and the like, and the particle size of materials is dispersed to the nanometer level, and the particle size distribution is uniform after homogenization. The method has wide application range, and can be used for homogeneously dispersing emulsion, dispersion liquid, suspension liquid and the like in various industries, in particular to research and preparation of nano-drug preparations.
The traditional Chinese medicine formula granule is a novel formula medicine with unified specification, unified dosage and unified quality standard, which is prepared by taking traditional Chinese medicine decoction pieces as raw materials through the production processes of extraction, separation, concentration, drying, granulation, packaging and the like. The traditional Chinese medicine formula particles can replace traditional decoction pieces for a middle doctor to treat according to the syndrome differentiation, increase and decrease the requirements along with symptoms, and have the characteristics of convenient carrying, small administration dosage, safety, stability and the like. At present, the pollen typhae charcoal formula particles have the conditions of over-high paste yield, over-low content of active ingredients and uneven distribution in the particles in the production process. Therefore, controlling the paste yield of the cattail pollen charcoal medicinal material decoction pieces, stabilizing the content and uniformity of active ingredients in the particles becomes an important means for guaranteeing the clinically effective application of the cattail pollen charcoal formula particles. In addition, the traditional cattail pollen charcoal formula particles can have obvious precipitation and layering phenomena after being dissolved in pure water, so that the taking experience of patients is affected, and the improvement of the dissolution stability of the cattail pollen charcoal formula particles is one of the problems to be solved urgently.
Disclosure of Invention
The invention aims to provide a preparation method of cattail pollen charcoal formula particles, which aims to solve the technical problems.
The technical scheme provided by the invention is as follows:
a preparation method of cattail pollen charcoal formula particles comprises the following steps:
step one, decocting: firstly, weighing a proper amount of cattail pollen charcoal medicinal material decoction pieces, wrapping the decoction pieces by using a non-woven fabric bag in a double-layer manner, adding pure water with the mass of 5-20 times of the medicinal material, soaking for 30-60min before first decoction, decocting for 2 times, each time for 20-90min, and combining the decoctions;
step two, preliminary impurity removal: standing the decoction at 4-15deg.C for 24-96 hr, collecting upper layer liquid, and discarding lower layer precipitate;
step three, centrifuging: the upper liquid obtained in the second step is put into a centrifugal machine, the centrifugal speed is 4500-10000r/min, the centrifugal time is 5-30min, and the liquid after the centrifugation is collected and put into a filter bag with 200-400 meshes to obtain filtrate;
step four, dynamic high-pressure micro-jet treatment: carrying out high-pressure microjet treatment on the filtrate obtained in the step three for 5-25 times under the condition of treatment pressure of 50-180MPa, collecting the treated liquid, concentrating, and drying to obtain pollen typhae carbon dry paste powder;
step five, granulating: adding medicinal maltodextrin, dextrin or soluble starch with the mass of 30-75% of that of the dry paste powder into the obtained dry paste powder, granulating, drying and finishing to obtain the pollen typhae charcoal formula granules.
Preferably, in the first step, the decocting condition is 2 times, each time of decocting is 60min, the ratio of decoction pieces of medicinal materials to pure water is 1:14, and the decoction pieces are soaked in advance for 40min before the first time of decoction.
Preferably, in the second step, the standing temperature is 10 ℃ and the standing time is 24 hours.
Preferably, in the third step, the centrifugal speed is 5500r/min and the centrifugal time is 10min.
Preferably, in the third step, the mesh number of the filter bags is 200 mesh.
Preferably, in the fourth step, the dynamic high-pressure micro-jet treatment pressure is 100MPa, and the treatment times are 10 times.
Preferably, in the fifth step, the auxiliary materials are medicinal maltodextrin and soluble starch, and the total addition amount of the medicinal maltodextrin and the soluble starch is 69% of the mass of the dry pollen typhae carbon paste powder.
