CN112023440A - Jet flow extraction device and application method thereof - Google Patents

Jet flow extraction device and application method thereof Download PDF

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Publication number
CN112023440A
CN112023440A CN202010981685.8A CN202010981685A CN112023440A CN 112023440 A CN112023440 A CN 112023440A CN 202010981685 A CN202010981685 A CN 202010981685A CN 112023440 A CN112023440 A CN 112023440A
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extraction
pressure
equipment
application example
solvent
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赵兵
常森林
赵庆生
王晓东
赵明霞
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Institute of Process Engineering of CAS
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Institute of Process Engineering of CAS
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01D11/02—Solvent extraction of solids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids
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    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F31/00—Mixers with shaking, oscillating, or vibrating mechanisms
    • B01F31/80—Mixing by means of high-frequency vibrations above one kHz, e.g. ultrasonic vibrations
    • B01F31/83—Mixing by means of high-frequency vibrations above one kHz, e.g. ultrasonic vibrations comprising a supplementary stirring element
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    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
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Abstract

The invention provides a jet flow extraction device and an application method thereof. According to the jet extraction device, the dissolution rate of effective components in the plant raw materials is improved by adopting a high-pressure extraction mode, and the solid-liquid extraction effect between the plant raw materials and the extraction solvent is enhanced; the decompression process after high-pressure extraction can strengthen the material exchange process, and the dissolved effective components are better brought into the main body of the solvent, so that the solid-liquid extraction process is further strengthened, and the aim of efficiently extracting the effective components is fulfilled; the device has the advantages of simple structure, simple and convenient process operation, greenness and environmental protection, and is beneficial to popularization of large-scale production.

Description

Jet flow extraction device and application method thereof
Technical Field
The invention belongs to the technical field of plant component extraction, and relates to a jet flow extraction device and an application method thereof.
Background
Due to the diversity of plant species, the active ingredients contained in the plants have wide application in a plurality of fields such as food, medicine and the like, and especially, the natural medicinal ingredients in the plants have important functions in the aspects of improving the curative effect of the medicine, reducing the toxicity of the medicine, promoting the research of new medicines, exploring disease curing mechanisms and the like, so the extraction technology of the plant active ingredients is indispensable. With the rapid development of modern science and technology, the technology for extracting effective components from plants is also changing day by day and is continuously applied to actual production, so that the development of plant extraction industry is accelerated.
The traditional plant effective component extraction technology comprises a soaking extraction process, a stewing extraction process and the like, and has the defects of complex process, long production period, large solvent consumption, difficult recovery, large equipment investment and the like to different degrees. Modern extraction technologies mainly comprise ultrasonic extraction, supercritical fluid extraction, countercurrent extraction, dynamic extraction and the like, and various extraction technologies have advantages, disadvantages and application ranges due to complexity and difference of plant structures, but generally have the problems of loss of activity of thermosensitive substances and large solvent consumption during hot extraction.
CN 209019954U discloses a plant composition countercurrent extraction equipment, including extraction element, extraction element is including being used for to the plant extract in the cream solvent that increases countercurrent solvent add the structure, be used for holding the solvent and add the finished extraction fluid reservoir of structure output, still including being used for carrying the plant to extraction element and extracting the raw materials processing structure of cream, raw materials processing structure is including the steeping vat that is used for depositing the plant raw materials, the material high-pressure pump that links to each other with the steeping vat, the ejection of compact position of material high-pressure pump is connected with the extraction vat that is used for holding semi-manufactured goods, the ejection of compact position of extraction vat leads to extraction element to link to each other with extraction element is sealed. The extraction equipment additionally adds solvent to perform countercurrent extraction of plant components, the solvent consumption is large, the countercurrent condition needs to maintain pressure, and a decompression process is not performed to release the extract by utilizing high pressure difference.
CN 102772912A discloses a device and a method for extracting active ingredients of natural plants by a high-pressure spray countercurrent method, wherein natural plant impurities to be extracted are crushed after the device is connected; adding the soaking solution into a stirring tank to obtain a material suspension, adding an extraction solvent into an extraction tank, spraying the prepared material suspension into mist-shaped liquid drops for spray extraction, then performing high-pressure spray countercurrent extraction, and finally removing solid impurities by using a centrifugal machine; concentrating under reduced pressure, and spray drying, microwave drying or vacuum drying to obtain product; the device comprises a multistage stirring tank and a multistage extraction tank, the extraction process is complex, the requirement of the spray extraction process on the conditions of technological operation is strict, and the device is difficult to enlarge and use.
In summary, for the extraction of plant effective components, an extraction device with wide applicability and simple structure is required to be selected, and the characteristics of extraction technology are fully utilized to improve the extraction efficiency.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a jet flow extraction device and an application method thereof, wherein the jet flow extraction device enhances the solid-liquid extraction effect between a plant raw material and an extraction solvent by adopting a high-pressure extraction mode, and enhances the separation effect between the plant raw material and the extraction solvent by a pressure reduction process, so that the extraction efficiency of plant effective components is improved, the extraction process is simplified, and the cost is reduced.
In order to achieve the purpose, the invention adopts the following technical scheme:
in one aspect, the invention provides a jet extraction device, which comprises a material mixing device, a pressurization device, a high-pressure extraction device and a pressure reduction circulation device, wherein the material mixing device, the pressurization device, the high-pressure extraction device and the pressure reduction circulation device are sequentially connected, and an outlet of the pressure reduction circulation device is connected with an inlet of the material mixing device.
