CN112168919A - Preparation process of traditional Chinese medicine composition - Google Patents
Preparation process of traditional Chinese medicine composition Download PDFInfo
- Publication number
- CN112168919A CN112168919A CN202011179066.3A CN202011179066A CN112168919A CN 112168919 A CN112168919 A CN 112168919A CN 202011179066 A CN202011179066 A CN 202011179066A CN 112168919 A CN112168919 A CN 112168919A
- Authority
- CN
- China
- Prior art keywords
- root
- radix
- parts
- adjust
- chinese medicine
- 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.)
- Pending
Links
Classifications
-
- 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)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/80—Scrophulariaceae (Figwort family)
- A61K36/804—Rehmannia
-
- 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)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/53—Lamiaceae or Labiatae (Mint family), e.g. thyme, rosemary or lavender
- A61K36/539—Scutellaria (skullcap)
-
- 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)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/63—Oleaceae (Olive family), e.g. jasmine, lilac or ash tree
- A61K36/634—Forsythia
-
- 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)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/80—Scrophulariaceae (Figwort family)
- A61K36/808—Scrophularia (figwort)
-
- 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)
- A61K36/896—Liliaceae (Lily family), e.g. daylily, plantain lily, Hyacinth or narcissus
- A61K36/8968—Ophiopogon (Lilyturf)
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
- A61K47/42—Proteins; Polypeptides; Degradation products thereof; Derivatives thereof, e.g. albumin, gelatin or zein
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/46—Ingredients of undetermined constitution or reaction products thereof, e.g. skin, bone, milk, cotton fibre, eggshell, oxgall or plant extracts
-
- 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
- A61K9/0087—Galenical forms not covered by A61K9/02 - A61K9/7023
- A61K9/0095—Drinks; Beverages; Syrups; Compositions for reconstitution thereof, e.g. powders or tablets to be dispersed in a glass of water; Veterinary drenches
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P11/00—Drugs for disorders of the respiratory system
- A61P11/04—Drugs for disorders of the respiratory system for throat disorders
-
- 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
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
Landscapes
- Health & Medical Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Pharmacology & Pharmacy (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- General Health & Medical Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Medicinal Chemistry (AREA)
- Epidemiology (AREA)
- Botany (AREA)
- Engineering & Computer Science (AREA)
- Mycology (AREA)
- Microbiology (AREA)
- Medical Informatics (AREA)
- Biotechnology (AREA)
- Alternative & Traditional Medicine (AREA)
- Pulmonology (AREA)
- Neurosurgery (AREA)
- Inorganic Chemistry (AREA)
- Otolaryngology (AREA)
- Proteomics, Peptides & Aminoacids (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Organic Chemistry (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention aims to provide a preparation method of a traditional Chinese medicine composition. In order to overcome the defects of the production process of the original laryngopharynx cleaning mixture, the inventor discovers through a large amount of experimental researches that the impregnation time can be greatly shortened by respectively adjusting the pH value to impregnate different components, and in addition, the pH value is strictly controlled after egg white is added, so that the clarity is improved, and the stability of a medicinal preparation is improved at the same time, and a common preservative sodium benzoate is not added in the preparation.
Description
Technical Field
The invention belongs to the technical field of medicines, and particularly relates to a preparation process of a traditional Chinese medicine composition.
Background
The mixture for clearing throat heat is a traditional Chinese medicine compound preparation prepared from five medicinal materials of rehmannia root, dwarf lilyturf tuber, figwort root, weeping forsythia and baical skullcap root, and is currently recorded in 2015 edition Chinese pharmacopoeia. The main functional indications are as follows: nourish yin to clear away the lung-heat, relieve sore throat and remove toxicity. Can be used for treating swelling and pain of throat, dry throat, white rot of throat, tunica albuginea, and swelling of throat due to yin deficiency, dryness-heat, and fire toxin; localized diphtheria, mild toxic diphtheria, acute tonsillitis, angina with the above symptoms.
The patent CN1366892A provides a method for preparing a nano throat-clearing preparation, which is a new medicinal preparation prepared from the nano raw materials of five medicinal materials in the original formula of the throat-clearing mixture according to a proportion, wherein the particle size of most of the medicinal materials is less than 100nm, and the medicinal preparation has new physical properties. It is prepared through microwave extraction, decompression concentration, spray drying in supersonic jet and other steps.
Patent CN104083618A provides a preparation method of a soft capsule for clearing throat, which comprises the following procedures: preparing extract dry powder: extracting the medicinal materials by soaking percolation method with ethanol solution, concentrating under reduced pressure, decocting the concentrated solution with water, concentrating the filtrate, drying under reduced pressure, and pulverizing to obtain dry extract powder; preparing a substrate; preparing contents; preparing glue solution; finally, the soft capsule is prepared by pressing. The throat clearing soft capsule prepared by the method can seal the bad smell and the bad taste of the medicine and improve the compliance of patients.
