CN117064939B - Pudi blue anti-inflammatory capsule and preparation method thereof - Google Patents

Pudi blue anti-inflammatory capsule and preparation method thereof Download PDF

Info

Publication number
CN117064939B
CN117064939B CN202311176697.3A CN202311176697A CN117064939B CN 117064939 B CN117064939 B CN 117064939B CN 202311176697 A CN202311176697 A CN 202311176697A CN 117064939 B CN117064939 B CN 117064939B
Authority
CN
China
Prior art keywords
extract
inflammatory
cattail
filtrate
preparation
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
Application number
CN202311176697.3A
Other languages
Chinese (zh)
Other versions
CN117064939A (en
Inventor
江秀山
蔡荣钦
张秋裕
胡杰雄
戴荣俭
吴丽琼
胡宏军
林琼英
李洁旋
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Guangdong Xinbao Pharmaceutical Technology Co ltd
Original Assignee
Guangdong Xinbao Pharmaceutical Technology Co ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Guangdong Xinbao Pharmaceutical Technology Co ltd filed Critical Guangdong Xinbao Pharmaceutical Technology Co ltd
Priority to CN202311176697.3A priority Critical patent/CN117064939B/en
Publication of CN117064939A publication Critical patent/CN117064939A/en
Application granted granted Critical
Publication of CN117064939B publication Critical patent/CN117064939B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/53Lamiaceae or Labiatae (Mint family), e.g. thyme, rosemary or lavender
    • A61K36/539Scutellaria (skullcap)
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/19Acanthaceae (Acanthus family)
    • A61K36/195Strobilanthes
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/28Asteraceae or Compositae (Aster or Sunflower family), e.g. chamomile, feverfew, yarrow or echinacea
    • A61K36/288Taraxacum (dandelion)
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/31Brassicaceae or Cruciferae (Mustard family), e.g. broccoli, cabbage or kohlrabi
    • A61K36/315Isatis, e.g. Dyer's woad
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/66Papaveraceae (Poppy family), e.g. bloodroot
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/14Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A61K9/16Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
    • A61K9/1605Excipients; Inactive ingredients
    • A61K9/1617Organic compounds, e.g. phospholipids, fats
    • A61K9/1623Sugars or sugar alcohols, e.g. lactose; Derivatives thereof; Homeopathic globules
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/14Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A61K9/16Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
    • A61K9/1605Excipients; Inactive ingredients
    • A61K9/1629Organic macromolecular compounds
    • A61K9/1652Polysaccharides, e.g. alginate, cellulose derivatives; Cyclodextrin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P11/00Drugs for disorders of the respiratory system
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P11/00Drugs for disorders of the respiratory system
    • A61P11/04Drugs for disorders of the respiratory system for throat disorders
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P29/00Non-central analgesic, antipyretic or antiinflammatory agents, e.g. antirheumatic agents; Non-steroidal antiinflammatory drugs [NSAID]
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P31/00Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
    • A61P31/12Antivirals
    • A61P31/14Antivirals for RNA viruses
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P39/00General protective or antinoxious agents
    • A61P39/02Antidotes
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/10Preparation or pretreatment of starting material
    • A61K2236/19Preparation or pretreatment of starting material involving fermentation using yeast, bacteria or both; enzymatic treatment
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/331Extraction 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
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30Against 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)
  • Natural Medicines & Medicinal Plants (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Veterinary Medicine (AREA)
  • Chemical & Material Sciences (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Public Health (AREA)
  • General Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Animal Behavior & Ethology (AREA)
  • Engineering & Computer Science (AREA)
  • Epidemiology (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • Botany (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Microbiology (AREA)
  • Medical Informatics (AREA)
  • Biotechnology (AREA)
  • Alternative & Traditional Medicine (AREA)
  • Mycology (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Pulmonology (AREA)
  • Virology (AREA)
  • Molecular Biology (AREA)
  • Neurosurgery (AREA)
  • Rheumatology (AREA)
  • Toxicology (AREA)
  • Otolaryngology (AREA)
  • Pain & Pain Management (AREA)
  • Biophysics (AREA)
  • Communicable Diseases (AREA)
  • Oncology (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The invention provides a cattail-basket anti-inflammatory capsule and a preparation method thereof, comprising the following steps: (1) weighing radix scutellariae, radix isatidis, herba violae and dandelion; (2) Mixing radix Isatidis, herba Violae and herba Taraxaci, pulverizing, adding water, adding compound enzyme composed of cellulase, pectase and hemicellulase, adjusting pH, extracting, filtering to obtain filtrate, and concentrating the filtrate to obtain extract A; (3) Pulverizing radix Scutellariae to obtain coarse powder, adding water, adjusting pH with HCl, and extracting under heat preservation for 1.5-3 hr; then adjusting the pH value by NaOH, extracting for 1.5-3 hours under heat preservation, filtering to obtain filtrate, and concentrating the filtrate to obtain extract B; (4) Mixing the extract A and the extract B with appropriate amount of adjuvants, and making into Typhonium giganteum anti-inflammatory capsule. The preparation method of the invention does not involve the use of organic solvents, can effectively extract anti-inflammatory active ingredients of the medicinal materials with the whole formula, and the prepared cattail blue anti-inflammatory capsule has high content of the active ingredients.

