CN108939613B - Eucommia ulmoides extract efficient extraction device and method for preventing and treating cardiovascular diseases - Google Patents

Eucommia ulmoides extract efficient extraction device and method for preventing and treating cardiovascular diseases Download PDF

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CN108939613B
CN108939613B CN201810793933.9A CN201810793933A CN108939613B CN 108939613 B CN108939613 B CN 108939613B CN 201810793933 A CN201810793933 A CN 201810793933A CN 108939613 B CN108939613 B CN 108939613B
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pipeline
extraction
eucommia ulmoides
valve
extract
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CN108939613A (en
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庞军
杨永耀
龙向淑
刘承铭
杨龙
蒋智
况春燕
田野
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Guizhou Provincial Peoples Hospital
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Guizhou Provincial Peoples Hospital
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/04Solvent extraction of solutions which are liquid
    • B01D11/0419Solvent extraction of solutions which are liquid in combination with an electric or magnetic field or with vibrations
    • B01D11/0423Applying ultrasound
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/04Solvent extraction of solutions which are liquid
    • B01D11/0488Flow sheets
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D15/00Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08Selective adsorption, e.g. chromatography
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D15/00Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08Selective adsorption, e.g. chromatography
    • B01D15/26Selective adsorption, e.g. chromatography characterised by the separation mechanism
    • B01D15/38Selective adsorption, e.g. chromatography characterised by the separation mechanism involving specific interaction not covered by one or more of groups B01D15/265 - B01D15/36
    • B01D15/3852Selective adsorption, e.g. chromatography characterised by the separation mechanism involving specific interaction not covered by one or more of groups B01D15/265 - B01D15/36 using imprinted phases or molecular recognition; using imprinted phases

Abstract

The invention discloses a eucommia ulmoides extract efficient extraction device and method for preventing and treating cardiovascular diseases, wherein the device mainly comprises a shell rotary cleaning juicing device, a primary ultrasonic extraction device, a filtering device, a solvent recovery device, a secondary solid-phase extraction device, a PLC (programmable logic controller) and a power supply, wherein the rotary cleaning juicing device, the primary ultrasonic extraction device, the filtering device, the solvent recovery device, the secondary solid-phase extraction device, the PLC and the power supply are all positioned in the shell, the rotary cleaning juicing device, the primary ultrasonic extraction device, the filtering device, the solvent recovery device and the secondary solid-phase extraction device are sequentially connected through pipelines, and the PLC is connected with an ultrasonic generator, valves and switch elements. The method can quickly and efficiently extract the eucommia ulmoides extract, the obtained eucommia ulmoides extract has higher purity, can realize automatic operation through PLC, is suitable for industrial mass production, and has better market popularization prospect.

Description

Eucommia ulmoides extract efficient extraction device and method for preventing and treating cardiovascular diseases
Technical Field
The invention relates to the technical field of medicine extraction and preparation, in particular to an efficient eucommia ulmoides extract extraction device and method for preventing and treating cardiovascular diseases.
Background
Coronary atherosclerosis causes stenosis or obstruction of the lumen, or/and coronary spasm, resulting in myocardial ischemia, hypoxia or necrosis, resulting in heart disease, collectively known as atherosclerotic heart disease, with hypertension and coronary heart disease being the most prevalent and frequently occurring cardiovascular disease. According to the latest data of 'Chinese cardiovascular disease report': it is currently estimated that 2.9 million patients with cardiovascular disease are present throughout the country, and 1 in 5 adults suffers from cardiovascular disease. Cardiovascular diseases become the first cause of death in China, and the proportion is more than 40%. Coronary atherosclerosis is a central pathogenesis of hypertension and coronary heart disease. The Ubiquitin-proteasome pathway (UPP) is widely involved in various physiological processes such as cell cycle regulation, DNA repair, and cell signal transduction, and can promote the process of atherosclerosis by inflammatory factors of Ubiquitin-proteasome system, so that it is the leading direction of the current research on atherosclerosis mechanism.
Eucommia ulmoides (Eucomia ulmoides) is a Chinese medicinal material with more than 2000 years of history, and has the effects of tonifying liver and kidney, strengthening bones and muscles, preventing miscarriage and the like; meanwhile, the eucommia bark has special effect on treating hypertension. Chlorogenic acid and flavonoid compounds are main effective components of folium Eucommiae, and have remarkable physiological activity. The eucommia ulmoides as a precious state medicinal material is dried bark of eucommia ulmoides of family eucommia, and contains active ingredients with pharmacological effects of reducing blood pressure, reducing blood fat, resisting thrombus, oxidation and atherosclerosis, protecting cardiac muscle and the like, and the active ingredients have wide cardiovascular effects. A large number of reports prove that the eucommia ulmoides extract has stronger pharmacological activity, and the active ingredients of the eucommia ulmoides extract can inhibit the vascular inflammatory reaction and delay the atherosclerosis process.
The existing eucommia ulmoides extract has high extraction cost, high requirements on equipment during recovery and certain limitations. And some processes are complex to operate, the emulsification phenomenon is easy to occur in the extraction process, the time consumption is long, and the industrialization is not easy to realize. With the increasing demand of eucommia ulmoides extracts in the market, the research on how to simply, conveniently and quickly extract eucommia ulmoides extracts from eucommia ulmoides raw materials, which have stable quality, high purity, high yield, safety and reliability, is necessary.
Disclosure of Invention
The invention solves the technical problems that the existing eucommia ulmoides extraction method and equipment are not advanced enough, and the extraction efficiency and purity are not high enough, and further provides an eucommia ulmoides extract high-efficiency extraction device and method for preventing and treating cardiovascular diseases.
The technical scheme of the invention is as follows: the eucommia ulmoides extract efficient extraction device for preventing and treating cardiovascular diseases mainly comprises a shell rotating, cleaning and juicing device, a primary ultrasonic extraction device, a filtering device, a solvent recovery device, a secondary solid-phase extraction device, a PLC (programmable logic controller) and a power supply, wherein the rotating, cleaning and juicing device, the primary ultrasonic extraction device, the filtering device, the solvent recovery device, the secondary solid-phase extraction device, the PLC and the power supply are all positioned inside the shell, and the shell is cuboid; the rotary cleaning juicing device mainly comprises a machine body and a base, wherein a rotary motor and a stirring motor are arranged in the base, a stirring head is arranged in the machine body, the rotary motor drives the machine body to rotate, and the stirring motor drives the stirring head to perform stirring action; a cleaning liquid storage device is arranged above the machine body and is communicated with the top of the machine body through a first pipeline, a first valve is arranged on the first pipeline, an eucommia ulmoides raw material channel is arranged on the side face of the machine body, one end of the eucommia ulmoides raw material channel is connected with the machine body, the other end of the eucommia ulmoides raw material channel is communicated with the outside of the shell, a cleaning liquid discharge port is also arranged at the lower part of the machine body, and a filter screen is arranged on the cleaning liquid discharge; the primary ultrasonic extraction device mainly comprises a main body, a first driving motor, a second driving motor, an ultrasonic generator, an extraction tube, a first rotating disk, a second rotating disk, a third rotating disk, a first driving shaft, a second driving shaft and an ultrasonic probe, wherein the first driving motor, the second driving motor and the ultrasonic generator are respectively positioned on the upper surface of the main body close to the rear side, the first driving shaft is connected to the first driving motor, the third rotating disk is positioned in the middle of the top surface of the main body and penetrates through the top surface of the main body, the third rotating disk is driven by the first driving shaft, the ultrasonic probes are multiple in number and are uniformly distributed on the bottom surface of the third rotating disk in a circular shape, the second driving shaft is connected to the second driving motor, the second driving shaft penetrates through the left side surface of the main body, and the right end of the second driving shaft is connected to the left end, the inner parts of the first rotating disc and the second rotating disc are both hollow, the second rotating disc is positioned on the right side of the first rotating disc, the axes of the first rotating disc and the second rotating disc are on the same straight line, the plurality of extraction tubes are circumferentially distributed between the first rotating disc and the second rotating disc and are communicated with the inner parts of the first rotating disc and the second rotating disc, the liquid outlet of the rotary cleaning juicing device is connected to the first rotating disc through a second pipeline, a second valve is arranged on the second pipeline, an extraction solvent storage device is arranged above the primary ultrasonic extraction device and is connected to the first rotating disc through a third pipeline, and a third valve is arranged on the third pipeline; the second rotating disc is connected to the filtering device through a fourth pipeline, and a fourth valve is arranged on the fourth pipeline; the filtering device is connected to the solvent recovery device through a pipeline five, a valve five is arranged on the pipeline five, the solvent recovery device is connected to the secondary solid-phase extraction device through a pipeline six, and a valve six is arranged on the pipeline six; be equipped with ethanol storage device in secondary solid phase extraction device's top, ethanol storage device is connected to secondary solid phase extraction device through pipeline seven be equipped with valve seven on the pipeline seven, be connected with the collecting vat through pipeline eight in secondary solid phase extraction device's bottom, the power does rotating electrical machines, agitator motor, first driving motor and second driving motor power supply all be equipped with the switching element on rotating electrical machines, agitator motor, first driving motor and the second driving motor, the PLC controller with supersonic generator, each valve and each switching element connect, the interconnecting link is not shown in the figure.