In the invention, because the effective components in the plant often exist in cells and organelles and need to be extracted and undergo a complex mass transfer process, the extraction technology generally needs to improve the permeability of cell membranes and cell walls and even break the cells, the device completes an extraction cycle by the mixing, pressurizing, extracting and depressurizing processes of raw materials and solvents, destroys the integrity of the cells by utilizing the high pressure condition, ensures that the effective components in the cells are dissolved out but still exist in the gaps of the cells or tissues, and then enhances the material exchange process by utilizing the larger pressure difference between the inside and the outside of the cells through rapid depressurization, so that the dissolved effective components are better brought into a solvent main body, thereby improving the extraction effect; the device has the advantages of simple structure, simple and convenient process operation, greenness and environmental protection, and is beneficial to large-scale production.
The following technical solutions are preferred technical solutions of the present invention, but not limited to the technical solutions provided by the present invention, and technical objects and advantageous effects of the present invention can be better achieved and achieved by the following technical solutions.
As the preferable technical scheme of the invention, the material mixing equipment is internally provided with a stirring component, and the outside is provided with a temperature control jacket.
Preferably, the temperature control jacket is also connected with a heat source device.
In the invention, due to the difference of effective components in plants, the suitable extraction temperature is also different, and the performance of the effective components is often greatly influenced by the temperature, so the extraction temperature needs to be controlled, the temperature of a mixed material can be controlled when the plant raw material is mixed with a solvent, a temperature control jacket mode is adopted, and in order to quickly mix, stirring is usually needed, and a primary extraction process can be completed.
Preferably, an ultrasonic generating device is further arranged in the material mixing device.
Preferably, the ultrasound generating device comprises a focused ultrasound transducer and/or a divergent ultrasound transducer.
According to the invention, the sound energy of ultrasonic waves can be utilized to break cells, accelerate the dissolution of effective components of the cells and promote the diffusion of the effective components, so that the ultrasonic conditions are supplemented in the material mixing process, the dispersive mixing of plant raw materials can be accelerated, the primary destruction of the cells can be preliminarily completed, and the subsequent high-pressure extraction is facilitated.
Preferably, the number of the ultrasonic generating devices is at least one, such as one, two, three or four, and the like, and the number is set according to the size of the material mixing device and the size and the type of the ultrasonic generating devices.
Preferably, the energy concentrating ultrasonic transducer and the diverging ultrasonic transducer are arranged separately or together.
As a preferred technical scheme, the pressurizing device comprises a high-pressure delivery pump.
According to the invention, the pressurizing equipment conveys the mixed material into the high-pressure extraction equipment, the pressure in the equipment is continuously increased, and the pressure is maintained after the required pressure is reached.
Preferably, the high pressure extraction device is hermetically hollow.
Preferably, a pressure detection device is arranged on the high-pressure extraction equipment.
Preferably, the pressure detecting means includes any one of an elastic pressure measuring instrument, an electrical pressure measuring instrument, or a load pressure measuring instrument.
Preferably, the electrically-measured pressure measuring instrument comprises a pressure sensor comprising any one of a piezoelectric pressure sensor, a resistive pressure sensor, a capacitive pressure sensor or a strain gauge pressure sensor.
Preferably, the outlet of the high-pressure extraction device is provided with a pressure reduction device.
Preferably, the pressure reducing means comprises a pressure reducing valve.
Preferably, the pressure reducing valve comprises any one of a piston type pressure reducing valve, a diaphragm type pressure reducing valve or a direct acting type pressure reducing valve.
In the invention, in order to maintain the pressure of the extraction equipment, a closed condition needs to be set, the pressure gauge is arranged to monitor the pressure in the equipment in real time, after the high-pressure extraction time is reached, the valve at the outlet is opened to quickly reduce the pressure, the material can be sprayed out by utilizing the pressure difference to enter the pressure reduction circulation equipment, and meanwhile, the process can also utilize the larger pressure difference to achieve the aim of further extraction.
In the present invention, the material of the high pressure extraction device is selected to withstand high pressure conditions, at least greater than the maximum extraction pressure, and according to the invention, the device material is selected to withstand at least a design pressure of 20MPa, such as 20MPa, 22MPa, 24MPa, 26MPa, 28MPa or 30MPa, but not limited to the recited values, and other values not recited within this range are equally applicable.
As the preferable technical scheme of the invention, a circulating pump is arranged on a connecting pipeline of the pressure reduction circulating equipment and the material mixing equipment.
Preferably, the decompression cycle equipment is further connected with an outlet pipeline which is parallel to the circulation pipeline.
Preferably, the decompression circulating equipment is provided with a sight glass.
Preferably, the decompression circulating equipment is provided with a jacket.
In the invention, the interior of the reduced-pressure circulating equipment is in a normal-pressure environment, a sight glass is arranged on the surface of the reduced-pressure circulating equipment, the internal condition of the reduced-pressure circulating equipment is observed, and the reduced-pressure circulating equipment has the functions of temporarily storing extracting solution and releasing the extracting solution; after the extracting solution of the device flows out, the extracting solution can return to the material mixing device for multiple times of extraction, and finally the extracting solution is discharged after reaching the extraction requirement for subsequent separation operation.
In the invention, a pipeline is directly connected between the outlet of the pressurizing equipment and the outlet of the pressure reduction circulating equipment, a valve is arranged on the pipeline, and circulating extraction under normal pressure can be realized through circulation of materials in the material mixing equipment.