Description

Pudi blue anti-inflammatory capsule and preparation method thereof
Technical Field
The invention belongs to the technical field of traditional Chinese medicine extracts, and in particular relates to a cattail-basket anti-inflammatory capsule and a preparation method thereof.
Background
The cattail herba isatidis anti-inflammatory preparation is a traditional Chinese patent medicine for clearing heat and detoxicating, the dandelion, the bunge corydalis herb and the radix isatidis in the formula have the effects of clearing heat and detoxicating, relieving swelling and relieving sore throat, the baikal skullcap root has the effects of clearing heat and drying dampness, cooling blood and stopping bleeding, and 4 medicines are used together to play roles of clearing heat and detoxicating, relieving sore throat and relieving swelling. In clinical use, compared with the Pu Di lan anti-inflammatory tablet, the Pu Di lan anti-inflammatory capsule has higher bioavailability, quick response, and can mask the bad smell of the medicine, improve the taste of the medicine and improve the compliance of patients. The cattail blue anti-inflammatory capsule has remarkable anti-inflammatory effect and higher application value.
The content measurement item of the Pudilan anti-inflammatory capsule is specified in the 2020 edition of Chinese pharmacopoeia, and takes baicalin of baikal skullcap root and chicoric acid of dandelion as control standards, while the effective components R, S- of radix isatidis and herba violae are mainly identified qualitatively. That is, the active ingredients of the radix isatidis and the herba violae in the cattail-herba anti-inflammatory capsules in the current stage lack quantitative standards, and the content control of the active ingredients is often easily ignored, so that the overall anti-inflammatory activity of the product is affected. In addition, the process parameters and internal control standards of different manufacturers are different, so that the problems of low content of active ingredients, poor preparation stability and the like of the commercial products are easily caused. Based on the above, it is necessary to research a preparation technology of the cattail blue anti-inflammatory capsule, so that the anti-inflammatory active ingredients of the whole prescription can be retained to the greatest extent in the preparation process, and the content of the anti-inflammatory active ingredients is further improved, so that the whole anti-inflammatory curative effect of the product can be fully exerted. In addition, how to better absorb the active ingredients of the cattail blue anti-inflammatory capsules by human bodies is also a problem to be solved.
Disclosure of Invention
The invention aims to provide a cattail-blue anti-inflammatory capsule and a preparation method thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
a method for preparing a cattail blue anti-inflammatory capsule, which comprises the following steps:
(1) 1 to 6 weight portions of baical skullcap root, indigowoad root, kudingchun herb and dandelion are weighed according to the weight ratio of 1 to 3;
(2) Mixing radix Isatidis, herba Violae and herba Taraxaci, pulverizing to 30-60 mesh, adding 10-12 times of water, adding compound enzyme composed of cellulase, pectase and hemicellulase, adjusting pH to 3.5-4, extracting at 35-42deg.C for 4-8 h, filtering to obtain filtrate, concentrating the filtrate to obtain extract A;
(3) Pulverizing radix Scutellariae to 80-100 meshes to obtain coarse powder of radix Scutellariae, adding 6-10 times of water, adjusting pH to 5.5-6.5 with HCl, heating to 100deg.C, and extracting for 1.5-3 hr; then adjusting the pH value to 7-9 by NaOH, extracting at 100 ℃ for 1.5-3 hours, filtering to obtain filtrate, and concentrating the filtrate to obtain extract B;
(4) Mixing the extract A and the extract B with appropriate amount of adjuvants, drying to obtain granule, and encapsulating to obtain the final product.
Further, in the step (1), the weight ratio of the baical skullcap root, the isatis root, the kudingchoffa herb and the dandelion is 1.5:1.5:1:4.
Further, the weight ratio of the cellulase, the pectase and the hemicellulase in the step (2) is (1-5) 1: (0.2-0.6).
When the invention is used for extracting the isatis root, the bunge corydalis herb and the dandelion, the three enzymes are compounded for enzymolysis, so that the content of effective active ingredients in the extracting solution is improved. The hypothesis is that cellulase, pectase and hemicellulase decompose plant tissues of radix Isatidis, herba Violae and herba Taraxaci, and transfer some insoluble active ingredients into water, and have synergistic effect. However, the enzymes of different types have optimal enzymolysis temperature and pH value, and a large number of experiments are carried out to obtain the optimal enzymolysis temperature and pH value. The inventors have also found that when the weight ratio of cellulase, pectinase and hemicellulase is (1-5): 1: (0.2-0.6), the medicinal effect of the cattail blue anti-inflammatory capsule takes effect more rapidly. The invention discloses a method for preparing a cattail-herba-like anti-inflammatory