Preferably, in the fifth step, the extract yield of the cattail pollen charcoal decoction pieces is 8.0%, the extract is 18.4%, and each 1g of cattail pollen charcoal formula granule contains typhonine (C 34 H 42 O 20 ) And isorhamnetin-3-O-neohesperidin (C) 28 H 32 O 16 ) The total amount was 6.6mg.
The invention has the beneficial effects that:
1. compared with the traditional mode of directly decocting decoction pieces, the cattail pollen charcoal formula granule prepared by the invention has the characteristics of instant use, small volume, definite dosage and convenient application and carrying, is convenient for middle doctors to clinically and dialectically treat and use, and ensures the consistency of the dosage each time during clinical treatment.
2. According to the invention, impurities in the cattail pollen charcoal decoction are removed by preliminary standing, impurity removal, centrifugation and filter bag permeation, so that the paste yield of decoction pieces is reduced, and the content of active ingredients in the formula particles is improved.
3. The invention uses dynamic high-pressure micro-jet technology to make the content of active ingredient in the formula granule uniform, and can maintain stability for a long time after rapidly dissolving in pure water at normal temperature.
Drawings
FIG. 1 is a characteristic map of a reference medicinal material of pollen Typhae charcoal;
FIG. 2 is a characteristic spectrum of the cattail pollen charcoal formulation granule in each of the examples and comparative examples;
FIG. 3 is a liquid chromatogram of a control solution;
FIG. 4 is a liquid chromatogram of a cattail pollen charcoal formulation in various examples;
FIG. 5 is a liquid chromatogram of the pollen Typhae charcoal formulation in each comparative example.
Detailed Description
Example 1
The embodiment discloses a preparation method of cattail pollen charcoal formula particles, which comprises the following specific steps:
(1) Firstly, 7300g of cattail pollen charcoal decoction pieces are weighed, double-layer wrapped by a non-woven fabric bag, then pure water with the mass of 12 times of that of the medicinal materials is added, soaked for 30min before the first decoction, decocted for 2 times, decocted for 60min each time, and the decoction is combined.
(2) Standing the decoction at 10deg.C for 24 hr, collecting upper liquid, and discarding lower precipitate. And then the obtained upper layer liquid is put into a centrifugal machine, the centrifugal speed is 4500r/min, the centrifugal time is 10min, and the liquid after the centrifugal is collected and is put into a 300-mesh filter bag to obtain filtrate.
(3) Carrying out high-pressure microjet treatment on the obtained filtrate for 10 times under the condition of treatment pressure of 100MPa, collecting the treated liquid, and drying to obtain the pollen typhae carbon dry paste powder. And finally, adding medicinal maltodextrin accounting for 25% of the mass of the dry paste powder and soluble starch accounting for 44% of the mass of the dry paste powder into the obtained dry paste powder, granulating, drying and finishing to obtain the cattail pollen charcoal formula granules.
Example 2
The embodiment discloses a preparation method of cattail pollen charcoal formula particles, which comprises the following specific steps:
(1) Firstly, 7300g of cattail pollen charcoal decoction pieces are weighed, double-layer wrapped by a non-woven fabric bag, then pure water with the mass 10 times of that of the medicinal materials is added, soaked for 30min before the first decoction, decocted for 2 times, decocted for 65min each time, and the decoction is combined.
(2) Standing the decoction at 4deg.C for 36 hr, collecting upper liquid, and discarding lower precipitate. And then the obtained upper layer liquid is put into a centrifugal machine, the centrifugal speed is 6500r/min, the centrifugal time is 12min, and the liquid after the centrifugal is collected and is put into a 300-mesh filter bag to obtain filtrate.
(3) Carrying out high-pressure microjet treatment on the obtained filtrate for 10 times under the condition of treatment pressure of 150MPa, collecting the treated liquid, and drying to obtain the pollen typhae carbon dry paste powder. And finally, adding medicinal maltodextrin accounting for 35% of the mass of the dry paste powder and soluble starch accounting for 30% of the mass of the dry paste powder into the obtained dry paste powder, granulating, drying and finishing to obtain the cattail pollen charcoal formula granules.