In another aspect, the present invention provides an application method of the above jet extraction device, where the application method includes:
mixing the plant material and the extraction solvent, pressurizing by a pressurizing device, performing high-pressure extraction, and performing cyclic extraction or discharge after pressure reduction and injection.
As a preferred embodiment of the present invention, the plant material comprises any one or a combination of at least two of lycium ruthenicum, cistanche, industrial hemp, asparagus, forsythia, gardenia, lycium barbarum or turmeric, and typical but non-limiting examples of the combination are: the combination of lycium ruthenicum mill and cistanche deserticola, the combination of asparagus and forsythia suspensa, the combination of cistanche deserticola, industrial hemp and asparagus, the combination of gardenia, lycium barbarum and turmeric, and the like.
Preferably, the plant material is first crushed and then mixed with the extraction solvent.
Preferably, the plant material is comminuted to a particle size of no greater than 2mm, for example 2mm, 1.8mm, 1.5mm, 1.2mm, 1mm, 0.75mm or 0.5mm, and the like, but is not limited to the values recited and other values not recited within the range of values are equally applicable.
Preferably, the solid-to-liquid ratio of the plant material to the extraction solvent is 1 (5-50) g/mL, for example, 1:5g/mL, 1:10g/mL, 1:15g/mL, 1:20g/mL, 1:25g/mL, 1:30g/mL, 1:40g/mL, or 1:50g/mL, but is not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the extraction solvent comprises water and/or an organic solvent.
Preferably, the organic solvent comprises any one of methanol, ethanol or N, N-dimethylformamide or a combination of at least two of these, typical but non-limiting examples being: a combination of methanol and ethanol, a combination of ethanol and N, N-dimethylformamide, a combination of methanol, ethanol and N, N-dimethylformamide, and the like.
As a preferred technical solution of the present invention, the mixing of the plant material and the extraction solvent is performed in a material mixing device.
Preferably, the material mixing device is jacketed at-110-120 deg.C, such as-110 deg.C, -80 deg.C, -60 deg.C, -40 deg.C, -20 deg.C, 0 deg.C, 20 deg.C, 40 deg.C, 60 deg.C, 80 deg.C, 100 deg.C or 120 deg.C, but not limited to the recited values, and other values not recited in the range of the recited values are also applicable.
In the invention, the control of the material mixing temperature needs to integrate various factors, the types of the plants to be extracted and the active ingredients, the selection of the solvent type and the like, and other conditions, such as equipment, materials, heat exchange media and the like, also need to meet the temperature requirement, so that the operation can be normally carried out.
Preferably, the temperature of the jacket is controlled to heat or cool the material.
Preferably, the heating mode comprises any one of steam heating, circulating water bath heating, circulating oil bath heating or a heating rod arranged in the heating sleeve.
Preferably, the cooling mode comprises any one of refrigerating by a refrigerator, refrigerating by liquid nitrogen or refrigerating by an organic solvent refrigerant.
In a preferred embodiment of the present invention, the pressure of the high-pressure extraction is 1 to 20MPa, for example, 1MPa, 2MPa, 5MPa, 8MPa, 10MPa, 12MPa, 15MPa, 18MPa, or 20MPa, but the pressure is not limited to the above-mentioned values, and other values not listed in the above-mentioned range are also applicable.
Preferably, the high pressure extraction is performed for 1-30 min, such as 1min, 2min, 5min, 10min, 15min, 20min, 25min, or 30min, but not limited to the recited values, and other values not recited in the range of values are also applicable.
As the preferable technical scheme of the invention, the material after high-pressure extraction is injected into the decompression circulation equipment under reduced pressure.
Preferably, the pressure in the reduced-pressure circulation device is normal pressure.
Preferably, the number of extraction cycles is at least 1, such as 1, 2, 4, 6, 8, or 10, but not limited to the recited values, and other values not recited within the range are equally applicable.
In the invention, the extraction solution is changed from high-pressure extraction equipment to reduced-pressure circulation equipment from high-pressure condition to normal pressure, the effective components are further extracted from the plant raw materials by utilizing rapid pressure difference change, and the separation effect of the materials and the extraction solvent is enhanced.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the jet extraction device, the dissolution rate of effective components in the plant raw materials is improved by adopting a high-pressure extraction mode, and the solid-liquid extraction effect between the plant raw materials and the extraction solvent is enhanced;
(2) the decompression process after the high-pressure extraction can strengthen the material exchange process, and the dissolved effective components are better brought into the main body of the solvent, so that the solid-liquid extraction process is further strengthened, and the aim of efficiently extracting the effective components is fulfilled;
(3) the device disclosed by the invention is simple in structure, simple and convenient in process operation, green and environment-friendly, and is beneficial to popularization of large-scale production.
Drawings
FIG. 1 is a schematic view of structural connection of a jet extraction device provided in example 1 of the present invention;
FIG. 2 is a schematic structural diagram of a material mixing apparatus provided in embodiment 1 of the present invention;
FIG. 3 is a schematic structural view of a high-pressure extraction apparatus provided in embodiment 1 of the present invention;
FIG. 4 is a schematic structural view of a pressure reducing cycle apparatus provided in example 1 of the present invention;
FIG. 5 is a schematic structural diagram of a material mixing apparatus provided in embodiment 2 of the present invention;
the device comprises a material mixing device 1, a temperature control jacket 11, an energy-gathering ultrasonic transducer 12, a divergence ultrasonic transducer 13, a pressurization device 2, a high-pressure extraction device 3, a pressure detection device 31, a pressure reduction circulation device 4, a sight glass 41 and a heat source device 5.