capsule, which comprises the steps of preparing a cattail-herba-like anti-inflammatory capsule, wherein the cattail-herba-like anti-inflammatory capsule comprises three plants, namely, a cell structure of the three plants, namely, isatis root, bunge corydalis herb and dandelion, is complex, and enzyme is compounded according to a proper proportion, so that cellulose, hemicellulose, pectin and other substances in cell walls and cell interstitium of the isatis root, the bunge corydalis herb and the dandelion are fully degraded, the compact structure of the cell walls is destroyed, the mass transfer resistance of the mass transfer barriers of the cell walls and the cell interstitium to the diffusion of active ingredients from cells to water is reduced, more active ingredients are promoted to be extracted, and the active ingredients are compounded with the active ingredients extracted from the baikal skullcap root.
Further, in the step (2), the mass volume fraction of the complex enzyme in the water is 1-3%.
Further, the step (3) also comprises superfine grinding of the coarse powder of the baical skullcap root to the fineness of 10-20 mu m.
In order to improve the extraction rate of active ingredients such as baicalin in the baical skullcap root, the baical skullcap root is coarsened to obtain coarse powder of 80-100 meshes, and superfine grinding is carried out until the fineness is 10-20 mu m, so that most of baical skullcap root cells can be broken by superfine grinding, and the active ingredients in the cells are directly exposed to water, so that the dissolution and the effect of the active ingredients are quicker and more complete. However, the applicant found that the superfine powder particle size is not smaller and better, and the superfine grinding of the coarse powder of the baical skullcap root of the invention to the fineness of 10-20 mu m has the best extraction effect. It is hypothesized that after pulverization, the particle size is too small, and more active substances in baicalin are exposed to air and are affected by light or temperature, the worse the stability is, and the extraction effect is further affected.
Further, the auxiliary materials in the step (4) comprise one or more of a filler, a disintegrating agent, a stabilizer and a lubricant.
Further, the ratio of the weight of the auxiliary materials to the total weight of the extract A and the extract B is 0.5-1.5:100.
Further, the filler is one or more of microcrystalline cellulose, lactose, sucrose and bifidobacterium.
Further, the auxiliary materials comprise (0.3-0.5) by weight: (0.7-1.3): 0.1 to 0.5 of filler, disintegrating agent, stabilizing agent and lubricant of 1.
The extracts of simple baical skullcap root, isatis root, kudingchogwort and dandelion are prepared into capsules, and the absorption effect in human bodies is not ideal. By adding the filler, the disintegrating agent, the stabilizer and the lubricant for compounding, as auxiliary materials, the absorption of the cattail blue anti-inflammatory capsule in a human body can be influenced, the drug effect is better, and when the additive is added (0.3-0.5): (0.7-1.3): the stability of the Pudilan anti-inflammatory capsule is higher when the filler, the disintegrating agent, the stabilizing agent and the lubricant of the formula (1) (0.1-0.5).
In order to improve the stability of the cattail blue anti-inflammatory capsule in a high-temperature environment, the stabilizer is further selected from sodium carboxymethyl cellulose or alpha-cyclodextrin.
Still further, the stabilizer is an α -cyclodextrin. The lubricant is magnesium stearate.
The addition of the auxiliary materials improves the efficacy and stability, but the uniformity in batches is still not ideal. In the research and development process, the stabilizer is alpha-cyclodextrin, the lubricant is magnesium stearate, and the uniformity of medicines in batches can be effectively improved. The hypothesis is that the hydrophobic and hydrophilic structure inside the alpha-cyclodextrin molecule affects the crystal structure distribution of magnesium stearate, the magnesium stearate flaky crystal structure is easier to play, the lubrication effect is improved, the mixing of the filler and the disintegrating agent is more uniform, and the batch uniformity of the cattail blue anti-inflammatory capsule is better.
Further, the disintegrating agent is selected from one or more of low-substituted-hydroxypropyl cellulose, croscarmellose sodium and sodium bicarbonate.
Further, the weight ratio of the disintegrating agent to the water is 1:1: (0.3-0.7) low-substituted-hydroxypropyl cellulose, croscarmellose sodium and sodium bicarbonate.
The cattail blue capsule can avoid the influence of moisture, air and light, and can mask the bitter taste of the medicine, but can influence the acting time compared with the tablet. The invention is characterized by adding the components according to the weight ratio of 1:1: (0.3-0.7) low-substituted-hydroxypropyl cellulose, croscarmellose sodium and sodium bicarbonate, and can make catchment blue quickly exert curative effect.
Further, the lubricant is one or more selected from sodium stearyl fumarate, aerosil and magnesium stearate.