Further, in the above scheme, two inlets are provided on the left end face of the first rotating disk, which are an extraction solvent inlet and an inlet for the extract to be extracted, respectively, the third pipeline is connected to the extraction solvent inlet, an electric telescopic sleeve is provided at the joint of the third pipeline and the extraction solvent inlet, the second pipeline is connected to the inlet for the extract to be extracted, an electric telescopic sleeve is also provided at the joint of the second pipeline and the inlet for the extract to be extracted, an extract outlet is provided on the right side face of the second rotating disk, the extract outlet is connected to the fourth pipeline, an electric telescopic sleeve is also provided at the joint of the extract outlet and the fourth pipeline, and each electric telescopic sleeve is connected to the PLC controller. Cover plates are arranged on the extraction solvent inlet, the extract inlet to be extracted and the extract outlet, when the electric telescopic sleeve is opened and extended, each pipeline port is tightly attached to the corresponding extraction solvent inlet, the extract inlet to be extracted and the extract outlet, each cover plate is pushed into the rotary table, each pipeline is correspondingly communicated with each rotary table, when the electric telescopic sleeve is shortened, each pipeline port is disconnected from the corresponding extraction solvent inlet, the extract inlet to be extracted and the extract outlet, each cover plate is automatically popped up to seal the corresponding extraction solvent inlet, the extract inlet to be extracted and the extract outlet, and each pipeline is correspondingly disconnected from each rotary table.
Further, in the above scheme, a visual window is further arranged on the side wall of the machine body, the visual window is circular and made of transparent materials, and the cleaning or crushing state of the interior can be observed.
Further, in the above scheme, the cleaning solution storage devices are three in total and respectively store clean water, 0.3-0.5% NaCl solution and 0.3-0.6% NaHCO3The solutions are respectively provided with independent valves, and the cleaning solution can be selected or matched according to the cleaning requirement.
Further, in the above scheme, the number of the extraction solvent storage devices is four, the extraction solvent storage devices respectively store petroleum ether, ethyl acetate, water and lower alcohol, and the extraction solvent storage devices are respectively provided with an independent valve, so that the extraction solvent can be selected or matched according to the extraction requirement.
Further, in the above scheme, the ethanol storage device stores therein an eluent, and the eluent is 75-82% methanol.
Further, in the above scheme, the packing in the secondary solid phase extraction device is: chlorogenic acid molecularly imprinted polymer microspheres, magnetic nanoparticles and zeolite particles, wherein the mass ratio of the chlorogenic acid molecularly imprinted polymer microspheres to the magnetic nanoparticles to the zeolite particles is 1-4: 5: 12-20.
Furthermore, the preparation method of the secondary solid phase extraction device comprises the following steps:
(1) weighing the filler: weighing filler chlorogenic acid molecularly imprinted polymer microspheres, magnetic nanoparticles and zeolite particles;
(2) filling: uniformly mixing chlorogenic acid molecular imprinting polymer microspheres, magnetic nanoparticles and zeolite particles, loading into a hopper of a semi-automatic solid phase extraction assembly instrument, starting the instrument, adjusting the system pressure to be 0.5MPa, controlling the column filling amount to be 0.25g by a precision balance, and then filling a lower sieve plate, filling a filler, vibrating the filler and filling an upper sieve plate.
Further, in the above scheme, the preparation method of the chlorogenic acid molecularly imprinted polymer microspheres comprises:
dissolving chlorogenic acid and methacrylic acid in a mixed solution of acetonitrile and 4-vinylaniline according to a molar ratio of 1:2-1:5, oscillating at room temperature for 8 hours, adding a crosslinking agent TRIM (1, 1, 1-tris (hydroxymethyl propane trimethacrylate) with the amount of 4.5 times of methacrylic acid to obtain a mixture, ultrasonically degassing, introducing nitrogen into the mixture to remove oxygen, sealing, polymerizing in a constant-temperature water bath at 50-60 ℃ for 20 hours, grinding and sieving the obtained polymer, settling for 1-3 times by using an acetic acid methanol solution with the volume fraction of 30-48%, eluting for 1-3 times by using tetrahydrofuran, filtering, and vacuum drying to constant weight to obtain the product.
The invention also provides a method for efficiently extracting the eucommia ulmoides extract by using the eucommia ulmoides extract efficient extraction device for preventing and treating cardiovascular diseases, which comprises the following steps of:
s1, cleaning: turning on a power supply, feeding fresh eucommia ulmoides raw materials into the rotary cleaning and juicing device from the eucommia ulmoides raw material channel, controlling the opening of a valve through a PLC (programmable logic controller), introducing cleaning liquid in a cleaning liquid storage device into the rotary cleaning and juicing device through a pipeline I, wherein the introduction amount of the cleaning liquid is 2/3-4/5 of the volume of a machine body, and introducing clean water, or 0.3-0.5% NaCl solution, or 0.3-0.6% NaHCO3The solution or any two or three of the solutions are mixed according to any proportion, then the PLC controller controls the switch element of the rotating motor to start the rotating motor to drive the machine body to rotate, the eucommia ulmoides raw material is cleaned, after the cleaning is finished, the cleaning solution is discharged from the cleaning solution discharge port, the cleaning is repeated for 2-4 times, and after the cleaning is finished for the last time, the cleaning solution is discharged from the cleaning solution discharge portClear water is injected into the machine body, and the amount of the clear water is 3-5 times of the mass of the eucommia ulmoides raw material;
s2, juicing: the PLC is used for controlling a switching element of the rotating motor to be closed and controlling a switching element of the stirring motor to be opened at the same time, the stirring motor is started to drive the stirring head to work, the cleaned eucommia ulmoides raw materials are squeezed into juice, and the eucommia ulmoides raw juice is obtained and discharged from a liquid outlet;
s3, primary extraction: controlling the opening of the second valve through a PLC (programmable logic controller), simultaneously controlling each electric telescopic sleeve to tightly joint the second pipeline with the inlet of the extract to be extracted, tightly joint the third pipeline with the inlet of the extraction solvent, disconnecting the fourth pipeline from the extraction liquid outlet, allowing the eucommia ulmoides normal juice to enter a first rotating disc in the primary ultrasonic extraction device through the second pipeline and the inlet of the extract to be extracted, continuously controlling the third valve on the third pipeline to be opened, and introducing the extraction solvent in the extraction solvent storage device into the first rotating disc through the third pipeline and the inlet of the extraction solvent; after the eucommia ulmoides normal juice and the extraction solvent are filled in the extraction pipe, the control valve II and the valve III are closed, the electric telescopic sleeves on the control pipeline II and the control pipeline III are disconnected with the inlet of the extract to be extracted and the inlet of the extraction solvent, the ultrasonic generator, the first driving motor and the second driving motor are continuously controlled to start to work, the first driving motor drives the third rotating disc to rotate through the driving shaft I, the second driving motor drives the first rotating disc to rotate through the driving shaft II, the first rotating disc simultaneously drives the extraction pipe and the second rotating disc to rotate together, and ultrasonic waves generated by the ultrasonic generator are emitted through the ultrasonic probe to perform ultrasonic extraction on the eucommia ulmoides normal juice in the extraction pipe; after extracting for a certain time, controlling the switching elements of the first driving motor and the second driving motor to be closed, and simultaneously closing the ultrasonic generator to finish primary extraction;
s4, filtering: the PLC controls an electric telescopic sleeve on the pipeline IV to tightly connect the pipeline IV with the extraction liquid outlet, and simultaneously opens a valve on the pipeline IV to introduce the extracted mixed liquid into a filtering device for filtering;
s5, solvent recovery: opening a valve V on the pipeline V under the control of a PLC (programmable logic controller), and enabling the filtered mixed solution to enter a solvent recovery device to recover the extraction solvent;
s6, secondary extraction: opening a valve six on a pipeline six through a PLC controller, introducing the mixed liquid with the recovered extraction solvent into a secondary solid-phase extraction device, and performing secondary adsorption extraction on the mixed liquid with the recovered extraction solvent through a filler in the secondary solid-phase extraction device;
s7, elution: controlling a valve seventh on the pipeline seventh to be opened through a PLC controller, introducing the ethanol in the ethanol storage device into a secondary solid phase extraction device for elution to obtain an eluent, and introducing the eluent into a collecting tank through a pipeline eighth for collection;
s8, drying: concentrating and drying the collected eluent to obtain the eucommia ulmoides extract.