Example 3
The embodiment discloses a preparation method of cattail pollen charcoal formula particles, which comprises the following specific steps:
(1) Firstly, 7300g of cattail pollen charcoal decoction pieces are weighed, double-layer wrapped by a non-woven fabric bag, then pure water with the mass 15 times of that of the medicinal materials is added, soaked for 30min before the first decoction, decocted for 2 times, decocted for 50min each time, and the decoction is combined.
(2) Standing the decoction at 8deg.C for 48 hr, collecting upper liquid, and discarding lower precipitate. And then the obtained upper layer liquid is put into a centrifugal machine, the centrifugal speed is 8000r/min, the centrifugal time is 15min, and the liquid after the centrifugal is collected and filtered by a 400-mesh filter bag to obtain filtrate.
(3) Carrying out high-pressure microjet treatment on the obtained filtrate for 15 times under the condition of treatment pressure of 50MPa, collecting the treated liquid, and drying to obtain the pollen typhae carbon dry paste powder. And finally, adding medicinal maltodextrin accounting for 40% of the mass of the dry paste powder and soluble starch accounting for 29% of the mass of the dry paste powder into the obtained dry paste powder, granulating, drying and finishing to obtain the cattail pollen charcoal formula granules.
Comparative example 1
The procedure of example 1 was followed in this comparative example, except for the preliminary removal of impurities, centrifugation and dynamic high pressure microfluidization treatment steps, the remaining steps being unchanged, as follows:
(1) Firstly, 7300g of cattail pollen charcoal decoction pieces are weighed, double-layer wrapped by a non-woven fabric bag, then pure water with the mass of 12 times of that of the medicinal materials is added, soaked for 30min before the first decoction, decocted for 2 times, decocted for 60min each time, and the decoction is combined.
(2) Concentrating the decoction directly, and drying to obtain pollen Typhae charcoal dry extract powder. And finally, adding medicinal maltodextrin accounting for 25% of the mass of the dry paste powder and soluble starch accounting for 44% of the mass of the dry paste powder into the obtained dry paste powder, granulating, drying and finishing to obtain the cattail pollen charcoal formula granules.
Comparative example 2
In this comparative example, the dynamic high pressure microfluidic treatment step was removed, the remaining steps were unchanged, and the specific steps were as follows:
(1) Firstly, 7300g of cattail pollen charcoal decoction pieces are weighed, double-layer wrapped by a non-woven fabric bag, then pure water with the mass of 12 times of that of the medicinal materials is added, soaked for 30min before the first decoction, decocted for 2 times, decocted for 60min each time, and the decoction is combined.
(2) Standing the decoction at 10deg.C for 24 hr, collecting upper liquid, and discarding lower precipitate. And then the obtained upper layer liquid is put into a centrifugal machine, the centrifugal speed is 4500r/min, the centrifugal time is 10min, and the liquid after the centrifugal is collected and is put into a 300-mesh filter bag to obtain filtrate.
(3) Directly concentrating the obtained filtrate, and drying to obtain pollen Typhae dry extract powder. And finally, adding medicinal maltodextrin accounting for 25% of the mass of the dry paste powder and soluble starch accounting for 44% of the mass of the dry paste powder into the obtained dry paste powder, granulating, drying and finishing to obtain the cattail pollen charcoal formula granules.
Test examples
1. Determination of paste yield of cattail pollen charcoal decoction pieces
Paste yield = (m×v)/(m×v) ×100%
Wherein M represents the mass (g) of the dry paste, V represents the sampling volume (mL), M represents the initial mass (g) of the decoction pieces, and V represents the volume (mL) of the water decoction.
The paste yield of the cattail pollen charcoal decoction pieces in the different examples and comparative examples is shown in table 1.