The invention also provides the cattail blue anti-inflammatory capsule prepared by the preparation method.
Compared with the prior art, the invention has the advantages that:
1. the preparation method comprises extracting the components (radix Isatidis, herba Violae, herba Taraxaci) in the compound medicinal materials by enzymolysis, filtering the medicinal liquid, and concentrating the extract; the radix scutellariae is extracted by semi-bionic extraction of the active ingredients in the medicinal materials, the medicinal materials are filtered and concentrated into extractum, the two extractum and a proper amount of auxiliary materials are granulated and dried into particles, the particles are filled, no organic solvent is involved, one-step operation can be realized, the use of the organic solvent can be reduced, and the extraction process simulates the human digestive environment, so that the extraction process is closer to the human stomach, and the active ingredients absorbed by the human body can be effectively protected.
2. When the invention is used for extracting the isatis root, the bunge corydalis herb and the dandelion, the three enzymes are compounded for enzymolysis, so that the content of effective active ingredients in the extracting solution is improved.
3. In order to improve the extraction rate of active ingredients in the baikal skullcap root, the baikal skullcap root is coarsened to obtain 80-100 meshes of baikal skullcap root coarse powder, and superfine grinding is carried out until the fineness is 10-20 mu m, so that most of baikal skullcap root cells are broken, and the active ingredients in the cells are directly exposed to water, thereby leading the dissolution and the effect of the active ingredients to be quicker and more complete.
4. The invention is characterized in that (0.3-0.5): (0.7-1.3): the filler, disintegrating agent, stabilizer and lubricant of (0.1-0.5) 1 can be used as auxiliary materials to influence the absorption of the Pu Di lan anti-inflammatory capsule in human body, and the efficacy is better.
Drawings
FIG. 1 is a liquid chromatogram of baicalin in the anti-inflammatory capsule of Pudilan of example 1.
FIG. 2 is a liquid chromatogram of chicoric acid in the anti-inflammatory capsule of Pudilan of example 1.
FIG. 3 is a liquid chromatogram of R, S-epigoitrin in the Pudilan anti-inflammatory capsule of example 1.
FIG. 4 is a liquid chromatogram of the determination of the corydaline in the Pudilan anti-inflammatory capsule of example 1.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The starting materials and test reagents in the examples were purchased from the following manufacturers
Baical skullcap Anhuikang and Chinese medicine science and technology Co., ltd., producing area: mountain and western fortune city
Isatis root Anhui Yude pharmaceutical Co., ltd., production place: gansu (Gansu province)
The kudi Ding Anhui Yude pharmaceutical Co., ltd., production place: hebei river
Dandelion Anhuiyude pharmaceutical Co., ltd., production place: gansu (Gansu province)
Cellulose merck C2605
Pectase merck P2401
Hemicellulase merck H2125
Microcrystalline cellulose merck 1.02331
Alpha-cyclodextrin merck C4642
Low substituted-hydroxypropyl cellulose merck Y0001798
Croscarmellose sodium Shanxi brocade pharmaceutical excipients, CAS:74811-65-7
Baicalin reference substance: CAS of China food and drug verification institute: 21967-41-9
Chicoric acid control: CAS of China food and drug verification institute: 70831-56-0
R, S-primula control: CAS of China food and drug verification institute: 13190-34-6 corydaline control: CAS of China food and drug verification institute: 18797-79-0
Acetonitrile: shanghai Starfish high purity solvent Co., ltd., CAS:75-05-8
Methanol: shanghai Starfish high purity solvent Co., ltd., CAS:67-56-1
Phosphoric acid: tianjin Fuyu fine chemical Co., ltd., CAS:7664-38-2
Hydrochloric acid: guangzhou chemical reagent plant CAS:7647-01-0
Sodium hydroxide: tianjin Fuchen chemical Co., ltd., CAS:1310-73-2
Example 1
The embodiment provides a preparation method of a cattail blue anti-inflammatory capsule, which comprises the following steps:
a method for preparing a cattail blue anti-inflammatory capsule, which comprises the following steps:
(1) Weighing radix Scutellariae, radix Isatidis, herba Violae, and herba Taraxaci according to weight ratio of 1.5:1.5:1:4.
(2) Mixing radix Isatidis, herba Violae and herba Taraxaci, pulverizing to 30-60 mesh, adding 11 times of water, adding compound enzyme composed of cellulase, pectase and hemicellulase, adjusting pH to 3.8, extracting at 40deg.C for 6 hr, filtering to obtain filtrate, and concentrating the filtrate to obtain extract A; wherein, the weight ratio of the cellulase to the pectase to the hemicellulase is 3:1:0.4; the mass volume fraction of the complex enzyme in the water is 2%.
(3) Pulverizing radix Scutellariae to 80-100 meshes to obtain radix Scutellariae coarse powder, superfine pulverizing radix Scutellariae coarse powder to fineness of 10-20 μm, adding 8 times of water, adjusting pH to 6 with HCl, heating to 100deg.C, and extracting for 2 hr; then adjusting pH to 8 with NaOH, extracting at 100deg.C for 2 hr, filtering to obtain filtrate, and concentrating the filtrate to obtain extract B;