Patent CN109288960A discloses a preparation method of a mixture for clearing throat, which uses ethyl acetate as a solvent, and a group of traditional Chinese medicine compositions with the efficacy of clearing throat are extracted by heating reflux, separated and purified by a high-speed centrifugation method, dried, granulated by a dry method, and prepared into a solid preparation by a conventional process. The method shortens production cycle, improves extraction rate of effective components, and reduces dissolution of ineffective components, so as to obtain more accurate therapeutic effect and safer administration.
The existing production method of the throat clearing preparation extracts all components together, does not consider the difference of characteristics among different components, and has different leaching effects of effective components in different components under the influence of pH, thereby prolonging the leaching time of the effective components. In addition, the clarity and stability of the traditional Chinese medicine composition are always the problems that researchers are trying to improve, egg white is used as a clarifying agent in a traditional Chinese medicine preparation, but is not applied to a throat clearing mixture, and the applicant finds that the clarity of the medicine can be immediately improved by using the egg white alone, but precipitates are generated along with the prolonging of time.
The invention content is as follows:
the invention aims to provide a preparation method of a traditional Chinese medicine composition. In order to overcome the defects of the production process of the original laryngopharynx cleaning mixture, the inventor discovers through a large amount of experimental researches that the impregnation time can be greatly shortened by respectively adjusting the pH value to impregnate different components, and in addition, the pH value is strictly controlled after egg white is added, so that the clarity is improved, and the stability of a medicinal preparation is improved at the same time, and a common preservative sodium benzoate is not added in the preparation.
In order to realize the purpose of the invention, the invention adopts the following technical scheme:
(1) pulverizing Chinese medicinal composition into coarse powder, wherein the Chinese medicinal composition comprises rehmanniae radix, radix Ophiopogonis, radix scrophulariae, fructus forsythiae and Scutellariae radix, the rehmanniae radix, radix Ophiopogonis, radix scrophulariae and fructus forsythiae use 57% ethanol as solvent, sodium bicarbonate solution is added to adjust pH, the Scutellariae radix uses 57% ethanol as solvent, sodium hydroxide solution is added to adjust pH, the materials are respectively soaked for 6 hours, the mixture is mixed, slowly percolated at the speed of about 1mL per minute, and percolate is collected;
(2) concentrating percolate under reduced pressure, adding purified water, boiling for 30min, standing for 48 hr, filtering, washing the residue with a small amount of purified water, mixing filtrates, concentrating under reduced pressure to obtain concentrated solution, adding egg white, adding sodium hydroxide solution to adjust pH, heating to 80-95 deg.C for 30-60min, cooling to room temperature, adding benzoic acid to adjust pH, stirring, refrigerating for 24-48 hr, collecting supernatant, filtering, centrifuging, adding water, and stirring.
Wherein:
the weight ratio of the traditional Chinese medicine composition in the step (1) is as follows: 5-10 parts of rehmannia, 5-10 parts of radix ophiopogonis, 10-20 parts of radix scrophulariae, 15-30 parts of fructus forsythiae and 15-30 parts of radix scutellariae; preferably, 8 parts by weight of rehmannia root, 10 parts by weight of dwarf lilyturf tuber, 1520 parts by weight of figwort root, 20 parts by weight of weeping forsythia capsule and 20 parts by weight of radix scutellariae;
in the step (1), adjusting the pH value of ethanol solution of rehmannia root, dwarf lilyturf tuber, figwort root and weeping forsythia to 6.5-7.0, and adjusting the pH value of ethanol solution of radix scutellariae to 7.0-7.5;
the mass volume ratio of the egg white added in the step (2) to the concentrated solution is 0.1-1: 100, respectively;
adding sodium hydroxide solution to regulate the pH value to 7.5-8.5 in the step (2);
adding benzoic acid to adjust the pH value to 5.5-6.0 in the step (2);
compared with the prior art, the invention has the following beneficial technical effects:
(1) different components are soaked in different pH environments, so that the leaching time of effective components is greatly shortened;
(2) egg white is added and the pH is adjusted, so that the clarity and stability of the liquid medicine are improved;
(3) benzoic acid is used to replace prior art hydrochloric acid to adjust the pH without the need for additional preservatives.
The specific implementation mode is as follows:
the following embodiments are further described to help further understand the advantages and effects of the technical solutions of the present invention, and the embodiments do not limit the scope of the present invention, which is determined by the claims.