TABLE 1 paste yield for cattail pollen charcoal decoction pieces in different examples and comparative examples
As can be seen from Table 1, the paste yield of the cattail pollen charcoal decoction pieces in each example is between 6.9% and 10.7%, which meets the requirements in the claims, and the comparative example 1 compared with the example 1 has no preliminary impurity removal, centrifugation and dynamic high-pressure microjet treatment steps, so that the paste yield exceeds the requirements in the paste yield range. In addition, comparative example 2 showed no significant change in paste yield compared to example 1, indicating that the dynamic high pressure microfluidic treatment did not change the paste yield.
2. Different examples and comparative examples of the extract from the cattail pollen charcoal formulation
The alcohol-soluble extract was measured by hot dipping under the condition of the general rule 2201 of the fourth edition of the Chinese pharmacopoeia 2020, and ethanol was used as a solvent.
Table 2 extract conditions of the cattail pollen charcoal formulations of the various examples and comparative examples
As can be seen from Table 2, the extract of the cattail pollen charcoal decoction pieces in each of the examples and comparative examples is higher than 10%, which meets the requirements in the claims.
3. Method for measuring content of active ingredients of cattail pollen charcoal formula particles in different examples and comparative examples
3.1 chromatographic conditions and System applicability test
Octadecylsilane chemically bonded silica is used as filler (column length is 100mm, inner diameter is 2.1mm, and particle diameter is 1.8 μm); acetonitrile is taken as a mobile phase A, 0.1% glacial acetic acid solution is taken as a mobile phase B, and gradient elution is carried out according to the specification in the following table; the flow rate is 0.3ml per minute; the column temperature is 30 ℃; the detection wavelength was 254nm. The theoretical plate number is calculated by isorhamnetin-3-O-new orange Pi Ganfeng to be not less than 5000.
3.2 preparation of control solution
Taking proper amounts of isorhamnetin-3-O-neohesperidin reference substance and typhonine reference substance, precisely weighing, adding methanol to prepare a mixed solution containing 25 mug isorhamnetin-3-O-neohesperidin and 25 mug typhonine per 1 ml.
3.3 preparation of sample solutions
Grinding the product, taking about 0.2g, precisely weighing, placing into a conical flask with a plug, precisely adding 25ml of 30% methanol, sealing, weighing, performing ultrasonic treatment (power 250W, frequency 40 kHz) for 30 minutes, cooling, weighing again, supplementing the lost weight with 30% methanol, shaking, filtering, and collecting the subsequent filtrate.
3.4 assay
Precisely sucking 2 μl of each of the control solution and the sample solution, and measuring with a liquid chromatograph.
3.5 analysis of measurement results
Table 3 data relating to the determination of the particle content of the cattail pollen charcoal formulation in each of the examples and comparative examples
As can be seen from the results of FIGS. 3-5 and Table 3, the content of the pollen Typhae charcoal formulation particles in each example is in the range of 1.0 mg/g-13.0 mg/g, which meets the requirements. Comparative example 1 compared with example 1, the content thereof was far below the lower limit of the required value of the content range because of not using the preliminary impurity removal, centrifugation and dynamic high pressure micro-jet treatment steps in the present invention. In addition, comparative example 2 showed no significant change in the content as compared with example 1, indicating that the dynamic high pressure microfluidic treatment did not change the content of the finite element in the particles. .
4. Characteristic spectrum conditions of cattail pollen charcoal formula granules in different examples and comparative examples
4.1 chromatographic conditions and System applicability test
Octadecylsilane chemically bonded silica is used as filler (column length is 100mm, inner diameter is 2.1mm, and particle diameter is 1.8 μm); acetonitrile is taken as a mobile phase A, 0.1% glacial acetic acid solution is taken as a mobile phase B, and gradient elution is carried out according to the specification in the following table; the flow rate is 0.3ml per minute; the column temperature is 30 ℃; the detection wavelength was 254nm. The theoretical plate number is calculated by isorhamnetin-3-O-new orange Pi Ganfeng to be not less than 5000.