(4) Mixing the extract A and the extract B with adjuvants, drying to obtain granule, and encapsulating to obtain a Typhae herba anti-inflammatory capsule; the ratio of the weight of the auxiliary materials to the total weight of the extract A and the extract B is 1:100, and the weight ratio of the auxiliary materials is 0.4:1.1:0.3:1 of filler, a disintegrating agent, a stabilizing agent and a lubricant, wherein the filler is microcrystalline cellulose, the stabilizing agent is alpha-cyclodextrin, and the disintegrating agent is prepared by the following components in percentage by weight: 0.6 of low-substituted-hydroxypropyl cellulose, croscarmellose sodium and sodium bicarbonate, wherein the lubricant is magnesium stearate.
Example 2
The differences between this embodiment and embodiment 1 are: the pH value in the step (2) is adjusted to 3.5, and the extraction is carried out for 6 hours at the temperature of 42 ℃; in the step (3), HCl is used for adjusting the pH value to 5.5, the temperature is raised to 100 ℃, and the heat preservation and extraction are carried out for 2 hours; then the pH value is adjusted to 8.5 by NaOH, and the temperature is kept at 100 ℃ for 2h of extraction.
Example 3
The differences between this embodiment and embodiment 1 are: in the step (2), the weight ratio of the cellulase to the pectase to the hemicellulase is 0.3:1:4.
example 4
The differences between this embodiment and embodiment 1 are: the weight ratio of the complex enzyme to the enzyme is 3:1: cellulase, xylanase and protease of 0.4.
Example 5
The differences between this embodiment and embodiment 1 are: the mass volume fraction of the complex enzyme in the water is 0.3%.
Example 6
The differences between this embodiment and embodiment 1 are: the step (3) does not comprise superfine grinding of the coarse powder of the baical skullcap root until the fineness is 10-20 mu m.
Example 7
The differences between this embodiment and embodiment 1 are: does not comprise auxiliary materials.
Example 8
The differences between this embodiment and embodiment 1 are: the ratio of the weight of the auxiliary materials to the total weight of the extract A and the extract B is 0.2:100.
Example 9
The differences between this embodiment and embodiment 1 are: the auxiliary materials comprise the following components in percentage by weight: 1:1:1 filler, disintegrant, stabilizer and lubricant.
Example 10
The differences between this embodiment and embodiment 1 are: the weight ratio of the disintegrating agent to the water is 1:0.1:2 low substituted-hydroxypropyl cellulose, croscarmellose sodium and sodium bicarbonate.
Example 11
The differences between this embodiment and embodiment 1 are: the weight ratio of the disintegrating agent to the water is 1:1:0.5 portions of chitin, sodium carboxymethyl starch and sodium bicarbonate.
Example 12
The differences between this embodiment and embodiment 1 are: the auxiliary material is starch.
Performance testing
1. The contents of baicalin, chicoric acid, R, S-epigoitrin and corydaline in the Pudilan anti-inflammatory capsules prepared in examples 1 to 12 were measured, the results are shown in Table 2, and the liquid chromatograms of example 1 are shown in FIGS. 1 to 4.
(1) The baicalin determination method comprises the following steps:
reference is made to the high performance liquid chromatography protocol.
Chromatographic conditions and system suitability test: octadecylsilane chemically bonded silica is used as a filler; methanol-0.4% phosphoric acid solution (40:60) is used as a mobile phase, and the detection wavelength is 280nm. The theoretical plate number should be not less than 5000 calculated according to baicalin peak.
Preparation of a control solution: taking appropriate amount of baicalin reference substance, precisely weighing, and adding 80% methanol to obtain solution containing 60 μg per 1 ml.
Preparation of test solution: taking the content of the product under different loading differences, grinding, taking about 0.5g, precisely weighing, placing into a conical flask with a plug, precisely adding 100ml of 80% methanol, sealing, weighing, performing ultrasonic treatment (power 380w, frequency 37 kHz) for 45 minutes, taking out, cooling, weighing again, supplementing the lost weight with 80% methanol, shaking uniformly, filtering, precisely measuring 2ml of the subsequent filtrate, placing into a measuring flask with 10ml, adding 80% methanol for dilution to scale, and shaking uniformly to obtain the product.
Assay: respectively precisely sucking 10 μl of the reference solution and the sample solution, and injecting into high performance liquid chromatograph for measurement.
(2) Chicoric acid determination method:
reference is made to the high performance liquid chromatography protocol.
Chromatographic conditions and system suitability test: octadecylsilane chemically bonded silica is used as a filler; acetonitrile as mobile phase A and 0.2% phosphoric acid solution as mobile phase B, and performing gradient elution according to the following specification in Table 1; the detection wavelength was 326nm. The theoretical plate number should be not less than 5000 calculated as chicoric acid peak.
TABLE 1 mobile phases