Example 1
Prescription: 50g of rehmannia root, 50g of dwarf lilyturf tuber, 100g of figwort root, 150g of weeping forsythia capsule and 150g of radix scutellariae
The process comprises the following steps:
(1) taking rehmannia root, dwarf lilyturf tuber, figwort root, weeping forsythia and radix scutellariae according to the prescription amount, respectively crushing the rehmannia root, the dwarf lilyturf tuber, the figwort root and the weeping forsythia into coarse powder, wherein 3000mL of 57 percent ethanol is used as a solvent, 5 percent sodium bicarbonate solution is added to adjust the pH value to 6.5, 1000mL of 57 percent ethanol is used as a solvent for the radix scutellariae, 10 percent sodium hydroxide solution is added to adjust the pH value to 7.0, respectively soaking for 6 hours, mixing, slowly percolating at the speed of about 1mL per minute, and collecting percolate;
(2) concentrating percolate under reduced pressure to 600mL, adding purified water 400mL, boiling for 30min, standing for 24 h, filtering, washing filter residue with a small amount of purified water, mixing filtrates, concentrating under reduced pressure to 500mL, adding egg white 0.5g, adding 10% sodium hydroxide solution to adjust pH to 7.5, heating to 80-95 deg.C for 30min, standing to room temperature, adding benzoic acid to adjust pH to 5.5, stirring, refrigerating for 24 h, collecting supernatant, filtering, centrifuging, adding water to 500mL, and stirring to obtain the final product.
Example 2
Prescription: 100g of rehmannia root, 100g of dwarf lilyturf tuber, 200g of figwort root, 300g of weeping forsythia capsule and 300g of radix scutellariae
The process comprises the following steps:
(1) taking rehmannia root, dwarf lilyturf tuber, figwort root, weeping forsythia and radix scutellariae according to the prescription amount, respectively crushing the rehmannia root, the dwarf lilyturf tuber, the figwort root and the weeping forsythia into coarse powder, wherein 6000mL of 57 percent ethanol is used as a solvent for the rehmannia root, the dwarf lilyturf tuber, the figwort root and the weeping forsythia, 5 percent sodium bicarbonate solution is added for adjusting the pH value to 7.0, 2000mL of 57 percent ethanol is used as a solvent for the radix scutellariae, 10 percent sodium hydroxide solution is added for adjusting the pH value to 7.5, respectively soaking for 6 hours, mixing;
(2) concentrating percolate under reduced pressure to 1200mL, adding purified water to 800mL, boiling for 30min, standing for 24 h, filtering, washing filter residue with a small amount of purified water, mixing filtrates, concentrating under reduced pressure to 1000mL, adding egg white 10g, adding 10% sodium hydroxide solution to adjust pH to 8.5, heating to 80-95 deg.C for 30min, standing to room temperature, adding benzoic acid to adjust pH to 5.7, stirring, refrigerating for 24 h, collecting supernatant, filtering, centrifuging, adding water to 1000mL, and stirring to obtain the final product.
Example 3
Prescription: 80g of rehmannia root, 100g of dwarf lilyturf tuber, 150g of figwort root, 200g of weeping forsythia capsule and 200g of radix scutellariae
The process comprises the following steps:
(1) taking rehmannia root, dwarf lilyturf tuber, figwort root, weeping forsythia and radix scutellariae according to the prescription amount, respectively crushing the rehmannia root, the dwarf lilyturf tuber, the figwort root and the weeping forsythia into coarse powder, wherein 4500mL of 57 percent ethanol is used as a solvent, 5 percent sodium bicarbonate solution is added to adjust the pH value to 6.8, 1500mL of 57 percent ethanol is used as a solvent for the radix scutellariae, 10 percent sodium hydroxide solution is added to adjust the pH value to 7.2, respectively soaking for 6 hours, mixing, slowly percolating at the speed of about 1mL per minute, and collecting percolate;
(2) concentrating percolate under reduced pressure to 900mL, adding 600mL of purified water, boiling for 30min, standing for 24 h, filtering, washing filter residue with a small amount of purified water, mixing filtrates, concentrating under reduced pressure to 750mL, adding 3.75g of egg white, adding 10% sodium hydroxide solution to adjust pH to 8.0, heating to 80-95 deg.C for 30min, standing to room temperature, adding benzoic acid to adjust pH to 6.0, stirring, refrigerating for 24 h, collecting supernatant, filtering, centrifuging, adding 750mL of water, and stirring to obtain the final product.