The invention has the beneficial effects that: the eucommia ulmoides extract efficient extraction device for preventing and treating cardiovascular diseases is designed by integrating rotary cleaning, juicing, primary extraction, solvent recovery by filtration, secondary extraction and elution, can quickly and efficiently extract eucommia ulmoides extract, and the eucommia ulmoides extract obtained by the extraction method is higher in purity and better in quality through two extraction procedures of ultrasonic extraction and solid-phase extraction. In addition, the invention can realize automatic operation through PLC, solves the problems of complex operation procedures and troublesome operation in the prior art, has high intelligent degree, is suitable for industrialized mass production, and has better market popularization prospect.
Drawings
FIG. 1 is a schematic view of the overall structure of the present invention;
FIG. 2 is a partially enlarged schematic view of a primary ultrasonic extraction apparatus;
FIG. 3 is a left side schematic view of the first carousel;
FIG. 4 is a right side schematic view of the first carousel;
wherein, 1-shell, 2-rotary cleaning and juicing device, 21-machine body, 22-base, 23-eucommia bark raw material channel, 24-second pipeline, 25-second valve, 26-cleaning liquid outlet, 27-filter screen, 28-visible window, 29-liquid outlet, 3-first ultrasonic extraction device, 31-main body, 32-first driving motor, 33-second driving motor, 34-ultrasonic generator, 35-extraction tube, 36-first rotating disk, 37-second rotating disk, 38-third rotating disk, 39-first driving shaft, 310-second driving shaft, 311-ultrasonic probe, 312-fourth pipeline, 313-fourth valve, 314-extraction solvent inlet, 315-extract inlet, 316-electric telescopic sleeve, 317-extraction liquid outlet, 4-filtering device, 41-pipeline five, 42-valve five, 5-solvent recovery device, 51-pipeline six, 52-valve six, 6-secondary solid phase extraction device, 61-pipeline eight, 62-collecting tank, 7-PLC controller, 8-power supply, 9-cleaning liquid storage device, 91-pipeline one, 92-valve one, 10-extraction solvent storage device, 101-pipeline three, 102-valve three, 11-ethanol storage device, 111-pipeline seven and 112-valve seven.
Detailed Description
Example 1:
a high-efficient extraction element of cortex Eucommiae extract for cardiovascular disease prevention and cure, mainly include the body 1 rotates and washes the extractor 2, the ultrasonic extractor 3 of the first time, filter equipment 4, solvent recovery unit 5, the solid phase extractor 6 of the second time, PLC controller 7 and power 8, rotate and wash the extractor 2, the ultrasonic extractor 3 of the first time, filter equipment 4, solvent recovery unit 5, the solid phase extractor 6 of the second time, PLC controller 7 and power 8 and locate in body 1, body 1 is cuboid; the rotary cleaning juicing device 2 mainly comprises a machine body 21 and a base 22, wherein a rotary motor and a stirring motor are arranged in the base 22, a stirring head is arranged in the machine body 21, the rotary motor drives the machine body 21 to rotate, and the stirring motor drives the stirring head to stir; a cleaning liquid storage device 9 is arranged above the machine body 21, the cleaning liquid storage device 9 is communicated with the top of the machine body 21 through a first pipeline 91, a first valve 92 is arranged on the first pipeline 91, an eucommia ulmoides raw material channel 23 is arranged on the side surface of the machine body 21, one end of the eucommia ulmoides raw material channel 23 is connected with the machine body 21, the other end of the eucommia ulmoides raw material channel 23 leads to the outside of the shell 1, a cleaning liquid outlet 26 is also arranged at the lower part of the machine body 21, and a filter screen; the primary ultrasonic extraction device 3 mainly comprises a main body 31, a first drive motor 32, a second drive motor 33, an ultrasonic generator 34, an extraction tube 35, a first rotary disk 36, a second rotary disk 37, a third rotary disk 38, a first drive shaft 39, a second drive shaft 310 and an ultrasonic probe 311, wherein the first drive motor 32, the second drive motor 33 and the ultrasonic generator 34 are respectively positioned at the upper surface of the main body 31 and at the rear side position, the first drive shaft 39 is connected to the first drive motor 32, the third rotary disk 38 is positioned at the middle position of the top surface of the main body 31 and penetrates through the top surface of the main body 31, the third rotary disk 38 is driven by the first drive shaft 39, the ultrasonic probes 311 are a plurality of probes which are uniformly distributed on the bottom surface of the third rotary disk 38 in a circular shape, the second drive shaft 310 is connected to the second drive motor 33, the second drive shaft 310 penetrates through the left side surface of the main body 31, the right end, the interiors of the first rotating disc 36 and the second rotating disc 37 are both hollow, the second rotating disc 37 is positioned on the right side of the first rotating disc 36, the axes of the first rotating disc 36 and the second rotating disc 37 are on the same straight line, the plurality of extraction pipes 35 are arranged, are circumferentially distributed between the first rotating disc 36 and the second rotating disc 37 and are communicated with the interiors of the first rotating disc 36 and the second rotating disc 37, the liquid outlet 29 of the rotary cleaning and juicing device 2 is connected to the first rotating disc 36 through a second pipeline 24, a second valve 25 is arranged on the second pipeline 24, an extraction solvent storage device 10 is arranged above the primary ultrasonic extraction device 3, the extraction solvent storage device 10 is connected to the first rotating disc 36 through a third pipeline 101, and a third valve 102 is arranged on the third pipeline 101; the second rotating disc 37 is connected to the filtering device 4 through a fourth pipe 312, and a fourth valve 313 is arranged on the fourth pipe 312; the filtering device 4 is connected to the solvent recovery device 5 through a pipeline five 41, a valve five 42 is arranged on the pipeline five 41, the solvent recovery device 5 is connected to the secondary solid-phase extraction device 6 through a pipeline six 51, and a valve six 52 is arranged on the pipeline six 51; an ethanol storage device 11 is arranged above the secondary solid-phase extraction device 6, the ethanol storage device 11 is connected to the secondary solid-phase extraction device 6 through a pipeline seven 111, a valve seven 112 is arranged on the pipeline seven 111, a collecting tank 62 is connected to the bottom of the secondary solid-phase extraction device 6 through a pipeline eight 61, a power supply 8 supplies power to a rotating motor, a stirring motor, a first driving motor 32 and a second driving motor 33, switch elements are arranged on the rotating motor, the stirring motor, the first driving motor 32 and the second driving motor 33, and the PLC 7 is connected with the ultrasonic generator 34, the valves and the switch elements.
Two inlets, namely an extraction solvent inlet 314 and an extract inlet 315, are arranged on the left end face of the first rotating disc 36, the third pipeline 101 is connected with the extraction solvent inlet 314, an electric telescopic sleeve 316 is arranged at the joint of the third pipeline 101 and the extraction solvent inlet 314, the second pipeline 24 is connected with the extract inlet 315, an electric telescopic sleeve 316 is also arranged at the joint of the second pipeline 24 and the extract inlet 315, an extraction liquid outlet 317 is arranged on the right side face of the second rotating disc 37, the extraction liquid outlet 317 is connected with the fourth pipeline 312, an electric telescopic sleeve 316 is also arranged at the joint of the extraction liquid outlet 317 and the fourth pipeline 312, and each electric telescopic sleeve 316 is connected to the PLC 7. Cover plates are arranged on the extraction solvent inlet 314, the to-be-extracted substance inlet 315 and the extraction liquid outlet 317, when the electric telescopic sleeve 316 is opened and extended, the pipeline ports are tightly attached to the corresponding extraction solvent inlet 314, the to-be-extracted substance inlet 315 and the extraction liquid outlet 317, the cover plates are pushed into the turntables to correspondingly connect the pipelines with the turntables, when the electric telescopic sleeve 316 is shortened, the pipeline ports are disconnected from the corresponding extraction solvent inlet 314, the to-be-extracted substance inlet 315 and the extraction liquid outlet 317, and the cover plates are automatically ejected to seal the corresponding extraction solvent inlet 314, the to-be-extracted substance inlet 315 and the extraction liquid outlet 317, so that the pipelines are correspondingly disconnected with the turntables.
A visual window 28 is further provided on the sidewall of the body 21, and the visual window 28 is circular and made of a transparent material so that the inside cleaning or pulverizing state can be observed.
Wherein, the cleaning solution storage devices 9 are three in total and respectively store clean water, 0.3 percent NaCl solution and 0.3 percent NaHCO3The solutions are respectively provided with independent valves, and the cleaning solution can be selected or matched according to the cleaning requirement.
The total number of the extraction solvent storage devices 10 is four, petroleum ether, ethyl acetate, water and lower alcohol are respectively stored in the extraction solvent storage devices, and the extraction solvent storage devices are respectively provided with independent valves, so that the extraction solvent can be selected or matched at will according to extraction requirements.
The ethanol storage device 11 stores an eluent which is 75% methanol.
The filler in the secondary solid phase extraction device 6 is: chlorogenic acid molecular imprinting polymer microspheres, magnetic nanoparticles and zeolite particles, wherein the mass ratio of the chlorogenic acid molecular imprinting polymer microspheres, the magnetic nanoparticles and the zeolite particles is 1: 5: 12.