Preparation of a control solution: taking appropriate amount of chicoric acid reference substance, precisely weighing, and adding 75% methanol to obtain solution containing 40 μg per 1 ml.
Preparation of test solution: taking the content of the product under different loading amounts, grinding, taking about 1g, precisely weighing, placing into a conical flask with a plug, precisely adding 50ml of 75% methanol, sealing, weighing, performing ultrasonic treatment (power 380w, frequency 37 kHz) for 45 minutes, taking out, cooling, weighing again, supplementing the lost weight with 75% methanol, shaking uniformly, filtering, and taking the subsequent filtrate.
Assay: precisely sucking 5 μl of each of the reference solution and the sample solution, and measuring with high performance liquid chromatograph.
(3) Method for measuring R, S-epigoitrin:
chromatographic conditions and system suitability test: octadecylsilane chemically bonded silica is used as a filler; methanol-water (5:95) is used as a mobile phase; the detection wavelength is 245nm; column temperature was 30 ℃. The theoretical plate number is not less than 6000 as calculated by R, S-epigoitrin.
Preparation of a control solution: precisely weighing R, S-epigoitrin reference substance, adding 80% methanol, and dissolving to obtain solution containing 10 μg per 1ml as reference substance solution.
Preparation of test solution: taking the content of the product under different loading differences, grinding, weighing 2g, precisely weighing, placing into a conical flask with a plug, precisely adding 25ml of 80% methanol, weighing, performing ultrasonic treatment (250 w,40 kHz) for 60min, taking out, cooling, weighing, supplementing the lost weight with 80% methanol, filtering, and collecting the subsequent filtrate.
Assay: precisely sucking 10 μl of each of the control solution and the sample solution, injecting into high performance liquid chromatograph, and recording chromatogram.
(4) Corydaline assay:
chromatographic conditions and system suitability test: octadecylsilane chemically bonded silica is used as a filler; methanol-0.1% phosphoric acid solution (pH value is adjusted to 7.0 by 40% sodium hydroxide solution) (68:32) is used as a mobile phase; the detection wavelength is 289nm; column temperature was 30 ℃. The theoretical plate number is not less than 6000 calculated according to the peak of the corydaline.
Preparation of a control solution: precisely weighing the corydaline reference substance, precisely weighing, and dissolving with methanol to obtain solution containing 10 μg per 1 ml.
Preparation of test solution: taking a test sample of the Pudi anti-inflammatory capsule, pouring out the content, grinding, taking about 1g, precisely weighing, placing into a conical bottle with a plug, precisely adding 20ml of methanol, weighing, performing ultrasonic treatment (250 w,40 kHz) for 30min, taking out, cooling, weighing, supplementing the lost weight with methanol, shaking uniformly, filtering, and taking the subsequent filtrate.
Assay: precisely sucking 10 μl of each of the control solution and the sample solution, injecting into high performance liquid chromatograph, and recording chromatogram.
TABLE 2 content of active ingredients of Pudi Lanyan anti-inflammatory Capsule
2. Stability investigation test
(1) The Pu Di lan anti-inflammatory capsule prepared in example 1 is taken and stored in a sample reserving room, and the results are shown in Table 3, wherein the results are tested in the sample reserving room for 0, 3, 6, 9, 12, 18 and 24 months, and the results show that the products are stable in quality within the effective period (24 months) and all accord with the 2020 edition of Chinese pharmacopoeia standard (moisture is less than 9.0%, baicalin content is not less than 18.5 mg/granule, chicoric acid content is not less than 0.40 mg/granule, the characteristics are brown-yellow to brown-brown granules and powder, the weight difference is +/-7.5%, namely 0.374-0.430 g, and the disintegration time is not more than 30 minutes).
TABLE 3 stability test results
(2) To prove the influence of different auxiliary materials and different auxiliary material proportions on the quality of the product, the invention carries out a comparison test, and the property, the moisture, the disintegration time limit, the content and the weight difference of the product are tested after the product is stored for 24 months, and the results are shown in Table 4.
TABLE 4 detection results after 24 months
The results show that when the types and proportions of the auxiliary materials selected in example 1 are used, the product stability is good, and when the types and proportions of the auxiliary materials are changed or even the auxiliary materials are not used, the contents of the product are easy to stick, and the product stability is poor.
While the foregoing is directed to the preferred embodiments of the present invention, it will be appreciated by those skilled in the art that various modifications and adaptations can be made without departing from the principles of the present invention, and such modifications and adaptations are intended to be comprehended within the scope of the present invention.