Comparative example 1 components without pH adjustment
Prescription: 100g of rehmannia root, 100g of dwarf lilyturf tuber, 200g of figwort root, 300g of weeping forsythia capsule and 300g of radix scutellariae
The process comprises the following steps:
(1) respectively pulverizing rehmanniae radix, radix Ophiopogonis, radix scrophulariae, fructus forsythiae and Scutellariae radix into coarse powder, soaking in 8000mL of 57% ethanol as solvent for 6 hr, mixing, slowly percolating at a speed of about 1mL per minute, and collecting percolate;
(2) concentrating percolate under reduced pressure to 1200mL, adding purified water to 800mL, boiling for 30min, standing for 24 h, filtering, washing filter residue with a small amount of purified water, mixing filtrates, concentrating under reduced pressure to 1000mL, adding egg white 10g, adding 10% sodium hydroxide solution to adjust pH to 8.5, heating to 80-95 deg.C for 30min, standing to room temperature, adding benzoic acid to adjust pH to 5.5, stirring, refrigerating for 24 h, collecting supernatant, filtering, centrifuging, adding water to 100mL, and stirring to obtain the final product.
Comparative example 2 without pH adjustment, the immersion was carried out for 24 hours
Prescription: 100g of rehmannia root, 100g of dwarf lilyturf tuber, 200g of figwort root, 300g of weeping forsythia capsule and 300g of radix scutellariae
The process comprises the following steps:
(1) respectively pulverizing rehmanniae radix, radix Ophiopogonis, radix scrophulariae, fructus forsythiae and Scutellariae radix into coarse powder, soaking in 8000mL of 57% ethanol as solvent for 24 hr, mixing, slowly percolating at a speed of about 1mL per minute, and collecting percolate;
(2) concentrating percolate under reduced pressure to 1200mL, adding purified water to 800mL, boiling for 30min, standing for 24 h, filtering, washing filter residue with a small amount of purified water, mixing filtrates, concentrating under reduced pressure to 1000mL, adding egg white 10g, adding 10% sodium hydroxide solution to adjust pH to 8.5, heating to 80-95 deg.C for 30min, standing to room temperature, adding benzoic acid to adjust pH to 5.5, stirring, refrigerating for 24 h, collecting supernatant, filtering, centrifuging, adding water to 100mL, and stirring to obtain the final product.
Comparative example 3 No egg white addition
Prescription: 100g of rehmannia root, 100g of dwarf lilyturf tuber, 200g of figwort root, 300g of weeping forsythia capsule and 300g of radix scutellariae
The process comprises the following steps:
(1) taking rehmannia root, dwarf lilyturf tuber, figwort root, weeping forsythia and radix scutellariae according to the prescription amount, respectively crushing the rehmannia root, the dwarf lilyturf tuber, the figwort root and the weeping forsythia into coarse powder, wherein 6000mL of 57 percent ethanol is used as a solvent for the rehmannia root, the dwarf lilyturf tuber, the figwort root and the weeping forsythia, 5 percent sodium bicarbonate solution is added for adjusting the pH value to 7.0, 2000mL of 57 percent ethanol is used as a solvent for the radix scutellariae, 10 percent sodium hydroxide solution is added for adjusting the pH value to 7.5, respectively soaking for 6 hours, mixing;
(2) concentrating percolate under reduced pressure to 1200mL, adding purified water to 800mL, boiling for 30min, standing for 24 h, filtering, washing filter residue with a small amount of purified water, mixing filtrates, concentrating under reduced pressure to 1000mL, adding 10% sodium hydroxide solution to adjust pH to 8.5, heating to 80-95 deg.C, heating for 30min, cooling to room temperature, adding benzoic acid to adjust pH to 5.5, stirring, refrigerating for 24 h, collecting supernatant, filtering, centrifuging, adding water to 1000mL, and stirring to obtain the final product.
Comparative example 4 No pH adjustment after egg white addition
Prescription: 100g of rehmannia root, 100g of dwarf lilyturf tuber, 200g of figwort root, 300g of weeping forsythia capsule and 300g of radix scutellariae
The process comprises the following steps:
(1) taking rehmannia root, dwarf lilyturf tuber, figwort root, weeping forsythia and radix scutellariae according to the prescription amount, respectively crushing the rehmannia root, the dwarf lilyturf tuber, the figwort root and the weeping forsythia into coarse powder, wherein 6000mL of 57 percent ethanol is used as a solvent for the rehmannia root, the dwarf lilyturf tuber, the figwort root and the weeping forsythia, 5 percent sodium bicarbonate solution is added for adjusting the pH value to 7.0, 2000mL of 57 percent ethanol is used as a solvent for the radix scutellariae, 10 percent sodium hydroxide solution is added for adjusting the pH value to 7.5, respectively soaking for 6 hours, mixing;
(2) concentrating percolate under reduced pressure to 1200mL, adding purified water to 800mL, boiling for 30min, standing for 24 h, filtering, washing filter residue with a small amount of purified water, mixing filtrates, concentrating under reduced pressure to 1000mL, adding 10g of egg white, heating to 80-95 deg.C for 30min, standing to room temperature, adding benzoic acid to adjust pH to 5.5, stirring, refrigerating for 24 h, collecting supernatant, filtering, centrifuging, adding water to 1000mL, and stirring to obtain the final product.