4.2 preparation of reference solutions
Taking 0.5g of pollen typhae reference medicine, placing the pollen typhae reference medicine into a conical flask with a plug, adding 25mL of water, heating and refluxing for 60 minutes, cooling, shaking uniformly, filtering, and taking the subsequent filtrate as a reference substance solution of the reference medicine. And taking the reference substance solution under the condition of content measurement as the reference substance solution of the reference substance. And then taking proper amounts of p-hydroxybenzoic acid reference substance, quercetin-3-O-neohesperidin reference substance and kaempferol-3-O-neohesperidin reference substance, and respectively adding methanol to prepare solutions containing 10 mug of p-hydroxybenzoic acid, 25 mug of quercetin-3-O-neohesperidin and 25 mug of kaempferol-3-O-neohesperidin per 1mL of the reference substance reference solution.
4.3 preparation of sample solutions
Grinding the product, taking about 0.2g, precisely weighing, placing into a conical flask with a plug, precisely adding 25ml of 30% methanol, sealing, weighing, performing ultrasonic treatment (power 250W, frequency 40 kHz) for 30 minutes, cooling, weighing again, supplementing the lost weight with 30% methanol, shaking, filtering, and collecting the subsequent filtrate.
4.4 assay
Precisely sucking 2 μl of each of the reference solution and the sample solution, and measuring with a liquid chromatograph. The sample chromatogram should show 8 characteristic peaks, and the retention time of 8 characteristic peaks in the control reference chromatogram should correspond to that of the control reference chromatogram. Wherein 5 peaks should correspond to the retention times of the corresponding reference peaks, respectively; the peak corresponding to typha neoglycoside reference substance is S peak, and the relative retention time of the rest characteristic peaks and S peak is calculated, wherein the relative retention time is within +/-10% of the specified value. The specified value is: 0.68 (Peak 2), 0.88 (Peak 3), 0.98 (Peak 5).
4.5 analysis of measurement results
TABLE 4 relative retention time for various peaks of cattail pollen charcoal formulas in various examples and comparative examples
As can be seen from fig. 1, fig. 2 and table 4, the characteristic spectrum of the cattail pollen charcoal formulation granule in each example and comparative example presents 8 characteristic peaks, which correspond to the retention time of 8 characteristic peaks in the chromatogram of the reference substance of the comparative medicinal material, and the relative retention time of each peak is in a range and meets the requirements.
5. Dissolution stability of cattail pollen charcoal formulation granules in different examples and comparative examples
And respectively taking a proper amount of cattail pollen charcoal formula particles in each example and comparative example, dissolving the cattail pollen charcoal formula particles in sterile pure water at 20 ℃, keeping the temperature in a sterile environment, standing, and observing the stability of the solution at intervals.
Table 5 dissolution stability of the cattail pollen charcoal formulation granules in each of the examples and comparative examples
As can be seen from Table 5, the cattail pollen charcoal formulation granule solution of example 1 did not precipitate or delaminate over time, whereas the comparative example did precipitate or delaminate. However, the delamination phenomenon in comparative example 2 was later than comparative example 1, which indicates that the preliminary impurity removal and centrifugation have an effect of delaying the occurrence time of the delamination phenomenon, but the problem could not be fundamentally solved. Compared with comparative example 2, the dynamic high-pressure micro-jet treatment has no sedimentation and layering phenomenon after the time is prolonged, which shows that the dynamic high-pressure micro-jet treatment can obviously improve the stability of the cattail pollen charcoal formula granule solution and prevent the layering and sedimentation phenomenon of the solution.
Based on the data analysis results, the cattail pollen charcoal formula particles prepared in the embodiment of the invention have higher content of active ingredients and better dissolution stability in pure water. On the other hand, the cattail pollen charcoal formula granule prepared by the invention has definite dosage, is convenient to apply and carry, is convenient for middle doctors to clinically and dialectically treat and use, and can ensure the consistency of the dosage of each time in clinical treatment. In summary, the foregoing embodiments are merely illustrative of the preferred embodiments of the present invention and do not include all embodiments of the invention. Various modifications and changes may be made by one skilled in the art without departing from the spirit and scope of the invention, which is therefore intended to be covered by the appended claims.