The preparation method of the secondary solid phase extraction device 6 comprises the following steps:
(3) weighing the filler: weighing filler chlorogenic acid molecularly imprinted polymer microspheres, magnetic nanoparticles and zeolite particles;
(4) filling: uniformly mixing chlorogenic acid molecular imprinting polymer microspheres, magnetic nanoparticles and zeolite particles, loading into a hopper of a semi-automatic solid phase extraction assembly instrument, starting the instrument, adjusting the system pressure to be 0.5MPa, controlling the column filling amount to be 0.25g by a precision balance, and then filling a lower sieve plate, filling a filler, vibrating the filler and filling an upper sieve plate.
The preparation method of the chlorogenic acid molecular imprinting polymer microspheres comprises the following steps:
dissolving chlorogenic acid and methacrylic acid in a molar ratio of 1:2 in a mixed solution of acetonitrile and 4-vinylaniline, wherein the molar ratio of acetonitrile to 4-vinylaniline is 2:7, oscillating for 8 hours at room temperature, adding a crosslinking agent TRIM (1, 1, 1-tris (hydroxymethyl propane trimethacrylate) with the amount of 4.5 times of methacrylic acid to obtain a mixture, ultrasonically degassing, introducing nitrogen into the mixture to remove oxygen, sealing, polymerizing for 20 hours in a constant-temperature water bath at 50 ℃, grinding and sieving the obtained polymer, settling for 1 time by using an acetic acid methanol solution with the volume fraction of 30%, eluting for 1 time by using tetrahydrofuran, filtering, and vacuum drying to constant weight to obtain the chlorogenic acid/methacrylic acid copolymer.
The method for efficiently extracting the eucommia ulmoides extract by using the device comprises the following steps:
s1, cleaning: turning on a power supply 8, feeding fresh eucommia ulmoides raw materials into the rotary cleaning and juicing device 2 from the eucommia ulmoides raw material channel 23, controlling a first valve 92 to be opened through a PLC (programmable logic controller) 7, introducing cleaning liquid in a cleaning liquid storage device 9 into the rotary cleaning and juicing device 2 through a first pipeline 91, wherein the introduction amount of the cleaning liquid is 2/3 of the volume of the machine body 21, introducing clean water, controlling a switching element of a rotary motor through the PLC 7, starting the rotary motor to drive the machine body 21 to rotate, cleaning the eucommia ulmoides raw materials, discharging the cleaning liquid from a cleaning liquid discharge port 26 after cleaning is completed, repeatedly cleaning for 2 times, and injecting clean water into the machine body after the last cleaning, wherein the amount of the clean water is 3 times of the mass of the eucommia ulmoides raw materials;
s2, juicing: the PLC controller 7 controls the switch element of the rotating motor to be closed, and simultaneously controls the switch element of the stirring motor to be opened, the stirring motor is started to drive the stirring head to work, the cleaned eucommia ulmoides raw material is squeezed into juice, and the eucommia ulmoides raw juice is discharged from a liquid outlet 29;
s3, primary extraction: controlling the opening of the second valve 25 through the PLC 7, controlling the electric telescopic sleeves 316 to tightly connect the second pipeline 24 with the inlet 315 of the extract to be extracted, tightly connecting the third pipeline 101 with the inlet 314 of the extraction solvent, disconnecting the fourth pipeline 312 with the outlet 317 of the extraction liquid, allowing the eucommia ulmoides juice to enter the first rotating disc 36 in the primary ultrasonic extraction device 3 through the second pipeline 24 and the inlet 315 of the extract to be extracted, continuously controlling the third valve 102 on the third pipeline 101 to be opened, and introducing the extraction solvent in the extraction solvent storage device 10 into the first rotating disc 36 through the third pipeline 101 and the inlet 314 of the extraction solvent; after the extraction tube 35 is filled with the eucommia ulmoides normal juice and the extraction solvent, the control valve II 25 and the valve III 102 are closed, the electric telescopic sleeves 316 on the control tube II 24 and the control tube III 101 are disconnected with the inlet 315 of the extract to be extracted and the inlet 314 of the extraction solvent, the ultrasonic generator 34, the first driving motor 32 and the second driving motor 33 are continuously controlled to start working, the first driving motor 32 drives the third rotating disc 38 to rotate through the first driving shaft 39, the second driving motor 33 drives the first rotating disc 36 to rotate through the second driving shaft 310, the first rotating disc simultaneously drives the extraction tube 35 and the second rotating disc 37 to rotate together, the ultrasonic wave generated by the ultrasonic generator 34 is emitted through the ultrasonic probe 311, and the eucommia ulmoides normal juice in the extraction tube 35 is subjected to ultrasonic extraction; after extracting for a certain time, controlling the switch elements of the first driving motor 32 and the second driving motor 33 to be closed, and simultaneously closing the ultrasonic generator 34 to finish primary extraction;
s4, filtering: the PLC 7 controls an electric telescopic sleeve 316 on the fourth pipeline 312 to tightly connect the fourth pipeline 312 with an extraction liquid outlet 317, and simultaneously opens a valve 313 on the fourth pipeline 312 to introduce the extracted mixed liquid into the filtering device 4 for filtering;
s5, solvent recovery: opening a valve five 42 on a pipeline five 41 under the control of a PLC 7, so that the filtered mixed solution enters a solvent recovery device 5 to recover the extraction solvent;
s6, secondary extraction: opening a valve six 52 on a pipeline six 51 under the control of the PLC 7, introducing the mixed solution with the recovered extraction solvent into a secondary solid-phase extraction device 6, and performing secondary adsorption extraction on the mixed solution with the recovered extraction solvent by using a filler in the secondary solid-phase extraction device 6;
s7, elution: controlling a valve seven 112 on a pipeline seven 111 to be opened through the PLC 7, introducing the ethanol in the ethanol storage device 11 into the secondary solid phase extraction device 6 for elution to obtain an eluent, and introducing the eluent into a collecting tank 62 through a pipeline eight 61 for collection;
s8, drying: concentrating and drying the collected eluent to obtain the eucommia ulmoides extract.
Example 2:
a high-efficient extraction element of cortex Eucommiae extract for cardiovascular disease prevention and cure, mainly include the body 1 rotates and washes the extractor 2, the ultrasonic extractor 3 of the first time, filter equipment 4, solvent recovery unit 5, the solid phase extractor 6 of the second time, PLC controller 7 and power 8, rotate and wash the extractor 2, the ultrasonic extractor 3 of the first time, filter equipment 4, solvent recovery unit 5, the solid phase extractor 6 of the second time, PLC controller 7 and power 8 and locate in body 1, body 1 is cuboid; the rotary cleaning juicing device 2 mainly comprises a machine body 21 and a base 22, wherein a rotary motor and a stirring motor are arranged in the base 22, a stirring head is arranged in the machine body 21, the rotary motor drives the machine body 21 to rotate, and the stirring motor drives the stirring head to stir; a cleaning liquid storage device 9 is arranged above the machine body 21, the cleaning liquid storage device 9 is communicated with the top of the machine body 21 through a first pipeline 91, a first valve 92 is arranged on the first pipeline 91, an eucommia ulmoides raw material channel 23 is arranged on the side surface of the machine body 21, one end of the eucommia ulmoides raw material channel 23 is connected with the machine body 21, the other end of the eucommia ulmoides raw material channel 23 leads to the outside of the shell 1, a cleaning liquid outlet 26 is also arranged at the lower part of the machine body 21, and a filter screen; the primary ultrasonic extraction device 3 mainly comprises a main body 31, a first drive motor 32, a second drive motor 33, an ultrasonic generator 34, an extraction tube 35, a first rotary disk 36, a second rotary disk 37, a third rotary disk 38, a first drive shaft 39, a second drive shaft 310 and an ultrasonic probe 311, wherein the first drive motor 32, the second drive motor 33 and the ultrasonic generator 34 are respectively positioned at the upper surface of the main body 31 and at the rear side position, the first drive shaft 39 is connected to the first drive motor 32, the third rotary disk 38 is positioned at the middle position of the top surface of the main body 31 and penetrates through the top surface of the main body 31, the third rotary disk 38 is driven by the first drive shaft 39, the ultrasonic probes 311 are a plurality of probes which are uniformly distributed on the bottom surface of the third rotary disk 38 in a circular shape, the second drive shaft 310 is connected to the second drive motor 33, the second drive shaft 310 penetrates through the left side surface of the main body 31, the right end, the interiors of the first rotating disc 36 and the second rotating disc 37 are both hollow, the second rotating disc 37 is positioned on the right side of the first rotating disc 36, the axes of the first rotating disc 36 and the second rotating disc 37 are on the same straight line, the plurality of extraction pipes 35 are arranged, are circumferentially distributed between the first rotating disc 36 and the second rotating disc 37 and are communicated with the interiors of the first rotating disc 36 and the second rotating disc 37, the liquid outlet 29 of the rotary cleaning and juicing device 2 is connected to the first rotating disc 36 through a second pipeline 24, a second valve 25 is arranged on the second pipeline 24, an extraction solvent storage device 10 is arranged above the primary ultrasonic extraction device 3, the extraction solvent storage device 10 is connected to the first rotating disc 36 through a third pipeline 101, and a third valve 102 is arranged on the third pipeline 101; the second rotating disc 37 is connected to the filtering device 4 through a fourth pipe 312, and a fourth valve 313 is arranged on the fourth pipe 312; the filtering device 4 is connected to the solvent recovery device 5 through a pipeline five 41, a valve five 42 is arranged on the pipeline five 41, the solvent recovery device 5 is connected to the secondary solid-phase extraction device 6 through a pipeline six 51, and a valve six 52 is arranged on the pipeline six 51; an ethanol storage device 11 is arranged above the secondary solid-phase extraction device 6, the ethanol storage device 11 is connected to the secondary solid-phase extraction device 6 through a pipeline seven 111, a valve seven 112 is arranged on the pipeline seven 111, a collecting tank 62 is connected to the bottom of the secondary solid-phase extraction device 6 through a pipeline eight 61, a power supply 8 supplies power to a rotating motor, a stirring motor, a first driving motor 32 and a second driving motor 33, switch elements are arranged on the rotating motor, the stirring motor, the first driving motor 32 and the second driving motor 33, and the PLC 7 is connected with the ultrasonic generator 34, the valves and the switch elements.