Claims (5)

1. A preparation method of a cattail blue anti-inflammatory capsule is characterized by comprising the following steps: the preparation method comprises the following steps:
(1) 1 to 3, 1 to 6 parts of baical skullcap root, indigowoad root, kudingchohl herb and dandelion are weighed according to the weight ratio of 1 to 3;
(2) Mixing radix isatidis, herba violae and dandelion, crushing to 30-60 meshes, adding 8-12 times of water, adding compound enzyme consisting of cellulase, pectase and hemicellulase, adjusting the pH to 3.5-4, extracting at 35-42 ℃ for 4-8 hours, filtering to obtain filtrate, and concentrating the filtrate to obtain extract A;
(3) Pulverizing radix scutellariae to 80-100 meshes to obtain coarse radix scutellariae powder, performing superfine grinding to fineness of 10-20 mu m, adding 6-10 times of water, adjusting the pH value to 5.5-6.5 by using HCl, heating to 100 ℃, and extracting for 1.5-3 h under heat preservation; then adjusting the pH value to 7-9 by NaOH, extracting at 100 ℃ for 1.5-3 hours, filtering to obtain filtrate, and concentrating the filtrate to obtain extract B;
(4) Mixing the extract A and the extract B with appropriate amount of auxiliary materials, drying to obtain granules, and filling the granules into capsules of 0.4 g/granule to obtain the Typhonium giganteum anti-inflammatory capsule;
in the step (2), the weight ratio of the cellulase to the pectase to the hemicellulase is (1-5) 1: (0.2 to 0.6);
the mass volume fraction of the complex enzyme in the step (2) accounting for water is 1-3%;
the auxiliary materials in the step (4) are in weight ratio of (0.3-0.5): (0.7-1.3): (0.1-0.5) filler, disintegrating agent, stabilizing agent and lubricant of 1;
the ratio of the weight of the auxiliary materials to the total weight of the extract A and the extract B is 0.5-1.5:100;
wherein the weight ratio of the disintegrating agent to the water is 1:1: (0.3-0.7) low-substituted-hydroxypropyl cellulose, croscarmellose sodium and sodium bicarbonate.
2. The method for preparing the cattail blue anti-inflammatory capsule according to claim 1, which is characterized in that: in the step (1), the weight ratio of the baical skullcap root, the isatis root, the kudingchoffm herb and the dandelion is 1.5:1.5:1:4.
3. The method for preparing the cattail blue anti-inflammatory capsule according to claim 1, which is characterized in that: the filler is one or more of microcrystalline cellulose, lactose, sucrose and bifidobacterium; the stabilizer is selected from sodium carboxymethyl cellulose or alpha-cyclodextrin.
4. The method for preparing the cattail blue anti-inflammatory capsule according to claim 3, wherein the method comprises the following steps: the lubricant is one or more selected from sodium stearyl fumarate, silica gel micropowder and magnesium stearate.
5. The cattail blue anti-inflammatory capsule prepared by the preparation method of any one of claims 1-4.
CN202311176697.3A 2023-09-13 2023-09-13 Pudi blue anti-inflammatory capsule and preparation method thereof Active CN117064939B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202311176697.3A CN117064939B (en) 2023-09-13 2023-09-13 Pudi blue anti-inflammatory capsule and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202311176697.3A CN117064939B (en) 2023-09-13 2023-09-13 Pudi blue anti-inflammatory capsule and preparation method thereof

