CN110483517A - A kind of preparation method of matrine - Google Patents
A kind of preparation method of matrine Download PDFInfo
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- CN110483517A CN110483517A CN201910773604.2A CN201910773604A CN110483517A CN 110483517 A CN110483517 A CN 110483517A CN 201910773604 A CN201910773604 A CN 201910773604A CN 110483517 A CN110483517 A CN 110483517A
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y5/00—Nanobiotechnology or nanomedicine, e.g. protein engineering or drug delivery
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D471/00—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, at least one ring being a six-membered ring with one nitrogen atom, not provided for by groups C07D451/00 - C07D463/00
- C07D471/22—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, at least one ring being a six-membered ring with one nitrogen atom, not provided for by groups C07D451/00 - C07D463/00 in which the condensed systems contains four or more hetero rings
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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Abstract
The invention discloses a kind of preparation methods of matrine, 1) investment fills in the glassware of sodium chloride solution after cleaning the raw material of matrine processed, the positive and negative electrode piece of pulse stimulater is located in the glassware in the sodium chloride solution at both ends, after pulse current stimulating, pulse stimulater is closed, taking-up raw material carries out cleaning and dries；2) raw material after drying is crushed, and is mixed after being crushed to 20~30 mesh with water, and the primary raw materials liquid that psychrometric ratio is 1~2:0.6~3.5 is obtained；3) primary raw materials liquid is ground to wherein particle diameter and less than 100 microns obtains intermediate material liquid；4) intermediate material liquid is subjected to CO2Supercritical extract, then twice by separator separation, spray drying is made content and is greater than the 50% matrine original powder less than 75%；Process of the present invention is simple, at low cost, easy to operate, low consumption, the matrine for efficiently, quickly producing high-purity.
Description
Technical field
The present invention relates to medicine extractive technique field more particularly to a kind of preparation methods of matrine.
Background technique
Sophora flavescens ait is the dry root of leguminous plant kuh-seng (Sophors flavescens Ait), bitter, it is cold in nature, have it is clear
The effects of tiing up eliminating dampness, desinsection, clinically for treating dysentery, jaundice and skin itching disease, in recent years it has also been found that having antitumor, liter
White equal pharmacological actions.
The alkaloids such as matrine, oxymatrine are mainly contained in kuh-seng.Wherein, matrine is that a kind of pair of human health has
The natural active matter of significant health-care effect, has caused the common concern of international community, has proved through scientific research and clinical application,
Matrine has antitumor, increasing leucocyte, eliminating the phlegm of relievining asthma, analgesia, antiallergy and immunosuppressive action.
Then matrine is not only and contains in kuh-seng, and Sophora alopecuroide, subprostrate sophora etc. also contain matrine, contains matrine vegetable
Matrine extracting method more there are commonly solvent extraction methodes and ion-exchange.Traditional extracting method, Banlangen go out
Cream rate is high, i.e., impurity is more in obtained extract, and extraction effect is poor.
And other abstraction techniques are used, the matrine content in the matrine original powder of extraction is often below 50%, extracts
Effect is also poor.
Summary of the invention
Of the invention provides a kind of preparation method of matrine.
The scheme of the invention is:
A kind of preparation method of matrine, including the following steps:
1) investment fills in the glassware of sodium chloride solution after cleaning the raw material of matrine processed, and pulse stimulater is just
Negative electrode plate is located in the glassware in the sodium chloride solution at both ends, after pulse current stimulating, closes pulse
Stimulator, taking-up raw material carry out cleaning and dry；
2) raw material after drying is crushed, and is mixed after being crushed to 20~30 mesh with water, and obtaining psychrometric ratio is 1~2:0.6
~3.5 primary raw materials liquid；
3) primary raw materials liquid is ground to wherein particle diameter and less than 100 microns obtains intermediate material liquid；
4) intermediate material liquid is subjected to CO2Then twice by separator separation supercritical extract is spray-dried, be made
Content is greater than the 50% matrine original powder less than 75%.
As a preferred technical solution, further include that step 5) mixes matrine original powder with water, obtain psychrometric ratio be 1:4~
8 kuh-seng lye, kuh-seng lye is ground, and being ground to wherein particle diameter, less than 30 microns, ground kuh-seng lye carries out
Extraction, obtains the kuh-seng lye that average particle size is less than 1000nm, and it is total that the particle that wherein partial size is less than 900nm accounts for all particles
95% or more of amount；
6) matrine slurries extracted are placed in cryogenic vacuum concentrator it to be carried out be concentrated into moisture content and are lower than
80%.
