CN114849276A - Scutellaria baicalensis stem element separation and purification device and purification method - Google Patents

Scutellaria baicalensis stem element separation and purification device and purification method Download PDF

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Publication number
CN114849276A
CN114849276A CN202210635667.3A CN202210635667A CN114849276A CN 114849276 A CN114849276 A CN 114849276A CN 202210635667 A CN202210635667 A CN 202210635667A CN 114849276 A CN114849276 A CN 114849276A
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China
Prior art keywords
solution
box
separation
baicalein
ultrasonic generator
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CN202210635667.3A
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田勇
李志平
江建朋
程松硕
刘叶凡
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Hebei Jinyuankang Pharmaceutical Co ltd
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Hebei Jinyuankang Pharmaceutical Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/02Solvent extraction of solids
    • B01D11/0261Solvent extraction of solids comprising vibrating mechanisms, e.g. mechanical, acoustical
    • B01D11/0265Applying ultrasound
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D36/00Filter circuits or combinations of filters with other separating devices

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Acoustics & Sound (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The invention provides a baicalein separation and purification device and a purification method, wherein the device comprises: the scutellaria baicalensis stem and leaf coarse powder is separated and extracted by the ultrasonic generator, and the cavitation effect generated by the ultrasonic generator has special functions of stirring, crushing and the like, so that cavitation bubbles generated in scutellaria baicalensis plant tissues in a solvent can be collapsed instantaneously, cells in the tissues can be broken, the solvent can permeate into the plant cells, and the baicalein components in the tissues can enter an aqueous solvent, and the high-concentration baicalein can be obtained conveniently. The purification method provided by the invention has higher transfer rate and purity of total baicalein in the stem and leaves of the scutellaria baicalensis.