Two inlets, namely an extraction solvent inlet 314 and an extract inlet 315, are arranged on the left end face of the first rotating disc 36, the third pipeline 101 is connected with the extraction solvent inlet 314, an electric telescopic sleeve 316 is arranged at the joint of the third pipeline 101 and the extraction solvent inlet 314, the second pipeline 24 is connected with the extract inlet 315, an electric telescopic sleeve 316 is also arranged at the joint of the second pipeline 24 and the extract inlet 315, an extraction liquid outlet 317 is arranged on the right side face of the second rotating disc 37, the extraction liquid outlet 317 is connected with the fourth pipeline 312, an electric telescopic sleeve 316 is also arranged at the joint of the extraction liquid outlet 317 and the fourth pipeline 312, and each electric telescopic sleeve 316 is connected to the PLC 7. Cover plates are arranged on the extraction solvent inlet 314, the to-be-extracted substance inlet 315 and the extraction liquid outlet 317, when the electric telescopic sleeve 316 is opened and extended, the pipeline ports are tightly attached to the corresponding extraction solvent inlet 314, the to-be-extracted substance inlet 315 and the extraction liquid outlet 317, the cover plates are pushed into the turntables to correspondingly connect the pipelines with the turntables, when the electric telescopic sleeve 316 is shortened, the pipeline ports are disconnected from the corresponding extraction solvent inlet 314, the to-be-extracted substance inlet 315 and the extraction liquid outlet 317, and the cover plates are automatically ejected to seal the corresponding extraction solvent inlet 314, the to-be-extracted substance inlet 315 and the extraction liquid outlet 317, so that the pipelines are correspondingly disconnected with the turntables.
A visual window 28 is further provided on the sidewall of the body 21, and the visual window 28 is circular and made of a transparent material so that the inside cleaning or pulverizing state can be observed.
Wherein, the cleaning solution storage devices 9 are three in total and respectively store clean water, 0.4 percent NaCl solution and 0.45 percent NaHCO3The solutions are respectively provided with independent valves, and the cleaning solution can be selected or matched according to the cleaning requirement.
The total number of the extraction solvent storage devices 10 is four, petroleum ether, ethyl acetate, water and lower alcohol are respectively stored in the extraction solvent storage devices, and the extraction solvent storage devices are respectively provided with independent valves, so that the extraction solvent can be selected or matched at will according to extraction requirements.
The ethanol storage device 11 stores the eluent which is 80% methanol.
The filler in the secondary solid phase extraction device 6 is: chlorogenic acid molecular imprinting polymer microspheres, magnetic nanoparticles and zeolite particles, wherein the mass ratio of the chlorogenic acid molecular imprinting polymer microspheres, the magnetic nanoparticles and the zeolite particles is 2.5: 5: 16.
The preparation method of the secondary solid phase extraction device 6 comprises the following steps:
(5) weighing the filler: weighing filler chlorogenic acid molecularly imprinted polymer microspheres, magnetic nanoparticles and zeolite particles;
(6) filling: uniformly mixing chlorogenic acid molecular imprinting polymer microspheres, magnetic nanoparticles and zeolite particles, loading into a hopper of a semi-automatic solid phase extraction assembly instrument, starting the instrument, adjusting the system pressure to be 0.5MPa, controlling the column filling amount to be 0.25g by a precision balance, and then filling a lower sieve plate, filling a filler, vibrating the filler and filling an upper sieve plate.
The preparation method of the chlorogenic acid molecular imprinting polymer microspheres comprises the following steps:
dissolving chlorogenic acid and methacrylic acid in a molar ratio of 1:3.5 in a mixed solution of acetonitrile and 4-vinylaniline, wherein the molar ratio of the acetonitrile to the 4-vinylaniline is 2:7, oscillating for 8 hours at room temperature, adding a crosslinking agent TRIM (1, 1, 1-tris (hydroxymethyl propane trimethacrylate) with the amount of 4.5 times of the amount of the methacrylic acid to obtain a mixture, ultrasonically degassing, introducing nitrogen into the mixture to remove oxygen, sealing, polymerizing for 20 hours in a constant-temperature water bath at 55 ℃, grinding and sieving the obtained polymer, settling for 2 times by using an acetic acid methanol solution with the volume fraction of 39%, eluting for 2 times by using tetrahydrofuran, filtering, and vacuum drying to constant weight to obtain the chlorogenic acid/methacrylic acid copolymer.
The method for efficiently extracting the eucommia ulmoides extract by using the device comprises the following steps:
s1, cleaning: the method comprises the following steps of turning on a power supply 8, feeding fresh eucommia ulmoides raw materials into a rotary cleaning and juicing device 2 from a eucommia ulmoides raw material channel 23, controlling a first valve 92 to be opened through a PLC (programmable logic controller) 7, introducing cleaning liquid in a cleaning liquid storage device 9 into the rotary cleaning and juicing device 2 through a first pipeline 91, wherein the introduction amount of the cleaning liquid is 11/15 of the volume of a machine body 21, introducing 0.4% NaCl solution, controlling a switching element of a rotary motor through the PLC 7, starting the rotary motor to drive the machine body 21 to rotate, cleaning the eucommia ulmoides raw materials, discharging the cleaning liquid from a cleaning liquid discharge port 26 after cleaning is finished, repeatedly cleaning for 3 times, and injecting clean water into the machine body after the last cleaning, wherein the amount of the clean water is 3 times of the mass of the eucommia ulm;
s2, juicing: the PLC controller 7 controls the switch element of the rotating motor to be closed, and simultaneously controls the switch element of the stirring motor to be opened, the stirring motor is started to drive the stirring head to work, the cleaned eucommia ulmoides raw material is squeezed into juice, and the eucommia ulmoides raw juice is discharged from a liquid outlet 29;
s3, primary extraction: controlling the opening of the second valve 25 through the PLC 7, controlling the electric telescopic sleeves 316 to tightly connect the second pipeline 24 with the inlet 315 of the extract to be extracted, tightly connecting the third pipeline 101 with the inlet 314 of the extraction solvent, disconnecting the fourth pipeline 312 with the outlet 317 of the extraction liquid, allowing the eucommia ulmoides juice to enter the first rotating disc 36 in the primary ultrasonic extraction device 3 through the second pipeline 24 and the inlet 315 of the extract to be extracted, continuously controlling the third valve 102 on the third pipeline 101 to be opened, and introducing the extraction solvent in the extraction solvent storage device 10 into the first rotating disc 36 through the third pipeline 101 and the inlet 314 of the extraction solvent; after the extraction tube 35 is filled with the eucommia ulmoides normal juice and the extraction solvent, the control valve II 25 and the valve III 102 are closed, the electric telescopic sleeves 316 on the control tube II 24 and the control tube III 101 are disconnected with the inlet 315 of the extract to be extracted and the inlet 314 of the extraction solvent, the ultrasonic generator 34, the first driving motor 32 and the second driving motor 33 are continuously controlled to start working, the first driving motor 32 drives the third rotating disc 38 to rotate through the first driving shaft 39, the second driving motor 33 drives the first rotating disc 36 to rotate through the second driving shaft 310, the first rotating disc simultaneously drives the extraction tube 35 and the second rotating disc 37 to rotate together, the ultrasonic wave generated by the ultrasonic generator 34 is emitted through the ultrasonic probe 311, and the eucommia ulmoides normal juice in the extraction tube 35 is subjected to ultrasonic extraction; after extracting for a certain time, controlling the switch elements of the first driving motor 32 and the second driving motor 33 to be closed, and simultaneously closing the ultrasonic generator 34 to finish primary extraction;
s4, filtering: the PLC 7 controls an electric telescopic sleeve 316 on the fourth pipeline 312 to tightly connect the fourth pipeline 312 with an extraction liquid outlet 317, and simultaneously opens a valve 313 on the fourth pipeline 312 to introduce the extracted mixed liquid into the filtering device 4 for filtering;
s5, solvent recovery: opening a valve five 42 on a pipeline five 41 under the control of a PLC 7, so that the filtered mixed solution enters a solvent recovery device 5 to recover the extraction solvent;
s6, secondary extraction: opening a valve six 52 on a pipeline six 51 under the control of the PLC 7, introducing the mixed solution with the recovered extraction solvent into a secondary solid-phase extraction device 6, and performing secondary adsorption extraction on the mixed solution with the recovered extraction solvent by using a filler in the secondary solid-phase extraction device 6;
s7, elution: controlling a valve seven 112 on a pipeline seven 111 to be opened through the PLC 7, introducing the ethanol in the ethanol storage device 11 into the secondary solid phase extraction device 6 for elution to obtain an eluent, and introducing the eluent into a collecting tank 62 through a pipeline eight 61 for collection;
s8, drying: concentrating and drying the collected eluent to obtain the eucommia ulmoides extract.