The extraction in the step 5) includes supercritical extract, microwave abstracting, ultrasonic wave extraction as a preferred technical solution,
Take, high hydrostatic pressure extraction and it is nano-milled extraction one of or multiple combinations.
The supercritical extract uses pressure for 25~80MPa as a preferred technical solution, 5~25KW of power, temperature
It is≤40 DEG C, fluid flow is 1000~1500L/h；
For the frequency that microwave abstracting uses for 300~900MHz, power is 5~25KW, and temperature is≤40 DEG C；
For the frequency that ultrasonic extraction uses for 20~50KHz, power is 5~25KW, and temperature is≤40 DEG C；
For the pressure that high hydrostatic pressure extraction uses for 200~300MPa, power is 5~25KW, and temperature is≤40 DEG C, fluid flow
For 1000~1500L/h；
For the nano-milled pressure used that extracts for 50~80MPa, power is 5~25KW, and temperature is≤40 DEG C, fluid flow
For 1000~5000L/h；
As a preferred technical solution, it is described 6) in after concentration matrine slurries by Vacuum Drying Equipment contain it
Water is lower than 15%, obtains solid high-purity nano matrine.
The electric current of positive and negative electrode piece described in step 1) is by the pulse stimulater through 20M as a preferred technical solution,
Ω resistance provides.
CO in step 4) as a preferred technical solution,2Supercritical extract, pressure control is in 20~40MPa, temperature control
At 25~40 DEG C, the time is 30~60min.
The grinding is one such using colloid mill or Cone crusher as a preferred technical solution,.
Raw material includes that kuh-seng, Sophora alopecuroide, subprostrate sophora etc. contain matrine in the step 1) as a preferred technical solution,
Plant.
By adopting the above-described technical solution, a kind of preparation method of matrine, 1) it will be after the raw material cleaning of matrine processed
Investment fills in the glassware of sodium chloride solution, and the positive and negative electrode piece of pulse stimulater is located at two in the glassware
In the sodium chloride solution at end, after pulse current stimulating, pulse stimulater is closed, taking-up raw material carries out cleaning and dries；2) it shines
Raw material after dry is crushed, and is mixed after being crushed to 20~30 mesh with water, and it is former to obtain the primary that psychrometric ratio is 1~2:0.6~3.5
Feed liquid；3) primary raw materials liquid is ground to wherein particle diameter and less than 100 microns obtains intermediate material liquid；It 4) will be intermediate former
Feed liquid carries out CO2Supercritical extract, then twice by separator separation, spray drying is made content and is less than greater than 50%
75% matrine original powder.
Advantages of the present invention:
Process is simple, at low cost, easy to operate, low consumption, efficiently, the matrine of quick production high-purity, and to containing
Matrine vegetable can use, and containing matrine vegetable raw material to all can extract, and this method low consumption is high
Effect, it is low-cost, it is suitble to industrialized production, extraction is complete, and level of residue is few, the purity of product is improved, because its nanoscale is high
Purity can be fully absorbed by organism, kill disease pest and weed when acting on plant pest, will not make to act on plant and generate to resist
Pharmacological property will not generate any harm to ecological environment, green safe.
Specific embodiment
In order to make up the above deficiency, the present invention provides a kind of preparation methods of matrine to solve in above-mentioned background technique
The problem of.
A kind of preparation method of matrine, including the following steps:
1) investment fills in the glassware of sodium chloride solution after cleaning the raw material of matrine processed, and pulse stimulater is just
Negative electrode plate is located in the glassware in the sodium chloride solution at both ends, after pulse current stimulating, closes pulse
Stimulator, taking-up raw material carry out cleaning and dry；
2) raw material after drying is crushed, and is mixed after being crushed to 20~30 mesh with water, and obtaining psychrometric ratio is 1~2:0.6
~3.5 primary raw materials liquid；
3) primary raw materials liquid is ground to wherein particle diameter and less than 100 microns obtains intermediate material liquid；
4) intermediate material liquid is subjected to CO2Then twice by separator separation supercritical extract is spray-dried, be made
Content is greater than the 50% matrine original powder less than 75%.