Description

Scutellaria baicalensis stem element separation and purification device and purification method
Technical Field
The invention relates to the technical field of baicalein purification, in particular to a device and a method for separating and purifying baicalein.
Background
The synonym of baicalein: baicalein, extraction source: leaves of Scutellaria baicalensis Georgi (Scutellaria altissima L.) belonging to the family Labiatae; leaves and roots of comfrey s.scorodifolia fisch. (s.galericulata l.); seeds and stem bark of the plant oroxylum indicum (L.) vent of the family bignoniaceae; leaves of plantagaomajorl, plantago major, a plant of plantago. The characteristics are as follows: melting point of yellow needle crystals (from ethanol): solubility at 264-265 ℃: dissolving in methanol, ethanol, acetone, ethyl acetate and hot glacial acetic acid, slightly dissolving in chloroform, dissolving in diluted sodium hydroxide to give green brown color, but is unstable and easily oxidized to green color. The molecular formula is as follows: C15H10O5, molecular weight: 270.24. the pharmacological action is as follows: baicalein has effects of reducing cerebrovascular resistance, improving cerebral blood circulation, increasing cerebral blood flow, and resisting platelet aggregation. The traditional Chinese medicine composition is clinically used for treating paralysis caused by cerebrovascular diseases.
The existing baicalein separating and purifying device needs various instruments and equipment for separation and purification due to the complicated separation process, so that the use is troublesome, the separating and extracting effect is poor, and the purified baicalein is low in concentration.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a baicalein separation and purification device and a purification method.
In order to achieve the purpose of the invention, the invention adopts the technical scheme that:
a baicalein separation and purification device comprises: a support base plate, a support frame is arranged above the support base plate, a rotary evaporator is arranged on one side of the support frame, a mixing box is arranged above the support frame, a motor is arranged outside one side of the mixing box, a rotating shaft is arranged in the middle of the inside of the mixing box, a stirring rod is arranged on the rotating shaft, an ultrasonic generator is arranged on one side above the mixing box, a generating end is arranged in the ultrasonic generator, a separation and extraction box is arranged above the ultrasonic generator, a liquid discharge pipe is arranged below one side of the separation and extraction box, which is far away from the ultrasonic generator, an electromagnetic valve is arranged on the liquid discharge pipe, a filter box is arranged below the electromagnetic valve on the liquid discharge pipe, a filter plate is arranged inside the filter box, the lower end of the liquid discharge pipe is communicated with the top of the mixing box, and a placing frame is arranged above the support base plate, and a centrifugal tube is arranged on the placing frame.
As the improvement, the feed inlet of rotary evaporator with below one side intercommunication of mixing box, the centrifuging tube is located under rotary evaporator's the drain pipe.
As a refinement, the generating end is arranged on the inner walls of two sides of the separation and extraction box.
A method for purifying scutellarin comprises the following steps:
the method comprises the following steps: weighing a scutellaria baicalensis stem and leaf medicinal material, and crushing the scutellaria baicalensis stem and leaf medicinal material into coarse powder;
step two: putting the crushed coarse powder into a separation extraction box, adding an ethanol solution into the separation extraction box, starting an ultrasonic generator, and separating and extracting the mixture;
step three: opening the electromagnetic valve, discharging the solution in the separation and extraction tank through a liquid discharge pipe, then filtering the solution through a filter tank, and enabling the filtered solution to fall into a mixing tank;
step four: the solution in the mixing box enters a rotary evaporator, and the solution is concentrated by the evaporator until the ethanol has no alcohol smell;
step five: adding concentrated hydrochloric acid into the concentrated solution, adjusting the pH value of the concentrated solution, standing for 15 hours, centrifuging by using a centrifuge, and drying the precipitate after centrifugation;
step six: adding distilled water into the dried precipitate, heating in 70 deg.C water bath, adding 10% sodium hydroxide solution to adjust pH, adding ethanol, and standing for 1 hr;
step seven: filtering, washing the precipitate with 45% ethanol, adding concentrated hydrochloric acid into the filtrate to adjust pH, keeping the temperature at 70 deg.C for 1 hr, standing for 10 hr, filtering, and drying the obtained precipitate.
As a modification, the concentration of the ethanol solution added in the second step is 60%.
As a modification, the pH value is adjusted to 1.0 in the fifth step.
As a modification, the pH value is adjusted to be 6.0 in the sixth step.
As a modification, the pH value is adjusted to 1.0 in the seventh step.
The invention has the beneficial effects that:
the scutellaria baicalensis stem and leaf coarse powder is separated and extracted by the ultrasonic generator, and cavitation effect generated by the ultrasonic generator has special functions of stirring, crushing and the like, so that cavitation bubbles generated in scutellaria baicalensis plant tissues in a solvent can be instantaneously collapsed, cells in the tissues can be broken, the solvent can permeate into the plant cells, and the baicalein in the tissues can enter an aqueous solvent, and high-concentration baicalein can be obtained conveniently. The purification method provided by the invention has higher transfer rate and purity of total baicalein in the stem and leaves of the scutellaria baicalensis.
Drawings
FIG. 1 is a schematic structural diagram of a separation and purification apparatus according to the present invention.
Reference numerals comparison table:
1. a support base plate; 2. a rotary evaporator; 3. a mixing box; 4. a motor; 5. a rotating shaft; 6. a stirring rod; 7. an ultrasonic generator; 8. a generating end; 9. separating and extracting the box; 10. a liquid discharge pipe; 11. an electromagnetic valve; 12. a filter box; 13. a filter plate; 14. placing a rack; 15. centrifuging the tube; 16. a support frame.
Detailed Description
In order to make the content of the present invention more clearly understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention. In which like parts are designated by like reference numerals. It should be noted that as used in the following description, the terms "front," "back," "left," "right," "upper" and "lower" refer to directions in the drawings, and the terms "inner" and "outer" refer to directions toward and away from, respectively, the geometric center of a particular component.
As shown in fig. 1, a baicalein separating and purifying device comprises: a support base plate 1, a support frame 16 is arranged above the support base plate 1, a rotary evaporator 2 is arranged on one side of the support frame 16, a mixing box 3 is arranged above the support frame 16, a motor 4 is arranged outside one side of the mixing box 3, a rotating shaft 5 is arranged in the middle of the inside of the mixing box 3, a stirring rod 6 is arranged on the rotating shaft 5, an ultrasonic generator 7 is arranged on one side above the mixing box 3, a generating end 8 is arranged in the ultrasonic generator 7, a separation and extraction box 9 is arranged above the ultrasonic generator 7, a liquid discharge pipe 10 is arranged below one side of the separation and extraction box 9 far away from the ultrasonic generator 7, an electromagnetic valve 11 is arranged on the liquid discharge pipe 10, a filter box 12 is arranged below the electromagnetic valve 11 on the liquid discharge pipe 10, and a filter plate 13 is arranged inside the filter box 12, the lower end of the liquid discharge pipe 10 is communicated with the top of the mixing box 3, a placing frame 14 is arranged above the supporting bottom plate 1, and a centrifugal pipe 15 is arranged on the placing frame 14.
It should be noted that the feed inlet of rotary evaporator 2 is communicated with one side of the lower part of mixing box 3, and centrifugal tube 15 is located under the liquid outlet tube of rotary evaporator 2.
When the device works, the solution in the mixing box 3 enters through the feed inlet of the rotary evaporator 2, the rotary evaporator 2 is started, and the solution entering the rotary evaporator 2 is concentrated.
The generating ends 8 are arranged on the inner walls of the two sides of the separation and extraction box 9, the ultrasonic generator 7 is started, the ultrasonic generator 7 generates ultrasonic waves to the inside of the mixing box 3 through the generating ends 8, the generated waves destroy cells of the scutellaria baicalensis coarse powder, so that baicalein components in tissues enter an aqueous solvent, and high-concentration baicalein is conveniently obtained.
A method for purifying scutellarin comprises the following steps:
the method comprises the following steps: weighing a scutellaria baicalensis stem and leaf medicinal material, and crushing the scutellaria baicalensis stem and leaf medicinal material into coarse powder;
step two: putting the crushed coarse powder into a separation and extraction box 9, adding an ethanol solution into the separation and extraction box 9, starting an ultrasonic generator 7, and separating and extracting the mixture;
step three: opening an electromagnetic valve 11, discharging the solution in the separation and extraction tank 9 through a liquid discharge pipe 10, then filtering the solution through a filter tank 12, and enabling the filtered solution to fall into the mixing tank 3;
step four: the solution in the mixing box 3 enters a rotary evaporator 2, and the solution is concentrated by the rotary evaporator 2 until the ethanol has no alcohol smell;
step five: adding concentrated hydrochloric acid into the concentrated solution, adjusting the pH value of the concentrated solution, standing for 15 hours, centrifuging by using a centrifuge, and drying the precipitate after centrifugation;
step six: adding distilled water into the dried precipitate, heating in 70 deg.C water bath, adding 10% sodium hydroxide solution to adjust pH, adding ethanol, and standing for 1 hr;
step seven: filtering, washing the precipitate with 45% ethanol, adding concentrated hydrochloric acid into the filtrate to adjust pH, keeping the temperature at 70 deg.C for 1 hr, standing for 10 hr, filtering, and drying the obtained precipitate.
Wherein the concentration of the ethanol solution added in the second step is 60%, the pH value is adjusted to 1.0 in the fifth step, the pH value is adjusted to 6.0 in the sixth step, and the pH value is adjusted to 1.0 in the seventh step.
During the operation of the invention, the medicinal material of the stem and leaf of the scutellaria baicalensis is weighed and crushed into coarse powder, the crushed coarse powder is put into a separation and extraction box 9, then 60 percent ethanol solution is added into the separation and extraction box 9, an ultrasonic generator 7 is started to separate and extract the medicinal material, an electromagnetic valve 11 is opened, the solution in the separation and extraction box 9 is discharged through a liquid discharge pipe 10, then the solution is filtered through a filter box 12, the filtered solution falls into a mixing box 3, extraction and separation are carried out for three times, the solution after the extraction for three times is discharged through the liquid discharge pipe 10, then the solution is filtered through the filter box 12, the filtered solution falls into the mixing box 3, then a motor 4 is started to mix the solution, then the mixed solution enters a rotary evaporator 2, the solution is concentrated through the rotary evaporator 2 until the ethanol smell does not exist, adding concentrated hydrochloric acid into the concentrated solution, adjusting the pH value of the concentrated solution to 1.0, standing for 15 hours, centrifuging by a centrifuge, drying the precipitate after centrifugation, adding distilled water into the dried precipitate, heating in a 70-degree water bath, adding 10% sodium hydroxide solution to adjust the pH value to 6.0, adding ethanol, standing for 1 hour, performing suction filtration, washing the precipitate with 45% ethanol, adding concentrated hydrochloric acid into the filtrate to adjust the pH value, keeping the temperature at 70 ℃ for 1 hour, standing for 10 hours, performing suction filtration, and drying the obtained precipitate to obtain the product.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the present invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (8)