Detailed Description
In order to better illustrate the present invention and facilitate the understanding of the technical solutions of the present invention, the present invention is further described in detail below. However, the following examples are only simple examples of the present invention and do not represent or limit the scope of the present invention, which is defined by the claims.
The invention provides a jet flow extraction device and an application method thereof, the jet flow extraction device comprises a material mixing device 1, a pressurizing device 2, a high-pressure extraction device 3 and a pressure reduction circulating device 4 which are sequentially connected, and an outlet of the pressure reduction circulating device 4 is connected with an inlet of the material mixing device 1.
The application method comprises the following steps:
mixing the plant material and the extraction solvent, pressurizing by a pressurizing device 2, performing high-pressure extraction, and performing cyclic extraction or discharge after pressure reduction and injection.
The following are typical but non-limiting examples of the invention:
example 1:
the embodiment provides a jet extraction device, the structural schematic diagram of which is shown in fig. 1, and the jet extraction device comprises a material mixing device 1, a supercharging device 2, a high-pressure extraction device 3 and a decompression circulation device 4 which are connected in sequence, wherein an outlet of the decompression circulation device 4 is connected with an inlet of the material mixing device 1.
The structure schematic diagram of the material mixing device 1 is shown in fig. 2, a stirring component is arranged in the material mixing device, and a temperature control jacket 11 is arranged outside the material mixing device.
The temperature control jacket 11 is also connected with a heat source device 5.
And an energy-gathering type ultrasonic transducer 12 is also arranged in the material mixing equipment 1.
The pressure boosting device 2 is a high-pressure delivery pump.
The structural schematic diagram of the high-pressure extraction device 3 is shown in fig. 3, and the interior is closed and hollow; the high-pressure extraction equipment 3 is provided with a pressure detection device 31; the pressure detection device 31 is a piezoelectric pressure sensor in an electrical measuring pressure measuring instrument.
And a pressure reducing device is arranged at an outlet of the high-pressure extraction equipment 3, and the pressure reducing device is a film type pressure reducing valve.
The structure schematic diagram of the decompression circulation equipment 4 is shown in fig. 4, and the connecting pipeline of the decompression circulation equipment 4 and the material mixing equipment 1 is a circulation pipeline.
The pressure reduction circulation equipment 4 is also connected with an outlet pipeline parallel to the circulation pipeline.
The decompression circulation device 4 is provided with a sight glass 41.
A washing pipeline is arranged between the outlet of the pressure increasing device 2 and the outlet of the pressure reducing circulating device 4.
Example 2:
this embodiment provides a efflux extraction element, efflux extraction element is including the material mixing apparatus 1, supercharging device 2, high pressure extraction equipment 3 and the decompression circulating equipment 4 that connect gradually, the export of decompression circulating equipment 4 links to each other with the entry of material mixing apparatus 1.
The structural schematic diagram of the material mixing device 1 is shown in fig. 5, a stirring component is arranged in the material mixing device, and a temperature control jacket 11 is arranged outside the material mixing device.
The temperature control jacket 11 is also connected with a heat source device 5.
The material mixing device 1 is simultaneously provided with an energy-gathering ultrasonic transducer 12 and a dispersive ultrasonic transducer 13.
The pressure boosting device 2 is a high-pressure delivery pump.
The interior of the high-pressure extraction equipment 3 is closed and hollow; the high-pressure extraction equipment 3 is provided with a pressure detection device 31; the pressure detection device 31 is an elastic pressure measuring instrument.
And a pressure reducing device is arranged at an outlet of the high-pressure extraction equipment 3, and the pressure reducing device is a piston type pressure reducing valve.
And a circulating pump is arranged on a connecting pipeline of the pressure reduction circulating equipment 4 and the material mixing equipment 1.
The pressure reduction circulation equipment 4 is also connected with an outlet pipeline parallel to the circulation pipeline.
The pressure reduction circulation equipment 4 is provided with a sight glass 41; and a jacket is arranged on the decompression circulating equipment 4.
Application example 1:
this application example provides a method for extracting anthocyanin from lycium ruthenicum by using the jet extraction device in example 1, and the method comprises the following steps:
crushing lycium ruthenicum raw materials, mixing with 0.01 wt% citric acid aqueous solution as an extraction solvent, extracting anthocyanin, and changing pressure, feed liquid ratio and extraction time under the condition of normal temperature; filtering and centrifuging after extraction to obtain the lycium ruthenicum extracting solution.
The determination method of anthocyanin is as follows:
and (3) testing by adopting a pH differential method, preparing buffer solutions with pH values of 1.0 and 4.5 respectively, measuring 0.5mL of lycium ruthenicum anthocyanin solution, adding buffer solutions with pH values of 1.0 and 4.5 respectively, standing at room temperature for 30 minutes, and measuring the light absorption value A of the lycium ruthenicum anthocyanin in the two buffer solutions at the wavelengths of 530nm and 700nm respectively.
The calculation formula of the anthocyanin content of the lycium ruthenicum comprises the following steps:
Figure BDA0002687748420000101
Figure BDA0002687748420000111
Figure BDA0002687748420000112
in the formula, delta A is an absorbance difference; mw is cyanidin-3-glucoside molecular weight (449.2); DF is the dilution factor; the molar extinction coefficient of cyanidin-3-glucoside (26900L/(mol cm)); l is the optical distance (1cm) of the cuvette; c is the anthocyanin concentration (g/mL) of the lycium ruthenicum in the solution to be detected; v is solution volume (mL); m is the weight (g) of the dried lycium ruthenicum; and Y is the anthocyanin yield of the dried lycium ruthenicum murr.