Further include that step 5) mixes matrine original powder with water, the kuh-seng lye that psychrometric ratio is 1:4~8 is obtained, by kuh-seng
Lye grinding, being ground to wherein particle diameter, less than 30 microns, ground kuh-seng lye is extracted, and is obtained particle and is averaged grain
Diameter is less than the kuh-seng lye of 1000nm, and wherein particle of the partial size less than 900nm accounts for 95% or more of all particle total amounts；
6) matrine slurries extracted are placed in cryogenic vacuum concentrator it to be carried out be concentrated into moisture content and are lower than
80%.
Extraction in the step 5) includes supercritical extract, microwave abstracting, ultrasonic extraction, high hydrostatic pressure extraction and nanometer
One of grinding extraction or multiple combinations.
The supercritical extract uses pressure for 25~80MPa, 5~25KW of power, and temperature is≤40 DEG C, and fluid flow is
1000~1500L/h；
For the frequency that microwave abstracting uses for 300~900MHz, power is 5~25KW, and temperature is≤40 DEG C；
For the frequency that ultrasonic extraction uses for 20~50KHz, power is 5~25KW, and temperature is≤40 DEG C；
For the pressure that high hydrostatic pressure extraction uses for 200~300MPa, power is 5~25KW, and temperature is≤40 DEG C, fluid flow
For 1000~1500L/h；
For the nano-milled pressure used that extracts for 50~80MPa, power is 5~25KW, and temperature is≤40 DEG C, fluid flow
For 1000~5000L/h；
6) matrine slurries make its water content lower than 15% by Vacuum Drying Equipment after the middle concentration, consolidate
Body high-purity nano matrine.
The electric current of positive and negative electrode piece described in step 1) is provided by the pulse stimulater through 20M Ω resistance.
CO in step 4)2Supercritical extract, pressure control is in 20~40MPa, and temperature control is at 25~40 DEG C, the time 30
~60min.
The grinding is one such using colloid mill or Cone crusher.
Raw material includes the plant containing matrine such as kuh-seng, Sophora alopecuroide, subprostrate sophora in the step 1).
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, tie below
Specific embodiment is closed, the present invention is further explained.
Embodiment 1:
1) investment fills in the glassware of sodium chloride solution after cleaning the raw material of matrine processed, and pulse stimulater is just
Negative electrode plate is located in the glassware in the sodium chloride solution at both ends, after pulse current stimulating, closes pulse
Stimulator, taking-up raw material carry out cleaning and dry；
2) raw material after drying is crushed, and is mixed after being crushed to 20 mesh with water, and it is former to obtain the primary that psychrometric ratio is 1:0.6
Feed liquid；
3) primary raw materials liquid is ground to wherein particle diameter and less than 100 microns obtains intermediate material liquid；
4) intermediate material liquid is subjected to CO2Then twice by separator separation supercritical extract is spray-dried, be made
Matrine content in matrine original powder is 68%.
Further include that step 5) mixes matrine original powder with water, the kuh-seng lye that psychrometric ratio is 1:4 is obtained, by kuh-seng lye
Grinding, being ground to wherein particle diameter, less than 30 microns, ground kuh-seng lye is extracted, and it is small to obtain average particle size
In the kuh-seng lye of 1000nm, wherein particle of the partial size less than 900nm accounts for 95% or more of all particle total amounts；
6) matrine slurries extracted are placed in cryogenic vacuum concentrator it to be carried out be concentrated into moisture content and are lower than
80%.
Extraction in the step 5) includes supercritical extract.
The supercritical extract uses pressure for 250MPa, power 5KW, and temperature is≤40 DEG C, fluid flow 1000L/
h；
6) matrine slurries make its water content lower than 15% by Vacuum Drying Equipment after the middle concentration, consolidate
Body high-purity nano matrine.
The electric current of positive and negative electrode piece described in step 1) is provided by the pulse stimulater through 20M Ω resistance.
CO in step 4)2Supercritical extract, pressure control is in 20MPa, and temperature control is at 25 DEG C, time 30min.
The grinding is one such using colloid mill.
Raw material includes subprostrate sophora, kuh-seng in the step 1).
Embodiment 2:
1) investment fills in the glassware of sodium chloride solution after cleaning the raw material of matrine processed, and pulse stimulater is just
Negative electrode plate is located in the glassware in the sodium chloride solution at both ends, after pulse current stimulating, closes pulse
Stimulator, taking-up raw material carry out cleaning and dry；
2) raw material after drying is crushed, and is mixed after being crushed to 30 mesh with water, and it is former to obtain the primary that psychrometric ratio is 2:3.5
Feed liquid；
3) primary raw materials liquid is ground to wherein particle diameter and less than 100 microns obtains intermediate material liquid；
4) intermediate material liquid is subjected to CO2Then twice by separator separation supercritical extract is spray-dried, be made
Matrine content in matrine original powder is 72%.