Claims (6)
1. A preparation method of cattail pollen charcoal formula particles is characterized in that: the method comprises the following steps:
step one, decocting: firstly, weighing cattail pollen charcoal decoction pieces, decocting the decoction pieces by using a non-woven fabric bag in a double-layer manner, and adding pure water for boiling to obtain decoction;
step two, preliminary impurity removal: standing the decoction at lower temperature for a period of time, collecting upper layer liquid, and discarding lower layer precipitate; the standing temperature is 4-15 ℃, and the standing time is 24-96 h;
step three, centrifuging: the upper liquid obtained in the second step is put into a centrifugal machine, and the liquid after the centrifugal is collected and filtered through a filter bag to obtain filtrate; the centrifugal speed is 4500-10000r/min, and the centrifugal time is 5-30 min;
step four, dynamic high-pressure micro-jet treatment: carrying out dynamic high-pressure micro-jet treatment on the filtrate in the step three, concentrating, and drying to obtain pollen typhae carbon dry paste powder; the dynamic high-pressure microjet treatment pressure is 50-180MPa, and the treatment times are 5-25 times;
step five, granulating: adding adjuvants into the obtained dry extract powder, granulating, drying, and grading to obtain pollen Typhae charcoal granule.
2. The method for preparing the cattail pollen charcoal formula granule according to claim 1, which is characterized in that: in the first step, the decoction condition is 1-3 times of decoction, the time of each decoction is 20-90min, the ratio of each decoction piece of medicinal materials to pure water is 1:5-20, and the decoction pieces of medicinal materials are soaked in advance for 30-60min before the first decoction.
3. The method for preparing the cattail pollen charcoal formula granule according to claim 1, which is characterized in that: in the third step, the mesh number of the filter bags is 200-400 meshes.
4. The method for preparing the cattail pollen charcoal formula granule according to claim 1, which is characterized in that: in the fifth step, the auxiliary materials are medicinal maltodextrin, dextrin or soluble starch, and the addition amount of the auxiliary materials is 30% -75% of the mass of the dry pollen typhae carbon paste powder.
5. The method for preparing the cattail pollen charcoal formula granule according to claim 1, which is characterized in that: in the fifth step, the paste yield of the cattail pollen charcoal decoction pieces is 6.9% -10.7%, the extract content of the cattail pollen charcoal formula granule is more than or equal to 10.0%, and every 1g of the cattail pollen charcoal formula granule contains typhonine (C) 34 H 42 O 20 ) And isorhamnetin-3-ONeohesperidin (C) 28 H 32 O 16 ) The total amount is 1.0mg to 13.0 mg.
6. The method for preparing the cattail pollen charcoal formula granule according to claim 1, which is characterized in that: in the fifth step, the cattail pollen charcoal formula particles are dissolved in pure water at 20 ℃, and no precipitation and layering phenomenon occur after standing for 24 and h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210672342.2A CN114931556B (en) | 2022-06-15 | 2022-06-15 | Preparation method of cattail pollen charcoal formula particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210672342.2A CN114931556B (en) | 2022-06-15 | 2022-06-15 | Preparation method of cattail pollen charcoal formula particles |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114931556A CN114931556A (en) | 2022-08-23 |
| CN114931556B true CN114931556B (en) | 2023-07-25 |
Family
ID=82866362
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210672342.2A Active CN114931556B (en) | 2022-06-15 | 2022-06-15 | Preparation method of cattail pollen charcoal formula particles |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114931556B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20070109426A (en) * | 2006-05-11 | 2007-11-15 | 한불화장품주식회사 | A cosmetic composition containing an extract of typhae pollen |