1. A baicalein separation and purification device is characterized by comprising: a support base plate (1), a support frame (16) is arranged above the support base plate (1), a rotary evaporator (2) is arranged on one side of the support frame (16), a mixing box (3) is arranged above the support frame (16), a motor (4) is arranged outside one side of the mixing box (3), a rotating shaft (5) is arranged in the middle of the inside of the mixing box (3), a stirring rod (6) is arranged on the rotating shaft (5), an ultrasonic generator (7) is arranged on one side above the mixing box (3), a generating end (8) is arranged in the ultrasonic generator (7), a separation extraction box (9) is arranged above the ultrasonic generator (7), a liquid discharge pipe (10) is arranged below one side, far away from the ultrasonic generator (7), of the separation extraction box (9), and an electromagnetic valve (11) is arranged on the liquid discharge pipe (10), a filter box (12) is arranged below the electromagnetic valve (11) on the liquid discharge pipe (10), a filter plate (13) is arranged inside the filter box (12), the lower end of the liquid discharge pipe (10) is communicated with the top of the mixing box (3), a placing frame (14) is arranged above the supporting bottom plate (1), and a centrifugal tube (15) is arranged on the placing frame (14).
2. The baicalein separating and purifying device according to claim 1, wherein the feed inlet of the rotary evaporator (2) is communicated with one side below the mixing box (3), and the centrifugal tube (15) is positioned right below the liquid outlet tube of the rotary evaporator (2).
3. The baicalein separating and purifying device according to claim 1, wherein the generating end (8) is arranged on the inner wall of both sides of the separating and extracting box (9).
4. A method for purifying baicalein is characterized by comprising the following steps:
the method comprises the following steps: weighing a scutellaria baicalensis stem and leaf medicinal material, and crushing the scutellaria baicalensis stem and leaf medicinal material into coarse powder;
step two: putting the crushed coarse powder into a separation and extraction box, adding an ethanol solution into the separation and extraction box, starting an ultrasonic generator, and separating and extracting the mixture;
step three: opening the electromagnetic valve, discharging the solution in the separation and extraction tank through a liquid discharge pipe, then filtering the solution through a filter tank, and enabling the filtered solution to fall into a mixing tank;
step four: the solution in the mixing box enters a rotary evaporator, and the solution is concentrated by the rotary evaporator until the ethanol has no alcohol smell;
step five: adding concentrated hydrochloric acid into the concentrated solution, adjusting the pH value of the concentrated solution, standing for 15 hours, centrifuging by using a centrifuge, and drying the precipitate after centrifugation;
step six: adding distilled water into the dried precipitate, heating in 70 deg.C water bath, adding 10% sodium hydroxide solution to adjust pH, adding ethanol, and standing for 1 hr;
step seven: filtering, washing the precipitate with 45% ethanol, adding concentrated hydrochloric acid into the filtrate to adjust pH, keeping the temperature at 70 deg.C for 1 hr, standing for 10 hr, filtering, and drying the obtained precipitate.
5. The method for purifying scutellarin according to claim 4, wherein the concentration of the ethanol solution added in the second step is 60%.
6. The method for purifying scutellarin according to claim 4, wherein the pH value is adjusted to 1.0 in the fifth step.
7. The method for purifying scutellarin according to claim 4, wherein the pH value is adjusted to 6.0 in the sixth step.
8. The method for purifying scutellarin according to claim 4, wherein the pH value in the seventh step is adjusted to 1.0.
CN202210635667.3A 2022-06-06 2022-06-06 Scutellaria baicalensis stem element separation and purification device and purification method Pending CN114849276A (en)