It as a preferred technical solution, further include that step 5) mixes matrine original powder with water, obtaining psychrometric ratio is 1:8's
Kuh-seng lye grinds kuh-seng lye, and being ground to wherein particle diameter, less than 30 microns, ground kuh-seng lye is extracted
It takes, obtains the kuh-seng lye that average particle size is less than 1000nm, wherein particle of the partial size less than 900nm accounts for all particle total amounts
95% or more；
6) matrine slurries extracted are placed in cryogenic vacuum concentrator it to be carried out be concentrated into moisture content and are lower than
80%.
Extraction in the step 5) includes microwave abstracting.
For the frequency that microwave abstracting uses for 900MHz, power is 5~25KW, and temperature is≤40 DEG C；
6) matrine slurries make its water content lower than 15% by Vacuum Drying Equipment after the middle concentration, consolidate
Body high-purity nano matrine.
The electric current of positive and negative electrode piece described in step 1) is provided by the pulse stimulater through 20M Ω resistance.
CO in step 4)2Supercritical extract, pressure control is in 40MPa, and temperature control is at 40 DEG C, time 60min.
The grinding is one such using colloid mill or Cone crusher.
Raw material includes Sophora alopecuroide in the step 1).
Embodiment 3:
1) investment fills in the glassware of sodium chloride solution after cleaning the raw material of matrine processed, and pulse stimulater is just
Negative electrode plate is located in the glassware in the sodium chloride solution at both ends, after pulse current stimulating, closes pulse
Stimulator, taking-up raw material carry out cleaning and dry；
2) raw material after drying is crushed, and is mixed after being crushed to 30 mesh with water, and the primary raw materials that psychrometric ratio is 1:2 is obtained
Liquid；
3) primary raw materials liquid is ground to wherein particle diameter and less than 100 microns obtains intermediate material liquid；
4) intermediate material liquid is subjected to CO2Then twice by separator separation supercritical extract is spray-dried, be made
Matrine content in matrine original powder is 75%.
It as a preferred technical solution, further include that step 5) mixes matrine original powder with water, obtaining psychrometric ratio is 1:5's
Kuh-seng lye grinds kuh-seng lye, and being ground to wherein particle diameter, less than 30 microns, ground kuh-seng lye is extracted
It takes, obtains the kuh-seng lye that average particle size is less than 1000nm, wherein particle of the partial size less than 900nm accounts for all particle total amounts
95% or more；
6) matrine slurries extracted are placed in cryogenic vacuum concentrator it to be carried out be concentrated into moisture content and are lower than
80%.
Extraction in the step 5) includes supercritical extract, microwave abstracting, ultrasonic extraction, high hydrostatic pressure extraction and nanometer
Multiple combinations in grinding extraction.
The supercritical extract uses pressure for 25~80MPa, 5~25KW of power, and temperature is≤40 DEG C, and fluid flow is
200L/h；
For the frequency that microwave abstracting uses for 300~900MHz, power is 5~25KW, and temperature is≤40 DEG C；
For the frequency that ultrasonic extraction uses for 20~50KHz, power is 5~25KW, and temperature is≤40 DEG C；
For the pressure that high hydrostatic pressure extraction uses for 200~300MPa, power is 5~25KW, and temperature is≤40 DEG C, fluid flow
For 1200L/h；
For the nano-milled pressure used that extracts for 50~80MPa, power is 5~25KW, and temperature is≤40 DEG C, fluid flow
For 2000L/h；
6) matrine slurries make its water content lower than 15% by Vacuum Drying Equipment after the middle concentration, consolidate
Body high-purity nano matrine.
The electric current of positive and negative electrode piece described in step 1) is provided by the pulse stimulater through 20M Ω resistance.
CO in step 4)2Supercritical extract, pressure control is in 30MPa, and temperature control is at 28 DEG C, time 50min.
The grinding uses colloid mill.
Raw material includes kuh-seng in the step 1).
The above shows and describes the basic principle, main features and advantages of the invention.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent circle.