Example 3:
a high-efficient extraction element of cortex Eucommiae extract for cardiovascular disease prevention and cure, mainly include the body 1 rotates and washes the extractor 2, the ultrasonic extractor 3 of the first time, filter equipment 4, solvent recovery unit 5, the solid phase extractor 6 of the second time, PLC controller 7 and power 8, rotate and wash the extractor 2, the ultrasonic extractor 3 of the first time, filter equipment 4, solvent recovery unit 5, the solid phase extractor 6 of the second time, PLC controller 7 and power 8 and locate in body 1, body 1 is cuboid; the rotary cleaning juicing device 2 mainly comprises a machine body 21 and a base 22, wherein a rotary motor and a stirring motor are arranged in the base 22, a stirring head is arranged in the machine body 21, the rotary motor drives the machine body 21 to rotate, and the stirring motor drives the stirring head to stir; a cleaning liquid storage device 9 is arranged above the machine body 21, the cleaning liquid storage device 9 is communicated with the top of the machine body 21 through a first pipeline 91, a first valve 92 is arranged on the first pipeline 91, an eucommia ulmoides raw material channel 23 is arranged on the side surface of the machine body 21, one end of the eucommia ulmoides raw material channel 23 is connected with the machine body 21, the other end of the eucommia ulmoides raw material channel 23 leads to the outside of the shell 1, a cleaning liquid outlet 26 is also arranged at the lower part of the machine body 21, and a filter screen; the primary ultrasonic extraction device 3 mainly comprises a main body 31, a first drive motor 32, a second drive motor 33, an ultrasonic generator 34, an extraction tube 35, a first rotary disk 36, a second rotary disk 37, a third rotary disk 38, a first drive shaft 39, a second drive shaft 310 and an ultrasonic probe 311, wherein the first drive motor 32, the second drive motor 33 and the ultrasonic generator 34 are respectively positioned at the upper surface of the main body 31 and at the rear side position, the first drive shaft 39 is connected to the first drive motor 32, the third rotary disk 38 is positioned at the middle position of the top surface of the main body 31 and penetrates through the top surface of the main body 31, the third rotary disk 38 is driven by the first drive shaft 39, the ultrasonic probes 311 are a plurality of probes which are uniformly distributed on the bottom surface of the third rotary disk 38 in a circular shape, the second drive shaft 310 is connected to the second drive motor 33, the second drive shaft 310 penetrates through the left side surface of the main body 31, the right end, the interiors of the first rotating disc 36 and the second rotating disc 37 are both hollow, the second rotating disc 37 is positioned on the right side of the first rotating disc 36, the axes of the first rotating disc 36 and the second rotating disc 37 are on the same straight line, the plurality of extraction pipes 35 are arranged, are circumferentially distributed between the first rotating disc 36 and the second rotating disc 37 and are communicated with the interiors of the first rotating disc 36 and the second rotating disc 37, the liquid outlet 29 of the rotary cleaning and juicing device 2 is connected to the first rotating disc 36 through a second pipeline 24, a second valve 25 is arranged on the second pipeline 24, an extraction solvent storage device 10 is arranged above the primary ultrasonic extraction device 3, the extraction solvent storage device 10 is connected to the first rotating disc 36 through a third pipeline 101, and a third valve 102 is arranged on the third pipeline 101; the second rotating disc 37 is connected to the filtering device 4 through a fourth pipe 312, and a fourth valve 313 is arranged on the fourth pipe 312; the filtering device 4 is connected to the solvent recovery device 5 through a pipeline five 41, a valve five 42 is arranged on the pipeline five 41, the solvent recovery device 5 is connected to the secondary solid-phase extraction device 6 through a pipeline six 51, and a valve six 52 is arranged on the pipeline six 51; an ethanol storage device 11 is arranged above the secondary solid-phase extraction device 6, the ethanol storage device 11 is connected to the secondary solid-phase extraction device 6 through a pipeline seven 111, a valve seven 112 is arranged on the pipeline seven 111, a collecting tank 62 is connected to the bottom of the secondary solid-phase extraction device 6 through a pipeline eight 61, a power supply 8 supplies power to a rotating motor, a stirring motor, a first driving motor 32 and a second driving motor 33, switch elements are arranged on the rotating motor, the stirring motor, the first driving motor 32 and the second driving motor 33, and the PLC 7 is connected with the ultrasonic generator 34, the valves and the switch elements.
Two inlets, namely an extraction solvent inlet 314 and an extract inlet 315, are arranged on the left end face of the first rotating disc 36, the third pipeline 101 is connected with the extraction solvent inlet 314, an electric telescopic sleeve 316 is arranged at the joint of the third pipeline 101 and the extraction solvent inlet 314, the second pipeline 24 is connected with the extract inlet 315, an electric telescopic sleeve 316 is also arranged at the joint of the second pipeline 24 and the extract inlet 315, an extraction liquid outlet 317 is arranged on the right side face of the second rotating disc 37, the extraction liquid outlet 317 is connected with the fourth pipeline 312, an electric telescopic sleeve 316 is also arranged at the joint of the extraction liquid outlet 317 and the fourth pipeline 312, and each electric telescopic sleeve 316 is connected to the PLC 7. Cover plates are arranged on the extraction solvent inlet 314, the to-be-extracted substance inlet 315 and the extraction liquid outlet 317, when the electric telescopic sleeve 316 is opened and extended, the pipeline ports are tightly attached to the corresponding extraction solvent inlet 314, the to-be-extracted substance inlet 315 and the extraction liquid outlet 317, the cover plates are pushed into the turntables to correspondingly connect the pipelines with the turntables, when the electric telescopic sleeve 316 is shortened, the pipeline ports are disconnected from the corresponding extraction solvent inlet 314, the to-be-extracted substance inlet 315 and the extraction liquid outlet 317, and the cover plates are automatically ejected to seal the corresponding extraction solvent inlet 314, the to-be-extracted substance inlet 315 and the extraction liquid outlet 317, so that the pipelines are correspondingly disconnected with the turntables.
A visual window 28 is further provided on the sidewall of the body 21, and the visual window 28 is circular and made of a transparent material so that the inside cleaning or pulverizing state can be observed.
Wherein, the cleaning solution storage devices 9 are three in total and respectively store clean water, 0.5 percent NaCl solution and 0.6 percent NaHCO3The solutions are respectively provided with independent valves, and the cleaning solution can be selected or matched according to the cleaning requirement.
The total number of the extraction solvent storage devices 10 is four, petroleum ether, ethyl acetate, water and lower alcohol are respectively stored in the extraction solvent storage devices, and the extraction solvent storage devices are respectively provided with independent valves, so that the extraction solvent can be selected or matched at will according to extraction requirements.
The ethanol storage device 11 stores an eluent which is 82% methanol.
The filler in the secondary solid phase extraction device 6 is: chlorogenic acid molecular imprinting polymer microspheres, magnetic nanoparticles and zeolite particles, wherein the mass ratio of the chlorogenic acid molecular imprinting polymer microspheres, the magnetic nanoparticles and the zeolite particles is 4: 5: 20.
The preparation method of the secondary solid phase extraction device 6 comprises the following steps:
(7) weighing the filler: weighing filler chlorogenic acid molecularly imprinted polymer microspheres, magnetic nanoparticles and zeolite particles;
(8) filling: uniformly mixing chlorogenic acid molecular imprinting polymer microspheres, magnetic nanoparticles and zeolite particles, loading into a hopper of a semi-automatic solid phase extraction assembly instrument, starting the instrument, adjusting the system pressure to be 0.5MPa, controlling the column filling amount to be 0.25g by a precision balance, and then filling a lower sieve plate, filling a filler, vibrating the filler and filling an upper sieve plate.
The preparation method of the chlorogenic acid molecular imprinting polymer microspheres comprises the following steps:
dissolving chlorogenic acid and methacrylic acid in a molar ratio of 1:5 in a mixed solution of acetonitrile and 4-vinylaniline, wherein the molar ratio of acetonitrile to 4-vinylaniline is 2:7, oscillating for 8 hours at room temperature, adding a crosslinking agent TRIM (1, 1, 1-tris (hydroxymethyl propane trimethacrylate) with the amount of 4.5 times of methacrylic acid to obtain a mixture, ultrasonically degassing, introducing nitrogen into the mixture to remove oxygen, sealing, polymerizing for 20 hours in a constant-temperature water bath at 60 ℃, grinding and sieving the obtained polymer, settling for 3 times by using an acetic acid methanol solution with the volume fraction of 48%, eluting for 3 times by using tetrahydrofuran, filtering, and vacuum drying to constant weight to obtain the chlorogenic acid-methacrylic acid copolymer.
The method for efficiently extracting the eucommia ulmoides extract by using the device comprises the following steps:
s1, cleaning: the power supply 8 is turned on, fresh eucommia ulmoides raw materials are sent into the rotary cleaning and juicing device 2 from the eucommia ulmoides raw material channel 23, the first valve 92 is controlled to be opened through the PLC 7, cleaning liquid in the cleaning liquid storage device 9 is introduced into the rotary cleaning and juicing device 2 through the first pipeline 91, the introduction amount of the cleaning liquid is 4/5 of the volume of the machine body 21, and 0.6% of NaHCO is introduced3The solution is then used for controlling a switching element of a rotating motor through a PLC (programmable logic controller) 7, the rotating motor is started to drive a machine body 21 to rotate, the eucommia ulmoides raw material is cleaned, after the cleaning is finished, cleaning liquid is discharged from a cleaning liquid discharge port 26, the cleaning is repeated for 4 times, clean water is injected into the machine body after the cleaning is finished for the last time, and the amount of the clean water is 5 times of the mass of the eucommia ulmoides raw material;
s2, juicing: the PLC controller 7 controls the switch element of the rotating motor to be closed, and simultaneously controls the switch element of the stirring motor to be opened, the stirring motor is started to drive the stirring head to work, the cleaned eucommia ulmoides raw material is squeezed into juice, and the eucommia ulmoides raw juice is discharged from a liquid outlet 29;
s3, primary extraction: controlling the opening of the second valve 25 through the PLC 7, controlling the electric telescopic sleeves 316 to tightly connect the second pipeline 24 with the inlet 315 of the extract to be extracted, tightly connecting the third pipeline 101 with the inlet 314 of the extraction solvent, disconnecting the fourth pipeline 312 with the outlet 317 of the extraction liquid, allowing the eucommia ulmoides juice to enter the first rotating disc 36 in the primary ultrasonic extraction device 3 through the second pipeline 24 and the inlet 315 of the extract to be extracted, continuously controlling the third valve 102 on the third pipeline 101 to be opened, and introducing the extraction solvent in the extraction solvent storage device 10 into the first rotating disc 36 through the third pipeline 101 and the inlet 314 of the extraction solvent; after the extraction tube 35 is filled with the eucommia ulmoides normal juice and the extraction solvent, the control valve II 25 and the valve III 102 are closed, the electric telescopic sleeves 316 on the control tube II 24 and the control tube III 101 are disconnected with the inlet 315 of the extract to be extracted and the inlet 314 of the extraction solvent, the ultrasonic generator 34, the first driving motor 32 and the second driving motor 33 are continuously controlled to start working, the first driving motor 32 drives the third rotating disc 38 to rotate through the first driving shaft 39, the second driving motor 33 drives the first rotating disc 36 to rotate through the second driving shaft 310, the first rotating disc simultaneously drives the extraction tube 35 and the second rotating disc 37 to rotate together, the ultrasonic wave generated by the ultrasonic generator 34 is emitted through the ultrasonic probe 311, and the eucommia ulmoides normal juice in the extraction tube 35 is subjected to ultrasonic extraction; after extracting for a certain time, controlling the switch elements of the first driving motor 32 and the second driving motor 33 to be closed, and simultaneously closing the ultrasonic generator 34 to finish primary extraction;
s4, filtering: the PLC 7 controls an electric telescopic sleeve 316 on the fourth pipeline 312 to tightly connect the fourth pipeline 312 with an extraction liquid outlet 317, and simultaneously opens a valve 313 on the fourth pipeline 312 to introduce the extracted mixed liquid into the filtering device 4 for filtering;
s5, solvent recovery: opening a valve five 42 on a pipeline five 41 under the control of a PLC 7, so that the filtered mixed solution enters a solvent recovery device 5 to recover the extraction solvent;
s6, secondary extraction: opening a valve six 52 on a pipeline six 51 under the control of the PLC 7, introducing the mixed solution with the recovered extraction solvent into a secondary solid-phase extraction device 6, and performing secondary adsorption extraction on the mixed solution with the recovered extraction solvent by using a filler in the secondary solid-phase extraction device 6;
s7, elution: controlling a valve seven 112 on a pipeline seven 111 to be opened through the PLC 7, introducing the ethanol in the ethanol storage device 11 into the secondary solid phase extraction device 6 for elution to obtain an eluent, and introducing the eluent into a collecting tank 62 through a pipeline eight 61 for collection;
s8, drying: concentrating and drying the collected eluent to obtain the eucommia ulmoides extract.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (9)

1. The eucommia ulmoides extract efficient extraction device for preventing and treating cardiovascular diseases is characterized by mainly comprising a shell (1), a rotary cleaning juicing device (2), a primary ultrasonic extraction device (3), a filtering device (4), a solvent recovery device (5), a secondary solid-phase extraction device (6), a PLC (programmable logic controller) and a power supply (8), wherein the rotary cleaning juicing device (2), the primary ultrasonic extraction device (3), the filtering device (4), the solvent recovery device (5), the secondary solid-phase extraction device (6), the PLC (7) and the power supply (8) are all located inside the shell (1), and the shell (1) is cuboid; the rotary cleaning juicing device (2) mainly comprises a machine body (21) and a base (22), wherein a rotary motor and a stirring motor are arranged in the base (22), a stirring head is arranged in the machine body (21), the rotary motor drives the machine body (21) to rotate, and the stirring motor drives the stirring head to perform stirring action; a cleaning liquid storage device (9) is arranged above the machine body (21), the cleaning liquid storage device (9) is communicated with the top of the machine body (21) through a first pipeline (91), a first valve (92) is arranged on the first pipeline (91), an eucommia ulmoides raw material channel (23) is arranged on the side face of the machine body (21), one end of the eucommia ulmoides raw material channel (23) is connected with the machine body (21), the other end of the eucommia ulmoides raw material channel is communicated with the outside of the shell (1), a cleaning liquid discharge port (26) is further arranged at the lower part of the machine body (21), and a filter screen (27) is arranged on the cleaning liquid; the primary ultrasonic extraction device (3) mainly comprises a main body (31), a first drive motor (32), a second drive motor (33), an ultrasonic generator (34), an extraction tube (35), a first rotary disk (36), a second rotary disk (37), a third rotary disk (38), a first drive shaft (39), a second drive shaft (310) and an ultrasonic probe (311), wherein the first drive motor (32), the second drive motor (33) and the ultrasonic generator (34) are respectively positioned on the upper surface of the main body (31) close to the rear side, the first drive shaft (39) is connected to the first drive motor (32), the third rotary disk (38) is positioned in the middle position of the top surface of the main body (31) and penetrates through the top surface of the main body (31), the third rotary disk (38) is driven by the first drive shaft (39), and the ultrasonic probes (311) are multiple in total, a second driving shaft (310) is circularly and uniformly distributed on the bottom surface of the third rotating disk (38), the second driving shaft (310) is connected to the second driving motor (33), the second driving shaft (310) traverses the left side surface of the main body (31), the right end of the second driving shaft (310) is connected to the left end surface of the first rotating disk (36), the first rotating disk (36) and the second rotating disk (37) are both hollow inside, the second rotating disk (37) is positioned at the right side of the first rotating disk (36), the axes of the first rotating disk and the second rotating disk are on the same straight line, the extraction pipes (35) are distributed in multiple numbers and are circumferentially distributed between the first rotating disk (36) and the second rotating disk (37) and are communicated with the insides of the first rotating disk (36) and the second rotating disk (37), and the liquid outlet (29) of the rotary cleaning and juicing device (2) is connected to the first rotating disk (36) through a second pipeline (24, a second valve (25) is arranged on the second pipeline (24), an extraction solvent storage device (10) is arranged above the primary ultrasonic extraction device (3), the extraction solvent storage device (10) is connected to the first rotating disc (36) through a third pipeline (101), and a third valve (102) is arranged on the third pipeline (101); the second rotating disc (37) is connected to the filtering device (4) through a fourth pipe (312), and a fourth valve (313) is arranged on the fourth pipe (312); the filtering device (4) is connected to the solvent recovery device (5) through a fifth pipeline (41), a fifth valve (42) is arranged on the fifth pipeline (41), the solvent recovery device (5) is connected to the secondary solid-phase extraction device (6) through a sixth pipeline (51), and a sixth valve (52) is arranged on the sixth pipeline (51); be equipped with ethanol storage device (11) in the top of secondary solid phase extraction device (6), ethanol storage device (11) are connected to secondary solid phase extraction device (6) through pipeline seven (111) be equipped with valve seven (112) on pipeline seven (111), are connected with collecting vat (62) through pipeline eight (61) in the bottom of secondary solid phase extraction device (6), power (8) do rotating electrical machines, agitator motor, first driving motor (32) and second driving motor (33) power supply all be equipped with the switch element on rotating electrical machines, agitator motor, first driving motor (32) and second driving motor (33), PLC controller (7) with supersonic generator (34), each valve and each switch element connect.