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CN202210635667.3A CN114849276A (en) 2022-06-06 2022-06-06 Scutellaria baicalensis stem element separation and purification device and purification method

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6084080A (en) * 1999-01-15 2000-07-04 Farlong International Inc. Breviscapinum and extracting process thereof from erigeron breviscapus
CN206027152U (en) * 2016-08-31 2017-03-22 靖海集团有限公司 Reation kettle is used in fertile production of marine alga
CN107513086A (en) * 2017-09-08 2017-12-26 珠海易嘉贸易有限公司 A kind of method and scutellarin that separating high-purity scutellarin is extracted from Scullcap stem and leaf
CN211273639U (en) * 2019-12-06 2020-08-18 朱显飞 Novel ultrasonic extraction device for traditional Chinese medicine
CN113896754A (en) * 2021-11-29 2022-01-07 郑州大学 Industrial production method for extracting and purifying baicalin from scutellaria baicalensis

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6084080A (en) * 1999-01-15 2000-07-04 Farlong International Inc. Breviscapinum and extracting process thereof from erigeron breviscapus
CN206027152U (en) * 2016-08-31 2017-03-22 靖海集团有限公司 Reation kettle is used in fertile production of marine alga
CN107513086A (en) * 2017-09-08 2017-12-26 珠海易嘉贸易有限公司 A kind of method and scutellarin that separating high-purity scutellarin is extracted from Scullcap stem and leaf
CN211273639U (en) * 2019-12-06 2020-08-18 朱显飞 Novel ultrasonic extraction device for traditional Chinese medicine
CN113896754A (en) * 2021-11-29 2022-01-07 郑州大学 Industrial production method for extracting and purifying baicalin from scutellaria baicalensis

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