Publications (2)

Publication Number Publication Date
CN117064939A CN117064939A (en) 2023-11-17
CN117064939B true CN117064939B (en) 2024-03-08

Family

ID=88715312

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202311176697.3A Active CN117064939B (en) 2023-09-13 2023-09-13 Pudi blue anti-inflammatory capsule and preparation method thereof

Country Status (1)

Country Link
CN (1) CN117064939B (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116763838B (en) * 2023-07-21 2024-02-13 广东心宝药业科技有限公司 Pudi blue anti-inflammatory tablet and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104940303A (en) * 2015-06-26 2015-09-30 江苏颐海药业有限责任公司 Method for preparing pudilan anti-inflammation capsules
CN109718278A (en) * 2017-10-27 2019-05-07 江苏颐海药业有限责任公司 A method of Pudilan antiphlogistic capsule is prepared using microwave crushing

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104940303A (en) * 2015-06-26 2015-09-30 江苏颐海药业有限责任公司 Method for preparing pudilan anti-inflammation capsules
CN109718278A (en) * 2017-10-27 2019-05-07 江苏颐海药业有限责任公司 A method of Pudilan antiphlogistic capsule is prepared using microwave crushing

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
复合酶提高黄柏水提效率的关键技术研究;文洪宇;中国中医急症;22(06);898-899,904 *
蒲地蓝胶囊的制备工艺研究;徐宁宁;山东化工;20191223(24);38-39, 42 *
黄芩三种方法提取液的血清图谱比较;王志江;世界中西医结合杂志;10(09);1230-1232,1325 *
黄芩半仿生提取法工艺条件的优选;姜仁禹;世界中西医结合杂志;06(03);230-233 *

Also Published As

Publication number Publication date
CN117064939A (en) 2023-11-17

Similar Documents

Publication Publication Date Title
CN117064939B (en) Pudi blue anti-inflammatory capsule and preparation method thereof
CN106389453B (en) Flavone glycoside composition
CN111358839B (en) Formula granules of polygonum capitatum and preparation method thereof
CN102133266A (en) Preparation method for macroporous resin purifying extract of golden hemorrhoid fumigating-washing powder
CN101711805A (en) Medicine composition for treating rheumatoid arthritis and preparation thereof
JP2016539955A (en) Drug composition, method for producing the same, and use
WO2015081703A1 (en) Solid dispersion containing desmodium styracifolium (osb.) merr. flavonoids, method of preparing same, and use thereof
CN103623059B (en) A kind of pharmaceutical composition and application thereof, containing its medicament
CA3113240A1 (en) Transmucosal psychoactive alkaloid composition and preparation thereof
WO2012027968A1 (en) Panaxatriol saponins enteric pellet, capsule comprising same and method for preparing same
CN104382964A (en) Method for preparing peganum harmala linn total alkaloid extract and peganum harmala linn total flavone extract from peganum harmala linn
CN1679780A (en) Chinese medicine preparation for treating gynecopathy, preparation and quality control thereof
CN113171412A (en) Callicarpa nudiflora traditional Chinese medicine composition and preparation method thereof
CN111110642A (en) Anoectochilus roxburghii polysaccharide dispersible tablet and preparation method thereof
CN100534476C (en) Traditional Chinese medicine composition made by isatis root and rhizoma belamcandae, and its preparation method and use
CN112569281B (en) Yiqing composition and preparation method thereof
CN115463175B (en) Universal capsule for clearing heat and detoxicating and its preparing process
CN116036159B (en) A method for preparing Chinese medicinal composition extract containing Ganoderma spore oil and semen Ziziphi Spinosae oil
CN107898942B (en) Cold clearing capsule and preparation method thereof
CN115554248B (en) Enteric-coated traditional Chinese medicine preparation for treating infant cytomegalovirus infectious hepatitis and preparation method thereof
CN110548042A (en) Achyranthes bidentata polysaccharide capsule preparation, preparation method and application
WO2023045005A1 (en) Method for preparing total glucosides of paeonia
CN108969567B (en) Preparation method of traditional Chinese medicine composition containing rock fat
CN101496818A (en) Kidney-nourishing and bone-tonifying chewable tablet and preparation method thereof
CN112569314A (en) Menstruation regulating and face nourishing medicinal preparation 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