Comparative application example 1:
the comparative application example provides a method for extracting anthocyanin from lycium ruthenicum by adopting an ultrasonic extraction method, the used extraction solvent, the material-liquid ratio and the extraction time are the same as those of the application example 1, and the difference is only that: the extraction pressure is replaced with ultrasonic power.
The determination method of anthocyanin in the lycium ruthenicum extracting solution is the same as the application example 1.
The extraction process conditions and extraction results in application example 1 and comparative application example 1 are shown in table 1.
Table 1 comparative table of extraction process conditions and extraction results in application example 1 and comparative application example 1
Figure BDA0002687748420000113
Figure BDA0002687748420000121
As can be seen from table 1, the extraction effect of the high-pressure jet extraction provided by the present invention is superior to that of the ultrasonic extraction technique according to the lateral comparison between the same experimental numbers.
Application example 2:
the application example provides a method for extracting phenylethanoid glycosides from cistanche deserticola by adopting the jet flow extraction device in the embodiment 1, and the method comprises the following steps:
crushing cistanche raw materials, taking 50% ethanol as an extraction solvent, mixing, extracting phenylethanoid glycosides, selecting a material-liquid ratio of 1:20g/mL under the condition of normal temperature, and changing pressure and extraction time; after extraction, filtering and centrifuging to obtain an extracting solution.
Because the representative components of the phenylethanoid glycosides in the cistanche are echinacoside and verbascoside, the contents of the echinacoside and the verbascoside in the extracting solution can be detected, and the contents of the echinacoside and the verbascoside are used as phenylethanoid glycoside total glycosides for calculation;
the detection method comprises the following steps: adopting a Shimadzu HPLC-20AT high performance liquid chromatography workstation, and the chromatographic conditions are as follows: waters XTerra C18 column (4.6 mm. times.250 mm, 5 μm); the mobile phase A is aqueous formic acid (0.2 percent) and the mobile phase B is acetonitrile; the gradient elution procedure was as follows: the proportion of B is changed in turn, and is 14% in 0-23 min; 14-17% in 23-24 min; 17% in 24-35 min; 17-20% in 35-60 min; 20% in 60-65 min; the detection wavelength is 330nm, the flow rate is 0.8mL/min, the temperature is 30 ℃, and the injection volume is 10 mu L. The contents of echinacoside and verbascoside were calculated separately using the following established standard equations:
Y＝574395X-734
wherein Y is the area of the peak and X is the concentration of echinacoside (mg/mL); r2＝0.9991。
Y＝954629X+747.7
Wherein Y is the area of the peak and X is the concentration of verbascoside (mg/mL); r2＝0.9995。
Comparative application example 2:
this comparison application example provides a method for extracting phenylethanoid glycosides from cistanche deserticola by adopting a hot reflux extraction method, the used extraction solvent, feed liquid ratio and extraction time are the same as those of application example 2, and the differences are only that: the extraction pressure is replaced by the extraction temperature.
The method for measuring anthocyanin in the obtained cistanche extracting solution is the same as the application example 2.
The extraction process conditions and extraction results in application example 2 and comparative application example 2 are shown in table 2.
Table 2 comparative table of extraction process conditions and extraction results in application example 2 and comparative application example 2
Figure BDA0002687748420000131
As can be seen from Table 2, the extraction effect of the high-pressure jet extraction provided by the present invention is superior to that of the hot reflux extraction technique according to the lateral comparison between the same experimental numbers.
Application example 3:
the present application example provides a method of extracting cannabidiol from industrial cannabis using the jet extraction device of example 1, the method comprising:
pulverizing hemp flowers and leaves, mixing with methanol as an extraction solvent, extracting cannabidiol, selecting a material-liquid ratio of 1:20g/mL under the condition of normal temperature, and changing pressure and extraction time; after extraction, filtering and centrifuging to obtain an extracting solution.
The cannabidiol detection method comprises the following steps: adopting a Shimadzu HPLC-20AT high performance liquid chromatography workstation, and the chromatographic conditions are as follows: waters XTerra C18 column (4.6 mm. times.250 mm, 5 μm); mobile phase a was aqueous acetic acid (0.1%), B was acetonitrile, a: B ═ 25: 75; the detection wavelength is 220nm, the flow rate is 0.8mL/min, the temperature is 25 ℃, and the injection volume is 10 mu L. And calculating the extraction effect of the cannabidiol according to the peak area.
Comparative application example 3:
this comparison application example provides a method for extracting cannabidiol from industrial hemp by using a thermal reflux extraction method, and the used extraction solvent, feed liquid ratio and extraction time are the same as those of application example 3, and the differences are only that: the extraction pressure is replaced by the extraction temperature.
The method for measuring cannabidiol in the obtained cannabis sativa extract was the same as in application example 3.
The extraction process conditions and extraction results in application example 3 and comparative application example 3 are shown in table 3.
Table 3 comparative table of extraction process conditions and extraction results in application example 3 and comparative application example 3
Figure BDA0002687748420000141
As can be seen from Table 3, the extraction effect of the high-pressure jet extraction provided by the present invention is superior to that of the hot reflux extraction technique based on the lateral comparison between the same experimental numbers.
Application example 4:
the present application example provides a method of extracting cannabis polysaccharide from industrial cannabis using the jet extraction device of example 1, the method comprising:
the method comprises the steps of mixing hemp leaf residue powder and water as an extraction solvent, extracting hemp polysaccharide, selecting a material-liquid ratio of 1:20g/mL under the condition of normal temperature, and changing pressure and extraction time; after extraction, filtering and centrifuging to obtain an extracting solution.