Claims (9)
1. a kind of preparation method of matrine, characterized in that it comprises the following steps:
1) investment fills in the glassware of sodium chloride solution after cleaning the raw material of matrine processed, the positive negative electricity of pulse stimulater
Pole piece is located in the glassware in the sodium chloride solution at both ends, after pulse current stimulating, closes impulse stimulation
Device, taking-up raw material carry out cleaning and dry；
2) raw material after drying is crushed, and is mixed after being crushed to 20~30 mesh with water, and obtaining psychrometric ratio is 1~2:0.6~3.5
Primary raw materials liquid；
3) primary raw materials liquid is ground to wherein particle diameter and less than 100 microns obtains intermediate material liquid；
4) intermediate material liquid is subjected to CO2Supercritical extract, then twice by separator separation, it is big that content is made in spray drying
In the 50% matrine original powder less than 75%.
2. a kind of preparation method of matrine as described in claim 1, it is characterised in that: further include that step 5) is former by matrine
Powder is mixed with water, obtains the kuh-seng lye that psychrometric ratio is 1:4~8, kuh-seng lye is ground, wherein particle diameter is ground to and is less than
30 microns, ground kuh-seng lye is extracted, and obtains the kuh-seng lye that average particle size is less than 1000nm, wherein partial size
95% or more of all particle total amounts is accounted for less than the particle of 900nm；
6) matrine slurries extracted are placed in cryogenic vacuum concentrator and carry out being concentrated into moisture content to it lower than 80%.
3. a kind of preparation method of matrine as claimed in claim 2, it is characterised in that: the extraction in the step 5) includes
One of supercritical extract, microwave abstracting, ultrasonic extraction, high hydrostatic pressure extraction and nano-milled extraction or multiple combinations.
4. a kind of preparation method of matrine as claimed in claim 3, it is characterised in that: the supercritical extract uses pressure
For 25~80MPa, 5~25KW of power, temperature is≤40 DEG C, and fluid flow is 1000~1500L/h；
For the frequency that microwave abstracting uses for 300~900MHz, power is 5~25KW, and temperature is≤40 DEG C；
For the frequency that ultrasonic extraction uses for 20~50KHz, power is 5~25KW, and temperature is≤40 DEG C；
For the pressure that high hydrostatic pressure extraction uses for 200~300MPa, power is 5~25KW, and temperature is≤40 DEG C, and fluid flow is
1000~1500L/h；
For the nano-milled pressure used that extracts for 50~80MPa, power is 5~25KW, and temperature is≤40 DEG C, and fluid flow is
1000~5000L/h.
5. a kind of preparation method of matrine as claimed in claim 2, it is characterised in that: 6) matrine is starched after the middle concentration
Liquid makes its water content lower than 15% by Vacuum Drying Equipment, obtains solid high-purity nano matrine.
6. a kind of preparation method of matrine as described in claim 1, it is characterised in that: positive negative electricity described in the step 1)
The electric current of pole piece is provided by the pulse stimulater through 20M Ω resistance.
7. a kind of preparation method of matrine as described in claim 1, it is characterised in that: CO in the step 4)2Overcritical extraction
It takes, pressure control is in 20~40MPa, and at 25~40 DEG C, the time is 30~60min for temperature control.
8. a kind of preparation method of matrine as described in claim 1, it is characterised in that: the grinding uses colloid mill or cone
Body mill is one such.
9. a kind of preparation method of matrine as described in claim 1, it is characterised in that: raw material includes hardship in the step 1)
The plant containing matrine such as ginseng, Sophora alopecuroide, subprostrate sophora.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1687063A (en) * | 2005-04-19 | 2005-10-26 | 黑龙江麦迪欣澳逸医药技术咨询有限公司 | Method for preparing axcnic high pure oxymatrine |
| CN110025659A (en) * | 2019-04-10 | 2019-07-19 | 暨南大学 | A kind of traditional Chinese medicine active site and preparation method and application with Anti-HBV activity effect |
-
2019
- 2019-08-21 CN CN201910773604.2A patent/CN110483517A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1687063A (en) * | 2005-04-19 | 2005-10-26 | 黑龙江麦迪欣澳逸医药技术咨询有限公司 | Method for preparing axcnic high pure oxymatrine |
| CN110025659A (en) * | 2019-04-10 | 2019-07-19 | 暨南大学 | A kind of traditional Chinese medicine active site and preparation method and application with Anti-HBV activity effect |
Non-Patent Citations (1)
| Title |
|---|
| 强利民: "超临界流体萃取苦参碱的研究", 《河北科技大学硕士学位论文》 * |
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