2. The eucommia ulmoides extract efficient extraction device for preventing and treating cardiovascular diseases according to claim 1, wherein two inlets are provided on the left end surface of the first rotating disk (36), namely an extraction solvent inlet (314) and an extract inlet (315), the third pipeline (101) is connected with the extraction solvent inlet (314), an electric telescopic sleeve (316) is provided at the connection of the third pipeline (101) and the extraction solvent inlet (314), the second pipeline (24) is connected with the extract inlet (315), an electric telescopic sleeve (316) is also provided at the connection of the second pipeline (24) and the extract inlet (315), an extract outlet (317) is provided on the right side surface of the second rotating disk (37), the extract outlet (317) is connected with the fourth pipeline (312), and an electric telescopic sleeve (316) is also provided at the connection of the extract outlet (317) and the fourth pipeline (312), each electric telescopic sleeve (316) is connected to the PLC controller (7).
3. The eucommia ulmoides extract efficient extraction device for cardiovascular disease prevention and treatment according to claim 1, wherein a visible window (28) is further provided on the side wall of the body (21), and the visible window (28) is circular and made of a transparent material.
4. The eucommia ulmoides extract efficient extraction device for cardiovascular disease prevention and treatment according to claim 1, wherein the cleaning solution storage device (9) has three cleaning solution storage devices, and each cleaning solution storage device is provided with three cleaning solution storage devicesStoring clear water, 0.3-0.5% NaCl solution and 0.3-0.6% NaHCO3Solutions, each equipped with a separate valve.
5. The eucommia ulmoides extract efficient extraction device for cardiovascular disease prevention and treatment according to claim 1, wherein the number of the extraction solvent storage devices (10) is four, petroleum ether, ethyl acetate, water and lower alcohol are respectively stored in the extraction solvent storage devices, and each extraction solvent storage device is provided with an independent valve.
6. The eucommia ulmoides extract efficient extraction device for preventing and treating cardiovascular diseases according to claim 1, wherein an eluent is stored in the ethanol storage device (11), and the eluent is 75-82% methanol.
7. The eucommia ulmoides extract efficient extraction device for cardiovascular disease prevention and treatment according to claim 1, wherein the filler in the secondary solid phase extraction device (6) is: chlorogenic acid molecularly imprinted polymer microspheres, magnetic nanoparticles and zeolite particles, wherein the mass ratio of the chlorogenic acid molecularly imprinted polymer microspheres to the magnetic nanoparticles to the zeolite particles is 1-4: 5: 12-20.
8. The eucommia ulmoides extract efficient extraction device for cardiovascular disease prevention and treatment according to claim 7, wherein the preparation method of the chlorogenic acid molecular imprinting polymer microspheres comprises the following steps:
dissolving chlorogenic acid and methacrylic acid in a molar ratio of 1:2-1:5 in a mixed solution of acetonitrile and 4-vinylaniline, wherein the molar ratio of acetonitrile to 4-vinylaniline is 2:7, oscillating for 8 hours at room temperature, adding a crosslinking agent TRIM with the amount of 4.5 times of methacrylic acid to obtain a mixture, then carrying out ultrasonic degassing, introducing nitrogen into the mixture to remove oxygen, sealing, polymerizing for 20 hours in a constant-temperature water bath at 50-60 ℃, grinding and sieving the obtained polymer, settling for 1-3 times by using an acetic acid methanol solution with the volume fraction of 30-48%, eluting for 1-3 times by using tetrahydrofuran, filtering, and carrying out vacuum drying to constant weight to obtain the chlorogenic acid-methacrylic acid copolymer.
9. The method for efficiently extracting the eucommia ulmoides extract according to any one of claims 1 to 8, wherein the method comprises the following steps:
s1, cleaning: turning on a power supply (8), sending fresh eucommia ulmoides raw materials into a rotary cleaning and juicing device (2) from a eucommia ulmoides raw material channel (23), controlling a first valve (92) to be opened through a PLC (7), introducing cleaning liquid in a cleaning liquid storage device (9) into the rotary cleaning and juicing device (2) through a first pipeline (91), wherein the introduction amount of the cleaning liquid is 2/3-4/5 of the volume of a machine body (21), and introducing clean water, or 0.3-0.5% of NaCl solution, or 0.3-0.6% of NaHCO solution selectively3The solution or any two or three of the solutions are mixed according to any proportion, then the PLC (7) is used for controlling a switching element of a rotating motor, the rotating motor is started to drive a machine body (21) to rotate, the eucommia ulmoides raw materials are cleaned, after the cleaning is finished, cleaning liquid is discharged from a cleaning liquid discharge port (26), the cleaning is repeated for 2 to 4 times, and clean water is injected into the machine body after the cleaning is finished for the last time, wherein the amount of the clean water is 3 to 5 times of the mass of the eucommia ulmoides raw materials;
s2, juicing: the PLC (7) is used for controlling the switch element of the rotating motor to be closed, and simultaneously controlling the switch element of the stirring motor to be opened, starting the stirring motor to drive the stirring head to work, squeezing the cleaned eucommia ulmoides raw materials into juice to obtain eucommia ulmoides normal juice, and discharging the eucommia ulmoides normal juice from a liquid outlet (29);
s3, primary extraction: controlling the opening of a second valve (25) through a PLC (7), simultaneously controlling each electric telescopic sleeve (316) to tightly joint a second pipeline (24) with an inlet (315) of the extract to be extracted, tightly joint a third pipeline (101) with an inlet (314) of the extraction solvent, disconnecting a fourth pipeline (312) with an extraction liquid outlet (317), allowing the eucommia ulmoides normal juice to enter a first rotating disc (36) in the primary ultrasonic extraction device (3) through the second pipeline (24) and the inlet (315) of the extract to be extracted, continuously controlling the opening of a third valve (102) on the third pipeline (101), and introducing the extraction solvent in the extraction solvent storage device (10) into the first rotating disc (36) through the third pipeline (101) and the inlet (314) of the extraction solvent; after the eucommia ulmoides normal juice and the extraction solvent are filled in the extraction pipe (35), the control valve II (25) and the valve III (102) are closed, the electric telescopic sleeves (316) on the control pipeline II (24) and the pipeline III (101) are disconnected with the inlet (315) of the extract to be extracted and the inlet (314) of the extraction solvent, the ultrasonic generator (34) and the first driving motor (32) are continuously controlled, the second driving motor (33) starts to work, the first driving motor (32) drives the third rotating disc (38) to rotate through the first driving shaft (39), the second driving motor (33) drives the first rotating disc (36) to rotate through the second driving shaft (310), the first rotating disc drives the extraction tube (35) and the second rotating disc (37) to rotate together, ultrasonic waves generated by the ultrasonic generator (34) are emitted through the ultrasonic probe (311), and ultrasonic extraction is carried out on the eucommia ulmoides normal juice in the extraction tube (35); after extracting for a certain time, controlling the switching elements of the first driving motor (32) and the second driving motor (33) to be closed, and simultaneously closing the ultrasonic generator (34) to finish primary extraction;
s4, filtering: the PLC (7) controls an electric telescopic sleeve (316) on the fourth pipeline (312) to tightly connect the fourth pipeline (312) with the extraction liquid outlet (317), meanwhile, a fourth valve (313) on the fourth pipeline (312) is opened, and the extracted mixed liquid is introduced into the filtering device (4) for filtering;
s5, solvent recovery: a valve five (42) on a pipeline five (41) is controlled to be opened through a PLC (7), so that the filtered mixed solution enters a solvent recovery device (5) to recover the extraction solvent;
s6, secondary extraction: opening a valve six (52) on a pipeline six (51) under the control of a PLC (7), introducing the mixed liquid with the recovered extraction solvent into a secondary solid-phase extraction device (6), and performing secondary adsorption extraction on the mixed liquid with the recovered extraction solvent by using a filler in the secondary solid-phase extraction device (6);
s7, elution: a valve seven (112) on a pipeline seven (111) is controlled to be opened by a PLC (7), ethanol in the ethanol storage device (11) is introduced into the secondary solid phase extraction device (6) for elution to obtain eluent, and then the eluent is introduced into a collecting tank (62) for collection through a pipeline eight (61);
s8, drying: concentrating and drying the collected eluent to obtain the eucommia ulmoides extract.
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