Comparative example 5 egg white addition followed by pH reduction
Prescription: 100g of rehmannia root, 100g of dwarf lilyturf tuber, 200g of figwort root, 300g of weeping forsythia capsule and 300g of radix scutellariae
The process comprises the following steps:
(1) taking rehmannia root, dwarf lilyturf tuber, figwort root, weeping forsythia and radix scutellariae according to the prescription amount, respectively crushing the rehmannia root, the dwarf lilyturf tuber, the figwort root and the weeping forsythia into coarse powder, wherein 6000mL of 57 percent ethanol is used as a solvent for the rehmannia root, the dwarf lilyturf tuber, the figwort root and the weeping forsythia, 5 percent sodium bicarbonate solution is added for adjusting the pH value to 7.0, 2000mL of 57 percent ethanol is used as a solvent for the radix scutellariae, 10 percent sodium hydroxide solution is added for adjusting the pH value to 7.5, respectively soaking for 6 hours, mixing;
(2) concentrating percolate under reduced pressure to 1200mL, adding purified water to 800mL, boiling for 30min, standing for 24 h, filtering, washing filter residue with a small amount of purified water, mixing filtrates, concentrating under reduced pressure to 1000mL, adding egg white 10g, adding 10% sodium hydroxide solution to adjust pH to 7.0, heating to 80-95 deg.C, heating for 30min, standing to room temperature, adding benzoic acid to adjust pH to 5.5, stirring, refrigerating for 24 h, collecting supernatant, filtering, centrifuging, adding water to 1000mL, and stirring to obtain the final product.
Comparative example 6 egg white addition followed by pH increase
Prescription: 100g of rehmannia root, 100g of dwarf lilyturf tuber, 200g of figwort root, 300g of weeping forsythia capsule and 300g of radix scutellariae
The process comprises the following steps:
(1) taking rehmannia root, dwarf lilyturf tuber, figwort root, weeping forsythia and radix scutellariae according to the prescription amount, respectively crushing the rehmannia root, the dwarf lilyturf tuber, the figwort root and the weeping forsythia into coarse powder, wherein 6000mL of 57 percent ethanol is used as a solvent for the rehmannia root, the dwarf lilyturf tuber, the figwort root and the weeping forsythia, 5 percent sodium bicarbonate solution is added for adjusting the pH value to 7.0, 2000mL of 57 percent ethanol is used as a solvent for the radix scutellariae, 10 percent sodium hydroxide solution is added for adjusting the pH value to 7.5, respectively soaking for 6 hours, mixing;
(2) concentrating percolate under reduced pressure to 1200mL, adding purified water to 800mL, boiling for 30min, standing for 24 h, filtering, washing filter residue with a small amount of purified water, mixing filtrates, concentrating under reduced pressure to 1000mL, adding egg white 10g, adding 10% sodium hydroxide solution to adjust pH to 9.0, heating to 80-95 deg.C for 30min, standing to room temperature, adding benzoic acid to adjust pH to 5.5, stirring, refrigerating for 24 h, collecting supernatant, filtering, centrifuging, adding water to 1000mL, and stirring to obtain the final product.
Comparative example 7 hydrochloric acid instead of benzoic acid
Prescription: 100g of rehmannia root, 100g of dwarf lilyturf tuber, 200g of figwort root, 300g of weeping forsythia capsule and 300g of radix scutellariae
The process comprises the following steps:
(1) taking rehmannia root, dwarf lilyturf tuber, figwort root, weeping forsythia and radix scutellariae according to the prescription amount, respectively crushing the rehmannia root, the dwarf lilyturf tuber, the figwort root and the weeping forsythia into coarse powder, wherein 6000mL of 57 percent ethanol is used as a solvent for the rehmannia root, the dwarf lilyturf tuber, the figwort root and the weeping forsythia, 5 percent sodium bicarbonate solution is added for adjusting the pH value to 7.0, 2000mL of 57 percent ethanol is used as a solvent for the radix scutellariae, 10 percent sodium hydroxide solution is added for adjusting the pH value to 7.5, respectively soaking for 6 hours, mixing;
(2) concentrating percolate under reduced pressure to 1200mL, adding purified water 800mL, boiling for 30min, standing for 24 h, filtering, washing filter residue with a small amount of purified water, mixing filtrates, concentrating under reduced pressure to 1000mL, adding egg white 10g, adding 10% sodium hydroxide solution to adjust pH to 8.5, heating to 80-95 deg.C for 30min, cooling to room temperature, adding concentrated hydrochloric acid to adjust pH to 5.5, stirring, refrigerating for 24 h, collecting supernatant, filtering, centrifuging, adding water to 1000mL, and stirring to obtain the final product.
Comparative example 8 concentrated hydrochloric acid + sodium benzoate
Prescription: 100g of rehmannia root, 100g of dwarf lilyturf tuber, 200g of figwort root, 300g of weeping forsythia capsule and 300g of radix scutellariae
The process comprises the following steps:
(1) taking rehmannia root, dwarf lilyturf tuber, figwort root, weeping forsythia and radix scutellariae according to the prescription amount, respectively crushing the rehmannia root, the dwarf lilyturf tuber, the figwort root and the weeping forsythia into coarse powder, wherein 6000mL of 57 percent ethanol is used as a solvent for the rehmannia root, the dwarf lilyturf tuber, the figwort root and the weeping forsythia, 5 percent sodium bicarbonate solution is added for adjusting the pH value to 7.0, 2000mL of 57 percent ethanol is used as a solvent for the radix scutellariae, 10 percent sodium hydroxide solution is added for adjusting the pH value to 7.5, respectively soaking for 6 hours, mixing;
(2) concentrating percolate under reduced pressure to 1200mL, adding purified water 800mL, boiling for 30min, standing for 24 h, filtering, washing filter residue with a small amount of purified water, mixing filtrates, concentrating under reduced pressure to 1000mL, adding egg white 10g, adding 10% sodium hydroxide solution to adjust pH to 8.5, heating to 80-95 deg.C for 30min, cooling to room temperature, adding concentrated hydrochloric acid to adjust pH to 5.5, adding sodium benzoate 3g, stirring, refrigerating for 24 h, collecting supernatant, filtering, centrifuging, adding water to 1000mL, and stirring to obtain the final product.
Comparative example 9 benzoic acid let down pH
Prescription: 100g of rehmannia root, 100g of dwarf lilyturf tuber, 200g of figwort root, 300g of weeping forsythia capsule and 300g of radix scutellariae
The process comprises the following steps:
(1) taking rehmannia root, dwarf lilyturf tuber, figwort root, weeping forsythia and radix scutellariae according to the prescription amount, respectively crushing the rehmannia root, the dwarf lilyturf tuber, the figwort root and the weeping forsythia into coarse powder, wherein 6000mL of 57 percent ethanol is used as a solvent for the rehmannia root, the dwarf lilyturf tuber, the figwort root and the weeping forsythia, 5 percent sodium bicarbonate solution is added for adjusting the pH value to 7.0, 2000mL of 57 percent ethanol is used as a solvent for the radix scutellariae, 10 percent sodium hydroxide solution is added for adjusting the pH value to 7.5, respectively soaking for 6 hours, mixing;
(2) concentrating percolate under reduced pressure to 1200mL, adding purified water to 800mL, boiling for 30min, standing for 24 h, filtering, washing filter residue with a small amount of purified water, mixing filtrates, concentrating under reduced pressure to 1000mL, adding egg white 10g, adding 10% sodium hydroxide solution to adjust pH to 8.5, heating to 80-95 deg.C for 30min, standing to room temperature, adding benzoic acid to adjust pH to 4.5, stirring, refrigerating for 24 h, filtering supernatant, centrifuging, adding water to 1000mL, and stirring to obtain the final product.
Comparative example 10 benzoic acid adjusted to an increased pH
Prescription: 100g of rehmannia root, 100g of dwarf lilyturf tuber, 200g of figwort root, 300g of weeping forsythia capsule and 300g of radix scutellariae
The process comprises the following steps:
(1) taking rehmannia root, dwarf lilyturf tuber, figwort root, weeping forsythia and radix scutellariae according to the prescription amount, respectively crushing the rehmannia root, the dwarf lilyturf tuber, the figwort root and the weeping forsythia into coarse powder, wherein 6000mL of 57 percent ethanol is used as a solvent for the rehmannia root, the dwarf lilyturf tuber, the figwort root and the weeping forsythia, 5 percent sodium bicarbonate solution is added for adjusting the pH value to 7.0, 2000mL of 57 percent ethanol is used as a solvent for the radix scutellariae, 10 percent sodium hydroxide solution is added for adjusting the pH value to 7.5, respectively soaking for 6 hours, mixing;
(2) concentrating percolate under reduced pressure to 1200mL, adding purified water to 800mL, boiling for 30min, standing for 24 h, filtering, washing filter residue with a small amount of purified water, mixing filtrates, concentrating under reduced pressure to 1000mL, adding egg white 10g, adding 10% sodium hydroxide solution to adjust pH to 8.5, heating to 80-95 deg.C for 30min, standing to room temperature, adding benzoic acid to adjust pH to 6.5, stirring, refrigerating for 24 h, filtering supernatant, centrifuging, adding water to 1000mL, and stirring to obtain the final product.
Experimental example 1
And (3) identifying radix scutellariae and fructus forsythiae: the procedure was carried out in accordance with pharmacopoeia department one, examples 1 to 3 and comparative examples 1 to 8 being in compliance with the regulations.
Experimental example 2
The qinghouyan mixture prepared in the above examples 1-3 and comparative examples 1-8 was taken for baicalin content determination.
Wherein, the content of baicalin is determined by high performance liquid chromatography, and the content is as follows:
liquid phase conditions: the stationary phase takes octadecylsilane chemically bonded silica as a filler; acetonitrile-0.2% phosphoric acid solution (28:72) is used as a mobile phase; the detection wavelength is 278nm, and the number of theoretical plates is not less than 5000 calculated according to baicalin.
Preparation of a reference solution: precisely weighing appropriate amount of baicalin, precisely weighing, and adding methanol to obtain solution containing 0.2 mg/lmL.
Preparing a test solution: precisely measuring 1mL of the product in a 50mL measuring flask, adding methanol to scale, performing ultrasonic treatment for 20min, taking out, cooling to room temperature, adding methanol to complement weight loss, shaking, filtering with 0.2 μm microporous membrane, and collecting the filtrate.
And (3) determination: precisely sucking 10 μ L of each of the reference solution and the sample solution, injecting into high performance liquid chromatograph, and measuring to obtain the results shown in Table 1.
Experimental example 3
And (4) checking properties: the results of visual inspection are shown in Table 1.
TABLE 1
| Sample (I) | Baicalin content mg/mL | Traits |
| Example 1 | 21.85 | Tan clear liquid |
| Example 2 | 21.26 | Tan clear liquid |
| Example 3 | 20.79 | Tan clear liquid |
| Comparative example 1 | 10.66 | Tan clear liquid |
| Comparative example 2 | 17.84 | Tan clear liquid |
| Comparative example 3 | 21.09 | A small amount of sediment at the bottom |
| Comparative example 4 | 20.96 | Tan clear liquid |
| Comparative example 5 | 21.21 | Tan clear liquid |
| Comparative example 6 | 21.45 | Tan clear liquid |
| Comparative example 7 | 20.68 | Tan clear liquid |
| Comparative example 8 | 21.17 | Tan clear liquid |
| Comparative example 9 | 20.54 | A small amount of sediment at the bottom |
| Comparative example 10 | 21.33 | Tan clear liquid |
Experimental example 4
And (3) long-term test:
placing the packaged mixture at 25 deg.C + -2 deg.C and relative humidity 60% + -10% for 12 months, sampling every 3 months, respectively sampling at 0 month, 3 months, 6 months, 9 months, and 12 months, detecting baicalin content, and checking properties, the results are shown in Table 2.
Claims (7)
1. A preparation process of a traditional Chinese medicine composition is characterized by comprising the following steps:
(1) pulverizing Chinese medicinal composition into coarse powder, wherein the Chinese medicinal composition comprises rehmanniae radix, radix Ophiopogonis, radix scrophulariae, fructus forsythiae and Scutellariae radix, the rehmanniae radix, radix Ophiopogonis, radix scrophulariae and fructus forsythiae use 57% ethanol as solvent, sodium bicarbonate solution is added to adjust pH, the Scutellariae radix uses 57% ethanol as solvent, sodium hydroxide solution is added to adjust pH, the materials are respectively soaked for 6 hours, the mixture is mixed, slowly percolated at the speed of about 1mL per minute, and percolate is collected;
(2) concentrating percolate under reduced pressure, adding purified water, boiling for 30min, standing for 48 hr, filtering, washing the residue with a small amount of purified water, mixing filtrates, concentrating under reduced pressure to obtain concentrated solution, adding egg white, adding sodium hydroxide solution to adjust pH, heating to 80-95 deg.C for 30-60min, cooling to room temperature, adding benzoic acid to adjust pH, stirring, refrigerating for 24-48 hr, collecting supernatant, filtering, centrifuging, adding water, and stirring.
2. The preparation process of the traditional Chinese medicine composition according to claim 1, wherein the weight ratio of the traditional Chinese medicine composition in the step (1) is as follows: 5-10 parts of rehmannia root, 5-10 parts of dwarf lilyturf tuber, 10-20 parts of figwort root, 15-30 parts of weeping forsythia capsule and 15-30 parts of radix scutellariae.
3. The preparation process of the traditional Chinese medicine composition according to claim 1, wherein the weight ratio of the traditional Chinese medicine composition in the step (1) is as follows: 8 parts of rehmannia root, 10 parts of dwarf lilyturf tuber, 15 parts of figwort root, 20 parts of weeping forsythia capsule and 20 parts of baical skullcap root.
4. The process for preparing a Chinese medicinal composition as claimed in claim 1, wherein the ethanol solution of rehmannia glutinosa, ophiopogon root, figwort root and forsythia fruit in the step (1) is adjusted to pH 6.5-7.0, and the ethanol solution of scutellaria root is adjusted to pH 7.0-7.5.
5. The preparation process of the traditional Chinese medicine composition according to claim 1, wherein the mass volume ratio of the egg white added in the step (2) to the concentrated solution is 0.1-1: 100.
6. the process for preparing a Chinese medicinal composition according to claim 1, wherein the pH of the solution obtained in step (2) is adjusted to 7.5-8.5 by adding sodium hydroxide solution.
7. The process for preparing a Chinese medicinal composition according to claim 1, wherein benzoic acid is added in step (2) to adjust the pH to 5.5-6.0.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011179066.3A CN112168919A (en) | 2020-10-29 | 2020-10-29 | Preparation process of traditional Chinese medicine composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011179066.3A CN112168919A (en) | 2020-10-29 | 2020-10-29 | Preparation process of traditional Chinese medicine composition |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112168919A true CN112168919A (en) | 2021-01-05 |
Family
ID=73917653
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011179066.3A Pending CN112168919A (en) | 2020-10-29 | 2020-10-29 | Preparation process of traditional Chinese medicine composition |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112168919A (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103520470A (en) * | 2013-10-21 | 2014-01-22 | 海南康芝药业股份有限公司 | Preparation method of Chinese medicine mixture |
-
2020
- 2020-10-29 CN CN202011179066.3A patent/CN112168919A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103520470A (en) * | 2013-10-21 | 2014-01-22 | 海南康芝药业股份有限公司 | Preparation method of Chinese medicine mixture |
Non-Patent Citations (1)
| Title |
|---|
| 国家药典委员会: "《中华人民共和国药典：2010年版 一部》", 31 January 2010, 中国医药科技出版社 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107029120B (en) | Preparation method of dendrobium and polygonatum sibiricum soft extract | |
| CN112870236B (en) | Flavone effective part of abelmoschus manihot and preparation method and application thereof | |
| CN111035666A (en) | Ginseng extract with high content of rare saponin, ginseng wine and ginseng oral liquid | |
| CN102293997A (en) | Preparation method of dried ginger extract | |
| CN107519227A (en) | A kind of honeysuckle composition particle and preparation method thereof | |
| CN101347491A (en) | Radical lobelia total flavones effective component and preparation thereof | |
| CN104945532B (en) | The preparation method of Gynura divaricata polysaccharide | |
| CN103463201B (en) | Extraction method of Shuanghuanglian extract | |
| CN110548075A (en) | Preparation method of veterinary ephedra, apricot kernel, gypsum and licorice oral liquid | |
| CN101574398A (en) | Lupulus extractive and preparation method and application thereof | |
| CN112168919A (en) | Preparation process of traditional Chinese medicine composition | |
| CN101190906B (en) | Method for preparing carthamin yellow carthamus B and application thereof | |
| CN108126000A (en) | Arasaponin extracts preparation method in fresh Radix Notoginseng | |
| CN106386810B (en) | New use of chrysanthemum indicum polysaccharide in promoting synthesis of atractylenolide in rhizoma Atractylodis Macrocephalae | |
| CN108969580B (en) | Preparation method and application of blue cloth total tannin | |
| CN107625852A (en) | A kind of clearing heat and promoting diuresis stagnation resolvation stop-band Chinese medicine composition and its preparation technology and application | |
| CN102940724A (en) | Preparation method of traditional Chinese medicine compound capsule for diminishing inflammation | |
| CN110585260A (en) | Single-ingredient freeze-dried powder and preparation method thereof | |
| CN107050095B (en) | Preparation method of gypenoside side chain oligosaccharide | |
| CN100455304C (en) | Compound Jinqiaomai preparation | |
| CN113398232B (en) | Preparation method of pharmaceutical composition for treating gout and gouty arthritis | |
| CN110357979A (en) | A kind of the extraction preparation method and its extract equipment of Fructus Fici extract | |
| CN109432193B (en) | Pharmaceutical composition for treating cough and preparation method thereof | |
| CN116159095B (en) | Preparation method of angelica hexa-yellow Shang Dong dry powder | |
| CN110585335B (en) | Preparation method of yin-nourishing lung-clearing oral liquid |
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 | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210105 |
|
| RJ01 | Rejection of invention patent application after publication |