| CN105241997A (en) * | 2015-11-10 | 2016-01-13 | 广东一方制药有限公司 | Thin-layer chromatography identification method of carbon traditional Chinese medicine formula granules |
| CN109170532A (en) * | 2018-09-10 | 2019-01-11 | 福建拓天生物科技有限公司 | A kind of preparation method and application of Semen Coicis extract |
| CN114403392A (en) * | 2022-01-26 | 2022-04-29 | 西南大学 | Preparation method of instant winter jujube powder and product thereof |
-
2022
- 2022-06-15 CN CN202210672342.2A patent/CN114931556B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20070109426A (en) * | 2006-05-11 | 2007-11-15 | 한불화장품주식회사 | A cosmetic composition containing an extract of typhae pollen |
| CN105241997A (en) * | 2015-11-10 | 2016-01-13 | 广东一方制药有限公司 | Thin-layer chromatography identification method of carbon traditional Chinese medicine formula granules |
| CN109170532A (en) * | 2018-09-10 | 2019-01-11 | 福建拓天生物科技有限公司 | A kind of preparation method and application of Semen Coicis extract |
| CN114403392A (en) * | 2022-01-26 | 2022-04-29 | 西南大学 | Preparation method of instant winter jujube powder and product thereof |
Non-Patent Citations (2)
| Title |
|---|
| Evaluation of ant i-inflammatory activity of Typha angustifolia pollen grains extracts in experimental animals;Saroj S. Varpe等;《Indian Journal of Pharmacology》;第44卷(第6期);第788-791页 * |
| 蒲黄配方颗粒质量标准的研究;刘斌等;《中成药》;第25卷(第8期);第624-626页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114931556A (en) | 2022-08-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108355047B (en) | Preparation process of lily and rehmannia decoction solid preparation | |
| CN108578375B (en) | Preparation process of licorice heart-fire-purging decoction solid preparation | |
| CN102327401B (en) | Method for preparing medicament for treating uterine bleeding | |
| CN114931556B (en) | Preparation method of cattail pollen charcoal formula particles | |
| CN107496375A (en) | A kind of preparation method of herbal mixture granule | |
| Koo et al. | Extraction of hypotensive principles from seeds of Cassia tora | |
| CN101439134A (en) | Method for preparing Chinese medicine preparation | |
| CN113769023B (en) | A Chinese medicinal composition for treating hypertension and its quality detection method | |
| CN1698774A (en) | Chinese medicinal soft capsule with heat-clearing toxin-removing function and its preparation process | |
| CN112724192B (en) | Method for extracting and preparing aescine sodium from buckeye seeds | |
| CN102228495A (en) | Preparation method of injection for treating cardio-cerebral vascular diseases | |
| CN113616596B (en) | Paclitaxel liposome pharmaceutical composition and preparation method thereof | |
| CN106492129A (en) | A kind of preparation method of reducing swelling and alleviating pain Chinese medicine composition | |
| CN110123901B (en) | Preparation method of Sihuang heart-clearing concentrated pills | |
| CN106943354A (en) | A kind of preparation method of novel biochemical particles | |
| CN113230309A (en) | Ephedra-cassia twig pair traditional Chinese medicine formula granule and preparation method thereof | |
| CN102048843A (en) | Qingpeng emplastrum for reducing swelling and stopping pain and preparation method thereof | |
| CN117618361A (en) | Lygodium japonicum traditional Chinese medicine formula granule and preparation method thereof | |
| CN115671055B (en) | Preparation method of traditional Chinese medicine granule and traditional Chinese medicine granule | |
| CN105079134A (en) | Preparation process of traditional Chinese medicine preparation used for treating cold and application of traditional Chinese medicine preparation | |
| WO2019205959A1 (en) | Pharmaceutical composition for treating epilepsy and convulsions, infantile convulsions and facial spasms and preparation method therefor | |
| CN105079135B (en) | A kind of Chinese medicine composition and preparation method thereof for treating flu | |
| CN114306415B (en) | Preparation method for improving content of index component in pulp powder of dogwood fruit | |
| CN112915066B (en) | Glabrous sarcandra herb formula granules and preparation method thereof | |
| CN107951959A (en) | A kind of callicarpa nudiflora plastics and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |