CN107126461B - Preparation process of water-soluble stephania tetrandra extract - Google Patents
Preparation process of water-soluble stephania tetrandra extract Download PDFInfo
- Publication number
- CN107126461B CN107126461B CN201710332417.1A CN201710332417A CN107126461B CN 107126461 B CN107126461 B CN 107126461B CN 201710332417 A CN201710332417 A CN 201710332417A CN 107126461 B CN107126461 B CN 107126461B
- Authority
- CN
- China
- Prior art keywords
- minutes
- treatment
- ultrasonic treatment
- filtrate
- time
- 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
- 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)
- A61K36/59—Menispermaceae (Moonseed family), e.g. hyperbaena or coralbead
-
- 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
-
- 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
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
-
- 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
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
-
- 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
Landscapes
- Health & Medical Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Alternative & Traditional Medicine (AREA)
- Biotechnology (AREA)
- Botany (AREA)
- Medical Informatics (AREA)
- Medicinal Chemistry (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Medicinal Preparation (AREA)
- Medicines Containing Plant Substances (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses a preparation process of a water-soluble stephania tetrandra extract, which comprises four steps of primary alcohol extraction, secondary alcohol extraction, intermittent ultrasonic treatment and intermittent microwave treatment. The preparation process of the invention realizes the comprehensive extraction of various effective components in the stephania tetrandra, such as isoquinoline alkaloids, flavonoid glycoside, phenols, volatile oil, organic acids, saccharides and the like, and improves the comprehensive utilization rate of the stephania tetrandra medicinal material.
Description
Technical Field
The invention relates to a preparation process, in particular to a preparation process of a water-soluble stephania tetrandra extract. Belongs to the technical field of traditional Chinese medicine extraction.
Background
Menispermum root is distributed in China mostly and mainly used for edema, beriberi, dysuresia, eczema, sore and the like. The tetrandrine mainly contains isoquinoline alkaloids, flavonoid glycoside, phenols, volatile oil, organic acid and saccharides, wherein the isoquinoline alkaloids comprise tetrandrine (tetrandrine), demethyltetrandrine, fangchinoline (fangchinoline) and cyclanoline. Tetrandrine and fangchinoline have analgesic, antiinflammatory, antiallergic, blood pressure lowering, coronary artery dilating, and antitumor effects.
The extraction process of the tetrandrine alkaloid components is researched in the literature 'research on the extraction and purification process of the tetrandrine alkaloid components' (Chinese patent medicine 2014, 36 (6): 1306 and 1309), and the optimal extraction condition of the tetrandrine alkaloid is determined to be 8 times of reflux extraction for 3 times, 3 hours each time, of 70% ethanol aqueous solution with volume concentration through an extraction condition orthogonal design test. However, the effective components of stephania tetrandra include flavonoid glycoside, saccharides and the like instead of one alkaloid, and the applicant finds that the method in the document can not realize the sufficient extraction of other effective components of the stephania tetrandra, and a comprehensive extraction method of the effective components of the stephania tetrandra is still lacked.
In addition, the effective components of the stephania tetrandra are basically insoluble in water except the flavonoid glycoside, so the production and application requirements of water-soluble preparations are difficult to adapt, the absorption of a human body is influenced when the effective components are prepared into other dosage forms, the bioavailability is low, and the clinical application of the stephania tetrandra medicinal material is influenced.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation process of a water-soluble radix stephaniae tetrandrae extract.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation process of a water-soluble radix Stephaniae Tetrandrae extract comprises the following steps:
(1) heating and refluxing a radix stephaniae tetrandrae medicinal material by using an ethanol water solution with the volume concentration of 50-60% and the weight of 3-5 times of that of the radix stephaniae tetrandrae medicinal material for 2-3 times, wherein the extraction time is 1-2 hours each time, combining extracting solutions, filtering, and concentrating the filtrate under reduced pressure to 0.5-1 time of the weight of the medicinal material to obtain an alcohol extract;
(2) heating and refluxing the alcohol extract obtained in the step (1) with an ethanol water solution with volume concentration of 30-40% and weight of 5-8 times of the alcohol extract for 30-50 minutes, cooling to-5 ℃, standing for 12-24 hours, and filtering to remove insoluble impurities to obtain a filtrate;
(3) sequentially adding polyvinylpyrrolidone and polyethylene glycol 4000 into the filtrate while stirring, carrying out intermittent ultrasonic treatment for 20-30 minutes, adding water at the temperature of 55-60 ℃ when ultrasonic treatment is started each time, and obtaining ultrasonic treatment liquid after the treatment is finished;
(4) adding the ultrasonic treatment solution into 1-1.2 times of ethanol water solution with volume concentration of 70-80% by weight, performing intermittent microwave treatment for 10-15 minutes, standing for 30-40 minutes, centrifuging to obtain a precipitate, and performing vacuum drying to obtain the ultrasonic treatment solution.
Wherein the mass ratio of the polyvinylpyrrolidone to the polyethylene glycol 4000 is 1: 1.1, the total mass of the two is 1.1-1.2 times of the filtrate.
Preferably, the specific method of the batch-type ultrasonic treatment in the step (3) is as follows: after the ultrasonic treatment is carried out for 3 minutes, the treatment is continued for 3 minutes after 5 minutes, and the process is circulated until the cumulative time of the ultrasonic treatment reaches 20-30 minutes.
Preferably, in the step (3), the addition amount of the water is 0.2-0.3 times of the filtrate each time.
Preferably, in the step (3), the addition time of the polyvinylpyrrolidone and the polyethylene glycol 4000 lasts for 10 to 15 minutes.
Preferably, the specific method of the batch-type microwave treatment in the step (4) is as follows: after the microwave treatment is carried out for 1 minute at the interval of 1 minute, the microwave treatment is continued for 1 minute at the interval of 300-450W, and the process is circulated until the cumulative time of the microwave treatment reaches 10-15 minutes.
It is further preferred that the microwave frequency during the batch microwave treatment is kept constant.
Preferably, in the step (4), the centrifugal treatment is carried out for 30-60 minutes under the centrifugal condition of 6000 r/min.
Preferably, in the step (4), vacuum drying is carried out for 18-24 hours under the vacuum drying condition of 1.3-6 Pa.
The invention has the beneficial effects that:
the invention mainly realizes the water solubility improvement of the effective components of the stephania tetrandra by adding the polyvinylpyrrolidone and the polyethylene glycol 4000, and because the polyvinylpyrrolidone and the polyethylene glycol 4000 are common auxiliary materials specified in Chinese pharmacopoeia, the safety problem does not exist after the polyvinylpyrrolidone and the polyethylene glycol 4000 are added.
The preparation process comprises four steps of primary alcohol extraction, secondary alcohol extraction, intermittent ultrasonic treatment and intermittent microwave treatment. The volume concentration of an ethanol water solution in the first alcohol extraction is 50-60%, so that the full extraction of effective components in the stephania tetrandra medicinal material is ensured, and the doping of impurities is reduced as much as possible; carrying out secondary alcohol extraction on the basis of the primary alcohol extraction, reducing the volume concentration of the used ethanol aqueous solution to 30-40%, cooling to-5 ℃ after the secondary alcohol extraction treatment, standing for 12-24 hours, and effectively reducing the doping of impurities; adding polyvinylpyrrolidone and polyethylene glycol 4000, then carrying out batch ultrasonic treatment, and adding warm water at the beginning of each ultrasonic treatment to facilitate the full mixing of the effective components with polyvinylpyrrolidone and polyethylene glycol 4000; and finally, adding the ultrasonic treatment liquid into an ethanol water solution with higher volume concentration, and combining intermittent microwave treatment to fully wrap the effective components between the molecules of polyvinylpyrrolidone and polyethylene glycol 4000, thereby greatly improving the water solubility of the obtained extract.
In a word, the preparation process of the invention realizes the comprehensive extraction of various effective components in the stephania tetrandra, such as isoquinoline alkaloids, flavonoid glycoside, phenols, volatile oil, organic acids, saccharides and the like, and improves the comprehensive utilization rate of the stephania tetrandra medicinal material.
Detailed Description
The present invention will be further illustrated by the following examples, which are intended to be merely illustrative and not limitative.
Example 1:
a preparation process of a water-soluble radix Stephaniae Tetrandrae extract comprises the following steps:
(1) heating and reflux-extracting radix Stephaniae Tetrandrae with 3 times of 50% ethanol water solution by volume concentration for 2 times, each time for 1 hr, mixing extractive solutions, filtering, and concentrating the filtrate under reduced pressure to 0.5 times of the weight of the medicinal materials to obtain ethanol extract;
(2) heating and refluxing the alcohol extract obtained in the step (1) with an ethanol water solution with volume concentration of 30% and weight of 5 times of the alcohol extract for 30 minutes, cooling to-5 ℃, standing for 12 hours, and filtering to remove insoluble impurities to obtain a filtrate;
(3) sequentially adding polyvinylpyrrolidone and polyethylene glycol 4000 into the filtrate while stirring, carrying out intermittent ultrasonic treatment for 20-30 minutes, adding water of 55 ℃ when ultrasonic treatment is started each time, and obtaining ultrasonic treatment liquid after the treatment is finished;
(4) adding the ultrasonic treatment solution into 1 time of ethanol water solution with volume concentration of 70% by weight, carrying out intermittent microwave treatment for 10 minutes, standing for 30 minutes, centrifuging to obtain a precipitate, and carrying out vacuum drying to obtain the ultrasonic treatment solution.
Wherein the mass ratio of the polyvinylpyrrolidone to the polyethylene glycol 4000 is 1: 1.1, the total mass of the two is 1.1 times of the filtrate.
The specific method of the intermittent ultrasonic treatment in the step (3) is as follows: after 3 minutes of ultrasonic treatment, the treatment is continued for 3 minutes after 5 minutes, and the process is circulated until the cumulative time of ultrasonic treatment reaches 20 minutes. The amount of water added was 0.2 times the amount of the filtrate each time.
The specific method of the intermittent microwave treatment in the step (4) is as follows: after the microwave treatment of 300W is carried out for 1 minute, the microwave treatment is continued for 1 minute at intervals, and the process is circulated until the cumulative time of the microwave treatment reaches 10 minutes. The microwave frequency in the intermittent microwave treatment process is kept constant. The centrifugation is carried out for 30 minutes under the rotation speed of 6000 r/min. The vacuum drying condition was 1.3Pa for 18 hours.
Example 2:
a preparation process of a water-soluble radix Stephaniae Tetrandrae extract comprises the following steps:
(1) heating and reflux-extracting radix Stephaniae Tetrandrae with 5 times of 60% ethanol water solution by volume concentration for 3 times, each time for 2 hr, mixing extractive solutions, filtering, and concentrating the filtrate under reduced pressure to 1 time of the weight of the medicinal materials to obtain ethanol extract;
(2) heating and refluxing the alcohol extract obtained in the step (1) with 8 times of ethanol water solution with volume concentration of 40% by weight for 50 minutes, cooling to-5 ℃, standing for 24 hours, and filtering to remove insoluble impurities to obtain filtrate;
(3) sequentially adding polyvinylpyrrolidone and polyethylene glycol 4000 into the filtrate while stirring, carrying out intermittent ultrasonic treatment for 30 minutes, adding water of 60 ℃ when each ultrasonic treatment is started, and obtaining ultrasonic treatment liquid after the treatment is finished;
(4) adding the ultrasonic treatment solution into ethanol water solution with volume concentration of 80% and weight of 1.2 times, performing intermittent microwave treatment for 15 minutes, standing for 40 minutes, centrifuging to obtain precipitate, and vacuum drying to obtain the product.
Wherein the mass ratio of the polyvinylpyrrolidone to the polyethylene glycol 4000 is 1: 1.1, the total mass of the two is 1.2 times of the filtrate.
The specific method of the intermittent ultrasonic treatment in the step (3) is as follows: after 3 minutes of ultrasonic treatment, the treatment is continued for 3 minutes after 5 minutes, and the process is circulated until the cumulative time of ultrasonic treatment reaches 30 minutes. The amount of water added was 0.3 times the amount of the filtrate each time.
The specific method of the intermittent microwave treatment in the step (4) is as follows: after the microwave treatment of 450W is carried out for 1 minute, the microwave treatment is continued for 1 minute at intervals, and the process is circulated until the cumulative time of the microwave treatment reaches 15 minutes. The microwave frequency in the intermittent microwave treatment process is kept constant. The centrifugation is carried out for 60 minutes under the rotation speed of 6000 r/min. The vacuum drying condition is 6Pa for 24 hours.
Example 3:
a preparation process of a water-soluble radix Stephaniae Tetrandrae extract comprises the following steps:
(1) heating and reflux-extracting radix Stephaniae Tetrandrae with 3 times of 60% ethanol water solution by volume concentration for 2 times, each time for 2 hr, mixing extractive solutions, filtering, and concentrating the filtrate under reduced pressure to 0.5 times of the weight of the medicinal materials to obtain ethanol extract;
(2) heating and refluxing the alcohol extract obtained in the step (1) with an ethanol water solution with the volume concentration of 30-40% which is 8 times of the weight of the alcohol extract for 30 minutes, cooling to-5 ℃, standing for 24 hours, and filtering to remove insoluble impurities to obtain a filtrate;
(3) sequentially adding polyvinylpyrrolidone and polyethylene glycol 4000 into the filtrate while stirring, carrying out intermittent ultrasonic treatment for 20 minutes, adding water of 60 ℃ when each ultrasonic treatment is started, and obtaining ultrasonic treatment liquid after the treatment is finished;
(4) adding the ultrasonic treatment solution into an ethanol aqueous solution with volume concentration of 80% and weight of 1 time, carrying out intermittent microwave treatment for 10 minutes, standing for 40 minutes, centrifuging to obtain a precipitate, and carrying out vacuum drying to obtain the ultrasonic treatment solution.
Wherein the mass ratio of the polyvinylpyrrolidone to the polyethylene glycol 4000 is 1: 1.1, the total mass of the two is 1.1 times of the filtrate.
The specific method of the intermittent ultrasonic treatment in the step (3) is as follows: after 3 minutes of ultrasonic treatment, the treatment is continued for 3 minutes after 5 minutes, and the process is circulated until the cumulative time of ultrasonic treatment reaches 30 minutes. The amount of water added was 0.2 times the amount of the filtrate each time. The addition time of polyvinylpyrrolidone and polyethylene glycol 4000 lasted 15 minutes.
The specific method of the intermittent microwave treatment in the step (4) is as follows: after the microwave treatment of 300W is carried out for 1 minute, the microwave treatment is continued for 1 minute at intervals, and the process is circulated until the cumulative time of the microwave treatment reaches 15 minutes. The microwave frequency in the intermittent microwave treatment process is kept constant. The centrifugation is carried out for 30 minutes under the rotation speed of 6000 r/min. The vacuum drying condition is 6Pa for 18 hours.
Example 4:
a preparation process of a water-soluble radix Stephaniae Tetrandrae extract comprises the following steps:
(1) heating and reflux-extracting radix Stephaniae Tetrandrae with 5 times of 50% ethanol water solution by volume concentration for 3 times, wherein the extraction time is 1 hr each time, mixing extractive solutions, filtering, and concentrating the filtrate under reduced pressure to 1 time of the weight of the medicinal materials to obtain ethanol extract;
(2) heating and refluxing the alcohol extract obtained in the step (1) with 5 times of ethanol water solution with volume concentration of 40% by weight for 30 minutes, cooling to-5 ℃, standing for 24 hours, and filtering to remove insoluble impurities to obtain filtrate;
(3) sequentially adding polyvinylpyrrolidone and polyethylene glycol 4000 into the filtrate while stirring, carrying out intermittent ultrasonic treatment for 20 minutes, adding water of 60 ℃ when each ultrasonic treatment is started, and obtaining ultrasonic treatment liquid after the treatment is finished;
(4) adding the ultrasonic treatment solution into an ethanol aqueous solution with volume concentration of 80% and weight of 1 time, carrying out intermittent microwave treatment for 10 minutes, standing for 40 minutes, centrifuging to obtain a precipitate, and carrying out vacuum drying to obtain the ultrasonic treatment solution.
Wherein the mass ratio of the polyvinylpyrrolidone to the polyethylene glycol 4000 is 1: 1.1, the total mass of the two is 1.1 times of the filtrate.
The specific method of the intermittent ultrasonic treatment in the step (3) is as follows: after 3 minutes of ultrasonic treatment, the treatment is continued for 3 minutes after 5 minutes, and the process is circulated until the cumulative time of ultrasonic treatment reaches 30 minutes. The amount of water added was 0.2 times the amount of the filtrate each time. The addition time of polyvinylpyrrolidone and polyethylene glycol 4000 lasted 15 minutes.
The specific method of the intermittent microwave treatment in the step (4) is as follows: after the microwave treatment of 300W is carried out for 1 minute, the microwave treatment is continued for 1 minute at intervals, and the process is circulated until the cumulative time of the microwave treatment reaches 15 minutes. The microwave frequency in the intermittent microwave treatment process is kept constant. The centrifugation is carried out for 30 minutes under the rotation speed of 6000 r/min. The vacuum drying condition is 6Pa for 18 hours.
Example 5:
a preparation process of a water-soluble radix Stephaniae Tetrandrae extract comprises the following steps:
(1) heating and reflux-extracting radix Stephaniae Tetrandrae with 55% ethanol water solution 4 times by weight for 2 times, each time for 1 hr, mixing extractive solutions, filtering, and concentrating the filtrate under reduced pressure to 0.8 times of the weight of the medicinal materials to obtain ethanol extract;
(2) heating and refluxing the alcohol extract obtained in the step (1) with an ethanol water solution with the volume concentration of 35% and the weight of 6 times of that of the alcohol extract for 40 minutes, cooling to-5 ℃, standing for 18 hours, and filtering to remove insoluble impurities to obtain a filtrate;
(3) sequentially adding polyvinylpyrrolidone and polyethylene glycol 4000 into the filtrate while stirring, carrying out intermittent ultrasonic treatment for 25 minutes, adding water of 55 ℃ when each ultrasonic treatment is started, and obtaining ultrasonic treatment liquid after the treatment is finished;
(4) adding the ultrasonic treatment solution into 1.1 times of ethanol water solution with volume concentration of 75% by weight, carrying out intermittent microwave treatment for 12 minutes, standing for 35 minutes, centrifuging to obtain a precipitate, and carrying out vacuum drying to obtain the ultrasonic treatment solution.
Wherein the mass ratio of the polyvinylpyrrolidone to the polyethylene glycol 4000 is 1: 1.1, the total mass of the two is 1.1 times of the filtrate.
The specific method of the intermittent ultrasonic treatment in the step (3) is as follows: after 3 minutes of ultrasonic treatment, the treatment is continued for 3 minutes after 5 minutes, and the process is circulated until the cumulative time of ultrasonic treatment reaches 25 minutes. The amount of water added was 0.33 times the amount of the filtrate each time. The addition time of polyvinylpyrrolidone and polyethylene glycol 4000 lasted 12 minutes.
The specific method of the intermittent microwave treatment in the step (4) is as follows: after the microwave treatment of 450W is carried out for 1 minute, the microwave treatment is continued for 1 minute at intervals, and the process is circulated until the cumulative time of the microwave treatment reaches 12 minutes. The microwave frequency in the intermittent microwave treatment process is kept constant. The centrifugation is carried out for 40 minutes under the rotation speed of 6000 r/min. The vacuum drying condition is 2Pa for 20 hours.
Comparative example 1
A preparation process of a radix stephaniae tetrandrae extract comprises the following specific steps:
(1) heating and reflux-extracting radix Stephaniae Tetrandrae with 4 times of 35% ethanol water solution by volume concentration for 2 times, each time for 1 hr, mixing extractive solutions, filtering, and concentrating the filtrate under reduced pressure to 0.8 times of the weight of the medicinal materials to obtain ethanol extract;
(2) heating and refluxing the alcohol extract obtained in the step (1) with 55% ethanol water solution with volume concentration 6 times of the weight of the alcohol extract for 40 minutes, cooling to-5 ℃, standing for 18 hours, and filtering to remove insoluble impurities to obtain filtrate;
(3) sequentially adding polyvinylpyrrolidone and polyethylene glycol 4000 into the filtrate while stirring, carrying out intermittent ultrasonic treatment for 25 minutes, adding water of 55 ℃ when each ultrasonic treatment is started, and obtaining ultrasonic treatment liquid after the treatment is finished;
(4) adding the ultrasonic treatment solution into 1.1 times of ethanol water solution with volume concentration of 75% by weight, carrying out intermittent microwave treatment for 12 minutes, standing for 35 minutes, centrifuging to obtain a precipitate, and carrying out vacuum drying to obtain the ultrasonic treatment solution.
Wherein the mass ratio of the polyvinylpyrrolidone to the polyethylene glycol 4000 is 1: 1.1, the total mass of the two is 1.1 times of the filtrate.
The specific method of the intermittent ultrasonic treatment in the step (3) is as follows: after 3 minutes of ultrasonic treatment, the treatment is continued for 3 minutes after 5 minutes, and the process is circulated until the cumulative time of ultrasonic treatment reaches 25 minutes. The amount of water added was 0.33 times the amount of the filtrate each time. The addition time of polyvinylpyrrolidone and polyethylene glycol 4000 lasted 12 minutes.
The specific method of the intermittent microwave treatment in the step (4) is as follows: after the microwave treatment of 450W is carried out for 1 minute, the microwave treatment is continued for 1 minute at intervals, and the process is circulated until the cumulative time of the microwave treatment reaches 12 minutes. The microwave frequency in the intermittent microwave treatment process is kept constant. The centrifugation is carried out for 40 minutes under the rotation speed of 6000 r/min. The vacuum drying condition is 2Pa for 20 hours.
Comparative example 2
A preparation process of a radix stephaniae tetrandrae extract comprises the following specific steps:
(1) heating and reflux-extracting radix Stephaniae Tetrandrae with 55% ethanol water solution 4 times by weight for 2 times, each time for 1 hr, mixing extractive solutions, filtering, concentrating the filtrate under reduced pressure to 0.8 times of the weight of the medicinal materials, cooling to-5 deg.C, standing for 18 hr, and filtering to remove insoluble impurities to obtain filtrate;
(2) sequentially adding polyvinylpyrrolidone and polyethylene glycol 4000 into the filtrate while stirring, carrying out intermittent ultrasonic treatment for 25 minutes, adding water of 55 ℃ when each ultrasonic treatment is started, and obtaining ultrasonic treatment liquid after the treatment is finished;
(3) adding the ultrasonic treatment solution into 1.1 times of ethanol water solution with volume concentration of 75% by weight, carrying out intermittent microwave treatment for 12 minutes, standing for 35 minutes, centrifuging to obtain a precipitate, and carrying out vacuum drying to obtain the ultrasonic treatment solution.
Wherein the mass ratio of the polyvinylpyrrolidone to the polyethylene glycol 4000 is 1: 1.1, the total mass of the two is 1.1 times of the filtrate.
The specific method of the intermittent ultrasonic treatment in the step (2) is as follows: after 3 minutes of ultrasonic treatment, the treatment is continued for 3 minutes after 5 minutes, and the process is circulated until the cumulative time of ultrasonic treatment reaches 25 minutes. The amount of water added was 0.33 times the amount of the filtrate each time. The addition time of polyvinylpyrrolidone and polyethylene glycol 4000 lasted 12 minutes.
The specific method of the intermittent microwave treatment in the step (3) is as follows: after the microwave treatment of 450W is carried out for 1 minute, the microwave treatment is continued for 1 minute at intervals, and the process is circulated until the cumulative time of the microwave treatment reaches 12 minutes. The microwave frequency in the intermittent microwave treatment process is kept constant. The centrifugation is carried out for 40 minutes under the rotation speed of 6000 r/min. The vacuum drying condition is 2Pa for 20 hours.
Comparative example 3
A preparation process of a radix stephaniae tetrandrae extract comprises the following specific steps:
(1) heating and reflux-extracting radix Stephaniae Tetrandrae with 55% ethanol water solution 4 times by weight for 2 times, each time for 1 hr, mixing extractive solutions, filtering, and concentrating the filtrate under reduced pressure to 0.8 times of the weight of the medicinal materials to obtain ethanol extract;
(2) heating and refluxing the alcohol extract obtained in the step (1) with an ethanol water solution with the volume concentration of 35% and the weight of 6 times of that of the alcohol extract for 40 minutes, cooling to-5 ℃, standing for 18 hours, and filtering to remove insoluble impurities to obtain a filtrate;
(3) adding polyvinylpyrrolidone into the filtrate while stirring, carrying out intermittent ultrasonic treatment for 25 minutes, adding water with the temperature of 55 ℃ when each ultrasonic treatment is started, and obtaining ultrasonic treatment liquid after the treatment is finished;
(4) adding the ultrasonic treatment solution into 1.1 times of ethanol water solution with volume concentration of 75% by weight, carrying out intermittent microwave treatment for 12 minutes, standing for 35 minutes, centrifuging to obtain a precipitate, and carrying out vacuum drying to obtain the ultrasonic treatment solution.
Wherein the mass of the polyvinylpyrrolidone is 1.1 times of that of the filtrate.
The specific method of the intermittent ultrasonic treatment in the step (3) is as follows: after 3 minutes of ultrasonic treatment, the treatment is continued for 3 minutes after 5 minutes, and the process is circulated until the cumulative time of ultrasonic treatment reaches 25 minutes. The amount of water added was 0.33 times the amount of the filtrate each time. The addition time of the polyvinylpyrrolidone lasted 12 minutes.
The specific method of the intermittent microwave treatment in the step (4) is as follows: after the microwave treatment of 450W is carried out for 1 minute, the microwave treatment is continued for 1 minute at intervals, and the process is circulated until the cumulative time of the microwave treatment reaches 12 minutes. The microwave frequency in the intermittent microwave treatment process is kept constant. The centrifugation is carried out for 40 minutes under the rotation speed of 6000 r/min. The vacuum drying condition is 2Pa for 20 hours.
Comparative example 4
A preparation process of a radix stephaniae tetrandrae extract comprises the following specific steps:
(1) heating and reflux-extracting radix Stephaniae Tetrandrae with 55% ethanol water solution 4 times by weight for 2 times, each time for 1 hr, mixing extractive solutions, filtering, and concentrating the filtrate under reduced pressure to 0.8 times of the weight of the medicinal materials to obtain ethanol extract;
(2) heating and refluxing the alcohol extract obtained in the step (1) with an ethanol water solution with the volume concentration of 35% and the weight of 6 times of that of the alcohol extract for 40 minutes, cooling to-5 ℃, standing for 18 hours, and filtering to remove insoluble impurities to obtain a filtrate;
(3) adding polyethylene glycol 4000 into the filtrate while stirring, carrying out intermittent ultrasonic treatment for 25 minutes, adding water with the temperature of 55 ℃ when each ultrasonic treatment is started, and obtaining an ultrasonic treatment solution after the treatment is finished;
(4) adding the ultrasonic treatment solution into 1.1 times of ethanol water solution with volume concentration of 75% by weight, carrying out intermittent microwave treatment for 12 minutes, standing for 35 minutes, centrifuging to obtain a precipitate, and carrying out vacuum drying to obtain the ultrasonic treatment solution.
Wherein, the mass of the polyethylene glycol 4000 is 1.1 times of that of the filtrate.
The specific method of the intermittent ultrasonic treatment in the step (3) is as follows: after 3 minutes of ultrasonic treatment, the treatment is continued for 3 minutes after 5 minutes, and the process is circulated until the cumulative time of ultrasonic treatment reaches 25 minutes. The amount of water added was 0.33 times the amount of the filtrate each time. The addition of polyethylene glycol 4000 continued for 12 minutes.
The specific method of the intermittent microwave treatment in the step (4) is as follows: after the microwave treatment of 450W is carried out for 1 minute, the microwave treatment is continued for 1 minute at intervals, and the process is circulated until the cumulative time of the microwave treatment reaches 12 minutes. The microwave frequency in the intermittent microwave treatment process is kept constant. The centrifugation is carried out for 40 minutes under the rotation speed of 6000 r/min. The vacuum drying condition is 2Pa for 20 hours.
Comparative example 5
A preparation process of a radix stephaniae tetrandrae extract comprises the following specific steps:
(1) heating and reflux-extracting radix Stephaniae Tetrandrae with 55% ethanol water solution 4 times by weight for 2 times, each time for 1 hr, mixing extractive solutions, filtering, and concentrating the filtrate under reduced pressure to 0.8 times of the weight of the medicinal materials to obtain ethanol extract;
(2) heating and refluxing the alcohol extract obtained in the step (1) with an ethanol water solution with the volume concentration of 35% and the weight of 6 times of that of the alcohol extract for 40 minutes, cooling to-5 ℃, standing for 18 hours, and filtering to remove insoluble impurities to obtain a filtrate;
(3) sequentially adding polyvinylpyrrolidone and polyethylene glycol 4000 into the filtrate while stirring, and carrying out intermittent ultrasonic treatment for 25 minutes to obtain an ultrasonic treatment solution after the treatment is finished;
(4) adding the ultrasonic treatment solution into 1.1 times of ethanol water solution with volume concentration of 75% by weight, carrying out intermittent microwave treatment for 12 minutes, standing for 35 minutes, centrifuging to obtain a precipitate, and carrying out vacuum drying to obtain the ultrasonic treatment solution.
Wherein the mass ratio of the polyvinylpyrrolidone to the polyethylene glycol 4000 is 1: 1.1, the total mass of the two is 1.1 times of the filtrate.
The specific method of the intermittent ultrasonic treatment in the step (3) is as follows: after 3 minutes of ultrasonic treatment, the treatment is continued for 3 minutes after 5 minutes, and the process is circulated until the cumulative time of ultrasonic treatment reaches 25 minutes. The amount of water added was 0.33 times the amount of the filtrate each time. The addition time of polyvinylpyrrolidone and polyethylene glycol 4000 lasted 12 minutes.
The specific method of the intermittent microwave treatment in the step (4) is as follows: after the microwave treatment of 450W is carried out for 1 minute, the microwave treatment is continued for 1 minute at intervals, and the process is circulated until the cumulative time of the microwave treatment reaches 12 minutes. The microwave frequency in the intermittent microwave treatment process is kept constant. The centrifugation is carried out for 40 minutes under the rotation speed of 6000 r/min. The vacuum drying condition is 2Pa for 20 hours.
Comparative example 6
A preparation process of a radix stephaniae tetrandrae extract comprises the following specific steps:
(1) heating and reflux-extracting radix Stephaniae Tetrandrae with 55% ethanol water solution 4 times by weight for 2 times, each time for 1 hr, mixing extractive solutions, filtering, and concentrating the filtrate under reduced pressure to 0.8 times of the weight of the medicinal materials to obtain ethanol extract;
(2) heating and refluxing the alcohol extract obtained in the step (1) with an ethanol water solution with the volume concentration of 35% and the weight of 6 times of that of the alcohol extract for 40 minutes, cooling to-5 ℃, standing for 18 hours, and filtering to remove insoluble impurities to obtain a filtrate;
(3) and sequentially adding polyvinylpyrrolidone and polyethylene glycol 4000 into the filtrate while stirring, carrying out intermittent ultrasonic treatment for 25 minutes, adding water with the temperature of 55 ℃ when each ultrasonic treatment is started, obtaining ultrasonic treatment liquid after the treatment is finished, standing for 35 minutes, centrifuging to obtain a precipitate, and carrying out vacuum drying to obtain the nano-silver-copper-zinc-aluminum composite material.
Wherein the mass ratio of the polyvinylpyrrolidone to the polyethylene glycol 4000 is 1: 1.1, the total mass of the two is 1.1 times of the filtrate.
The specific method of the intermittent ultrasonic treatment in the step (3) is as follows: after 3 minutes of ultrasonic treatment, the treatment is continued for 3 minutes after 5 minutes, and the process is circulated until the cumulative time of ultrasonic treatment reaches 25 minutes. The amount of water added was 0.33 times the amount of the filtrate each time. The addition time of polyvinylpyrrolidone and polyethylene glycol 4000 lasted 12 minutes.
Test examples
The preparation processes of examples 1 to 5 and comparative examples 1 to 6 are respectively adopted to obtain extracts of stephania tetrandra of the same producing area, the solubility in water is measured according to the standard in the Chinese pharmacopoeia 2010 edition, and the contents of tetrandrine (tetrandrine), fangchinoline (tetrandrine), flavonoid glycoside, phenols and organic acid in the extracts (the contents of all effective components in the extracts are converted into 100g of stephania tetrandra medicinal materials) are detected, and the results are shown in table 1.
TABLE 1 test results
As can be seen from Table 1, in the step (3) of examples 1 and 2, the slow addition of polyvinylpyrrolidone and polyethylene glycol 4000 was not controlled, and the obtained extracts had slightly low solubility in water and slightly low contents of the respective active ingredients; comparative example 1 the concentration of the ethanol aqueous solution in the step (1) and the step (2) is reversed, and the comparative example 2 only carries out alcohol extraction once, so that the content of each effective component of the obtained extract is obviously reduced; comparative example 3 only polyvinylpyrrolidone was added in step (3), comparative example 4 only polyethylene glycol 4000 was added in step (3), comparative example 5 no warm water was added during the sonication in step (3), and comparative example 6 the microwave treatment step was omitted, and the aqueous solubility of the obtained extract was significantly reduced.
Although the present invention has been described with reference to the specific embodiments, it is not intended to limit the scope of the present invention, and various modifications and variations can be made by those skilled in the art without inventive changes based on the technical solution of the present invention.
Claims (6)
1. A preparation process of a water-soluble radix Stephaniae Tetrandrae extract comprises the following steps:
(1) heating and refluxing a radix stephaniae tetrandrae medicinal material by using an ethanol water solution with the volume concentration of 50-60% and the weight of 3-5 times of that of the radix stephaniae tetrandrae medicinal material for 2-3 times, wherein the extraction time is 1-2 hours each time, combining extracting solutions, filtering, and concentrating the filtrate under reduced pressure to 0.5-1 time of the weight of the medicinal material to obtain an alcohol extract;
(2) heating and refluxing the alcohol extract obtained in the step (1) with an ethanol water solution with volume concentration of 30-40% and weight of 5-8 times of the alcohol extract for 30-50 minutes, cooling to-5 ℃, standing for 12-24 hours, and filtering to remove insoluble impurities to obtain a filtrate;
(3) sequentially adding polyvinylpyrrolidone and polyethylene glycol 4000 into the filtrate while stirring, carrying out intermittent ultrasonic treatment for 20-30 minutes, adding water at the temperature of 55-60 ℃ when ultrasonic treatment is started each time, and obtaining ultrasonic treatment liquid after the treatment is finished;
(4) adding the ultrasonic treatment solution into 1-1.2 times of ethanol water solution with volume concentration of 70-80% by weight, performing intermittent microwave treatment for 10-15 minutes, standing for 30-40 minutes, centrifuging to obtain a precipitate, and performing vacuum drying to obtain the ultrasonic treatment solution;
wherein the mass ratio of the polyvinylpyrrolidone to the polyethylene glycol 4000 is 1: 1.1, wherein the total mass of the two is 1.1-1.2 times of that of the filtrate;
the specific method of the intermittent ultrasonic treatment in the step (3) is as follows: after the ultrasonic treatment is carried out for 3 minutes, the treatment is continued for 3 minutes after 5 minutes, and the process is circulated until the cumulative time of the ultrasonic treatment reaches 20-30 minutes;
in the step (3), the addition amount of water is 0.2-0.3 times of the filtrate each time.
2. The process according to claim 1, wherein the polyvinylpyrrolidone and the polyethylene glycol 4000 are added for 10 to 15 minutes in the step (3).
3. The production process according to claim 1, wherein the specific method of the batch-type microwave treatment in the step (4) is: after the microwave treatment is carried out for 1 minute at the interval of 1 minute, the microwave treatment is continued for 1 minute at the interval of 300-450W, and the process is circulated until the cumulative time of the microwave treatment reaches 10-15 minutes.
4. The process according to claim 3, wherein the frequency of the microwaves is kept constant during the batch-wise microwave treatment.
5. The preparation process according to claim 1, wherein in the step (4), the centrifugal treatment is carried out for 30-60 minutes at a rotating speed of 6000 r/min.
6. The preparation process according to claim 1, wherein in the step (4), the vacuum drying is performed under 1.3 to 6Pa for 18 to 24 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710332417.1A CN107126461B (en) | 2017-05-12 | 2017-05-12 | Preparation process of water-soluble stephania tetrandra extract |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710332417.1A CN107126461B (en) | 2017-05-12 | 2017-05-12 | Preparation process of water-soluble stephania tetrandra extract |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107126461A CN107126461A (en) | 2017-09-05 |
| CN107126461B true CN107126461B (en) | 2020-08-04 |
Family
ID=59732862
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710332417.1A Active CN107126461B (en) | 2017-05-12 | 2017-05-12 | Preparation process of water-soluble stephania tetrandra extract |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107126461B (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1658890A (en) * | 2002-07-18 | 2005-08-24 | 中国中医研究院中药研究所 | Preparation extracted from tetrandra root and its use |
| CN101259166A (en) * | 2008-04-23 | 2008-09-10 | 中国科学院化学研究所 | Application of stephania tetrandra extract in preparing anti-tumor medicaments |
-
2017
- 2017-05-12 CN CN201710332417.1A patent/CN107126461B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1658890A (en) * | 2002-07-18 | 2005-08-24 | 中国中医研究院中药研究所 | Preparation extracted from tetrandra root and its use |
| CN101259166A (en) * | 2008-04-23 | 2008-09-10 | 中国科学院化学研究所 | Application of stephania tetrandra extract in preparing anti-tumor medicaments |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107126461A (en) | 2017-09-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112375075B (en) | Method for extracting puerarin by using natural eutectic solvent | |
| CN113150867B (en) | Preparation method of ganoderma lucidum extract oil rich in ganoderma lucidum triterpenes | |
| CN103145660B (en) | Andrographolide and preparation method thereof | |
| CN102816155B (en) | Preparation method of silymarin | |
| CN1171610C (en) | Traditional Chinese medicine injection for curing cardiovascular and cerebrovascular diseases and fundus disease and its preparing method | |
| CN112618583A (en) | Preparation method of antrodia camphorata dropping pill | |
| CN105311075A (en) | Preparation method of manyprickle acanthopanax root extract | |
| CN110437041A (en) | It is a kind of using industrial hemp as the preparation method of the cannabidiol of raw material | |
| CN107126461B (en) | Preparation process of water-soluble stephania tetrandra extract | |
| CN115844937A (en) | Preparation method and application of sonchus oleraceus extract with functions of dispelling effects of alcohol and protecting brain | |
| CN100484929C (en) | Rod sage root extract and making method of its preparation | |
| CN115227744B (en) | Lung-tonifying and blood-activating capsule and preparation method thereof | |
| CN107474151A (en) | A kind of processing method for obtaining dendrobium polysaccharide from the stem of noble dendrobium with alcohol deposition method | |
| CN112143769B (en) | A method for preparing radix Puerariae polypeptide extract from radix Puerariae residue and radix Puerariae polypeptide extract prepared thereby | |
| CN105395583A (en) | Preparing method for acanthopanax senticosus extract | |
| CN115737569B (en) | Preparation method of radix angelicae formula particles | |
| CN112315937A (en) | Fibrauretine soft capsule and preparation method thereof | |
| CN106632549B (en) | A kind of method of naringin in ionic liquid extract pomelo peel | |
| CN111297807A (en) | Method for preparing bifunctional genistein-high polymer nano complex by ion crosslinking method and application | |
| CN110559360A (en) | Ganmaoling granules and alcohol precipitation process thereof | |
| CN114306415B (en) | Preparation method for improving content of index component in pulp powder of dogwood fruit | |
| CN104758241B (en) | Left golden micro emulsion gel for treating epigastric pain and preparation method thereof | |
| CN102755396A (en) | Preparation process and matrix for gel cream for treating coronary heart disease | |
| CN106822251B (en) | Preparation method of corydalis amabilis capsule | |
| CN104546994A (en) | Jatropha extracting method and antifungal application |
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 | ||
| CP03 | Change of name, title or address |
Address after: No.324, jingwuweiqi Road, Jinan City, Shandong Province Patentee after: Shandong Provincial Hospital Affiliated to Shandong First Medical University Address before: Shandong Provincial Hospital, No.324, jingwuweiqi Road, Huaiyin District, Jinan City, Shandong Province, 250021 Patentee before: SHANDONG PROVINCIAL Hospital |
|
| CP03 | Change of name, title or address | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Application publication date: 20170905 Assignee: Shandong Xiyang infinite good medical technology Co.,Ltd. Assignor: Shandong Provincial Hospital Affiliated to Shandong First Medical University Contract record no.: X2021980015262 Denomination of invention: A preparation process of water-soluble Fangji extract Granted publication date: 20200804 License type: Common License Record date: 20211217 |
|
| EE01 | Entry into force of recordation of patent licensing contract |