The detection method of the content of the hemp polysaccharide comprises the following steps: weighing 2.0mL of liquid to be detected, adding 1.0mL of 6% phenol and 5.0mL of concentrated sulfuric acid, standing for 10min, shaking, standing at room temperature for 20min, measuring optical density at 490nm, using 2.0mL of water as blank according to the same color development operation, and calculating the extraction rate of cannabis sativa polysaccharide according to the optical density value.
Comparative application example 4:
this comparative application example provides a method for extracting hemp polysaccharide from industrial hemp by using a thermal reflux extraction method, and the used extraction solvent, feed liquid ratio and extraction time are the same as those of application example 4, and the differences are only that: the extraction pressure is replaced by the extraction temperature.
The method for measuring cannabis polysaccharide in the obtained cannabis extract was the same as in application example 4.
The extraction process conditions and extraction results in application example 4 and comparative application example 4 are shown in table 4.
Table 4 comparative table of extraction process conditions and extraction results in application example 4 and comparative application example 4
Figure BDA0002687748420000151
As can be seen from Table 4, the extraction effect of the high-pressure jet extraction provided by the present invention is superior to that of the hot reflux extraction technique based on the lateral comparison between the same experimental numbers.
Application example 5:
this application example provides a method for extracting phillyrin from forsythia suspensa using the jet extraction apparatus of example 2, the method including:
taking fructus forsythiae powder as a raw material, taking 60% ethanol as an extraction solvent, mixing, extracting phillyrin, and sampling and detecting at different times under the conditions of 50 ℃, the material-liquid ratio of 1:20g/mL and the pressure of 15 MPa; after extraction, filtering and centrifuging to obtain an extracting solution.
The phillyrin detection method comprises the following steps: measuring absorbance values at 229nm, and determining phillyrin content by taking the mass concentration (mg/mL) of phillyrin standard solution as abscissa.
Comparative application example 5:
the comparative application example provides a method for extracting phillyrin from forsythia suspense by adopting a hot reflux extraction method, and the conditions of the used extraction solvent, the material-liquid ratio, the extraction temperature and the pressure are the same as those of the application example 5.
The determination method of phillyrin in the obtained forsythia suspense extract is the same as that of application example 5.
The extraction results in application example 5 and comparative application example 5 are shown in table 5.
Table 5 comparative table of extraction results in application example 5 and comparative application example 5
Figure BDA0002687748420000161
As can be seen from Table 5, the high pressure jet extraction provided by the present invention is superior to the hot reflux extraction technique in terms of the lateral comparison between the same experimental numbers.
Application example 6:
this application example provides a method for extracting phillyrin from forsythia suspense leaves using the jet extraction apparatus of example 2, the method including:
taking a forsythia suspense leaf raw material and 60% ethanol as an extraction solvent, mixing, extracting phillyrin, and sampling and detecting at different times under the condition of 50 ℃ and under the conditions that the material-liquid ratio is 1:25g/mL and the pressure is 15 MPa; after extraction, filtering and centrifuging to obtain an extracting solution.
The phillyrin detection method comprises the following steps: measuring absorbance values at 229nm, and determining phillyrin content by taking the mass concentration (mg/mL) of phillyrin standard solution as abscissa.
Comparative application example 6:
the comparative application example provides a method for extracting phillyrin from forsythia suspense leaves by adopting a thermal reflux extraction method, and the conditions of an extraction solvent, a material-liquid ratio, an extraction temperature and extraction pressure are the same as those of the application example 6.
The method for measuring phillyrin in the obtained phillyrin leaf extract was the same as in application example 6.
The extraction results in application example 6 and comparative application example 6 are shown in table 6.
Table 6 comparison table of extraction results in application example 6 and comparative application example 6
Figure BDA0002687748420000171
As can be seen from table 6, the extraction effect of the high-pressure jet extraction provided by the present invention is superior to that of the hot reflux extraction technique according to the lateral comparison between the same experimental numbers.
Application example 7:
this application example provides a method of extracting lycium barbarum polysaccharides from lycium barbarum using the jet extraction device of example 2, the method comprising:
crushing a Chinese wolfberry raw material, taking water as an extraction solvent, mixing, extracting Chinese wolfberry polysaccharide, and performing sampling detection at different times under the condition of 50 ℃ and under the conditions that the material-liquid ratio is 1:20g/mL and the pressure is 15 MPa; after extraction, filtering and centrifuging to obtain an extracting solution.
The method for detecting the content of the lycium barbarum polysaccharide comprises the following steps: weighing 2.0mL of liquid to be detected, adding 1.0mL of 6% phenol and 5.0mL of concentrated sulfuric acid, standing for 10min, shaking, standing at room temperature for 20min, measuring optical density at 490nm, using 2.0mL of water as blank according to the same color development operation, and calculating polysaccharide extraction rate according to optical density value.
Comparative application example 7:
the comparative application example provides a method for extracting lycium barbarum polysaccharide from lycium barbarum by adopting a thermal reflux extraction method, and the used extraction solvent, material-liquid ratio, extraction temperature and pressure conditions are the same as those of application example 7.
The method for measuring the lycium barbarum polysaccharide in the obtained lycium barbarum extract is the same as in application example 7.
The extraction results in application example 7 and comparative application example 7 are shown in table 7.
Table 7 comparative table of extraction results in application example 7 and comparative application example 7
Figure BDA0002687748420000181
As can be seen from table 7, the extraction effect of the high-pressure jet extraction provided by the present invention is superior to the hot reflux extraction technique according to the lateral comparison between the same experimental numbers.
Application example 8:
this application example provides a method for extracting jasminoidin and crocin from gardenia by using the jet extraction device in example 2, which includes:
pulverizing fructus Gardeniae raw material, mixing with 70% ethanol as extraction solvent, extracting, and sampling at 50 deg.C under 15MPa at a ratio of 1:15 g/mL; after extraction, filtering and centrifuging to obtain an extracting solution.
The detection method of the content of the geniposide and the crocin comprises the following steps: c18 bonded silica gel column (4.6 mm. times.250 mm, 5 μm); mobile phase: acetonitrile (a) -0.1% aqueous phosphoric acid; gradient elution: 0-15 min (10% -18% A), 15-20 min (18% -28% A), 20-40 min (28% -38% A), 40-41 min (38% -95% A), 41-50 min (95% -95% A), 50-51 min (95% -10% A), 51-60 min (10% -10% A); the detection wavelength is 238nm for geniposide, 440nm for crocin, the column oven is 25 deg.C, and the flow rate is 1 mL/min.
Comparative application example 8:
the comparative application example provides a method for extracting geniposide and crocin from gardenia by adopting a thermal reflux extraction method, and the conditions of the used extraction solvent, the material-liquid ratio, the extraction temperature and the extraction pressure are the same as those of the application example 8.
The determination method of geniposide and crocin in the obtained gardenia extract is the same as that of application example 8.
The extraction results in application example 8 and comparative application example 8 are shown in table 8.
Table 8 comparative table of extraction results in application example 8 and comparative application example 8
Figure BDA0002687748420000201
As can be seen from table 8, the extraction effect of the high-pressure jet extraction provided by the present invention is superior to the hot reflux extraction technique according to the lateral comparison between the same experimental numbers.
Application example 9:
the present application example provides a method of extracting curcumin from turmeric using the jet extraction device of example 2, the method comprising:
pulverizing Curcuma rhizome raw material, extracting with 70% ethanol as extraction solvent, mixing, and sampling at 50 deg.C under 15MPa at a ratio of 1:40 g/mL; after extraction, filtering and centrifuging to obtain an extracting solution.
The curcumin detection method comprises the following steps: c18 bonded silica gel column (4.6 mm. times.250 mm, 5 μm); mobile phase: 85% methanol water solution with flow rate of 1mL/min, column oven 25 deg.C, detection wavelength of 420nm, and sample injection amount of 20 μ L.
Comparative application example 9:
the comparative application example provides a method for extracting curcumin from turmeric by adopting a thermal reflux extraction method, and the conditions of the used extraction solvent, the material-liquid ratio, the extraction temperature and the pressure are the same as those of the application example 9.
The method for measuring curcumin in the obtained turmeric extract was the same as in application example 9.
The extraction results in application example 9 and comparative application example 9 are shown in table 9.
Table 9 comparative table of extraction results in application example 9 and comparative application example 9
Figure BDA0002687748420000211
As can be seen from table 9, the extraction effect of the high pressure jet extraction provided by the present invention is superior to the hot reflux extraction technique based on the lateral comparison between the same experimental numbers.
Application example 10:
the present application example provides a method for extracting asparagus saponin from asparagus by using the jet extraction device in embodiment 2, the method comprising:
pulverizing Germinatus Phragmitis, extracting with 80% ethanol as extraction solvent, mixing, and sampling at 50 deg.C under 15MPa at a ratio of 1:20 g/mL; after extraction, filtering and centrifuging to obtain an extracting solution.
The asparagus total saponin is detected by adopting a vanillin-glacial acetic acid solution method as follows: precisely sucking 400 mu L of asparagus saponin standard substance and sample with different concentrations, and volatilizing the solvent in 70 ℃ water bath; preparing 5% vanillin-glacial acetic acid solution (0.5g vanillin, using glacial acetic acid to fix the volume to 10mL), adding 200 μ L5% vanillin-glacial acetic acid solution and 800 μ L perchloric acid, performing 70 deg.C water bath for 15min, taking out, and cooling to room temperature. Adding 5mL of glacial acetic acid, detecting the absorbance at 540nm, and determining the content of the total saponin according to the obtained saponin standard curve.
Comparative application example 10:
the comparative application example provides a method for extracting asparagus saponin from asparagus by adopting a hot reflux extraction method, and the conditions of the used extraction solvent, the material-liquid ratio, the extraction temperature and the pressure are the same as those of the application example 10.
The determination method of the asparagus saponin in the obtained asparagus extract is the same as the application example 10.
The extraction results in application example 10 and comparative application example 10 are shown in table 10.
Table 10 comparative table of extraction results in application example 10 and comparative application example 10
Figure BDA0002687748420000221
As can be seen from table 10, the extraction effect of the high-pressure jet extraction provided by the present invention is superior to that of the hot reflux extraction technique according to the lateral comparison between the same experimental numbers.
By combining the embodiment and the application example, the jet extraction device disclosed by the invention improves the dissolution rate of the effective components in the plant raw materials by adopting a high-pressure extraction mode, and enhances the solid-liquid extraction effect between the plant raw materials and the extraction solvent; the decompression process after high-pressure extraction can strengthen the material exchange process, and the dissolved effective components are better brought into the main body of the solvent, so that the solid-liquid extraction process is further strengthened, and the aim of efficiently extracting the effective components is fulfilled; the device has the advantages of simple structure, simple and convenient process operation, greenness and environmental protection, and is beneficial to popularization of large-scale production.
The applicant states that the present invention is illustrated by the detailed apparatus and method of the present invention through the above embodiments, but the present invention is not limited to the above detailed apparatus and method, i.e. it is not meant to imply that the present invention must be implemented by the above detailed apparatus and method. It will be apparent to those skilled in the art that any modifications to the present invention, equivalents of the means for substitution and addition of means for carrying out the invention, selection of specific means, etc., are within the scope and disclosure of the invention.

Claims (10)

1. The jet extraction device is characterized by comprising material mixing equipment, supercharging equipment, high-pressure extraction equipment and pressure reduction circulating equipment which are sequentially connected, wherein an outlet of the pressure reduction circulating equipment is connected with an inlet of the material mixing equipment.
2. The jet extraction device of claim 1, wherein the material mixing apparatus is provided with a stirring assembly inside and a temperature control jacket outside;
preferably, the temperature control jacket is also connected with a heat source device.
3. The jet extraction device of claim 1 or 2, wherein an ultrasonic generation device is further arranged in the material mixing device;
preferably, the ultrasound generating device comprises a focused ultrasound transducer and/or a divergent ultrasound transducer;
preferably, the number of ultrasound generating devices is at least one;
preferably, the energy concentrating ultrasonic transducer and the diverging ultrasonic transducer are arranged separately or together.
4. The jet extraction apparatus of any one of claims 1 to 3, wherein the pressurising means comprises a high pressure delivery pump;
preferably, the high-pressure extraction equipment is closed and hollow;
preferably, a pressure detection device is arranged on the high-pressure extraction equipment;
preferably, the pressure detection device comprises any one of an elastic pressure measuring instrument, an electrical pressure measuring instrument or a load pressure measuring instrument;
preferably, the electrically-measured pressure measuring instrument comprises a pressure sensor, the pressure sensor comprising any one of a piezoelectric pressure sensor, a resistive pressure sensor, a capacitive pressure sensor or a strain gauge pressure sensor;
preferably, a pressure reducing device is arranged at an outlet of the high-pressure extraction equipment;
preferably, the pressure reducing means comprises a pressure reducing valve;
preferably, the pressure reducing valve comprises any one of a piston type pressure reducing valve, a diaphragm type pressure reducing valve or a direct acting type pressure reducing valve.
5. The jet extraction apparatus of any one of claims 1 to 4, wherein a circulation pump is provided on a connection pipe between the pressure reduction circulation device and the material mixing device;
preferably, the decompression circulating equipment is also connected with an outlet pipeline which is parallel to the circulating pipeline;
preferably, a sight glass is arranged on the decompression circulating equipment;
preferably, the decompression circulating equipment is provided with a jacket.
6. Method of application of the jet extraction device according to any one of claims 1 to 5, characterized in that it comprises:
mixing the plant material and the extraction solvent, pressurizing by a pressurizing device, performing high-pressure extraction, and performing cyclic extraction or discharge after pressure reduction and injection.
7. The use method as claimed in claim 6, wherein the plant material comprises any one or combination of at least two of Lycium ruthenicum Murr, Cistanchis herba, Industrial hemp, Asparagus officinalis, forsythiae fructus, Gardeniae fructus, Lycii fructus or Curcuma rhizome;
preferably, the plant material is first crushed and then mixed with an extraction solvent;
preferably, the plant material is crushed to a particle size of no more than 2 mm;
preferably, the solid-liquid ratio of the plant raw material to the extraction solvent is 1 (5-50) g/mL;
preferably, the extraction solvent comprises water and/or an organic solvent;
preferably, the organic solvent comprises any one of methanol, ethanol or N, N-dimethylformamide or a combination of at least two thereof.
8. The use of the method according to claim 6 or 7, wherein the mixing of the plant material with the extraction solvent is performed in a material mixing device;
preferably, the temperature of the material mixing equipment is controlled to be-110-120 ℃ by a jacket;
preferably, the temperature of the jacket is controlled by heating or cooling the material;
preferably, the heating mode comprises any one of steam heating, circulating water bath heating, circulating oil bath heating or heating rod arranged in the heating sleeve;
preferably, the cooling mode comprises any one of refrigerating by a refrigerator, refrigerating by liquid nitrogen or refrigerating by an organic solvent refrigerant.
9. The use of any one of claims 6 to 8, wherein the pressure of the high pressure extraction is 1 to 20 MPa;
preferably, the time of the high-pressure extraction is 1-30 min.
10. The use of any one of claims 6 to 9, wherein the high pressure extracted material is injected under reduced pressure into a pressure reduction circulation device;
preferably, the pressure in the reduced-pressure circulation equipment is normal pressure;
preferably, the number of said cyclic extractions is at least 1.
CN202010981685.8A 2020-09-17 2020-09-17 Jet flow extraction device and application method thereof Pending CN112023440A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114163642A (en) * 2021-12-21 2022-03-11 富海(东营)新材料科技有限公司 Energy-saving and environment-friendly purification process and purification equipment for polysulfone resin

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114163642A (en) * 2021-12-21 2022-03-11 富海(东营)新材料科技有限公司 Energy-saving and environment-friendly purification process and purification equipment for polysulfone resin
CN114163642B (en) * 2021-12-21 2023-08-15 富海(东营)新材料科技有限公司 Purification process and purification equipment of energy-saving environment-friendly polysulfone resin

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