CN212395943U - High-pressure circulation extraction element - Google Patents
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- CN212395943U CN212395943U CN202022043861.1U CN202022043861U CN212395943U CN 212395943 U CN212395943 U CN 212395943U CN 202022043861 U CN202022043861 U CN 202022043861U CN 212395943 U CN212395943 U CN 212395943U
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Abstract
The utility model provides a high pressure circulation extraction element, high pressure circulation extraction element is including the material mixing equipment, high-pressure delivery pump, the high pressure extraction equipment and the decompression circulating equipment that connect gradually, the export of decompression circulating equipment links to each other with the entry of material mixing equipment. The high-pressure circulation extraction device of the utility model improves the dissolution rate of 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.
Description
Technical Field
The utility model belongs to the technical field of the plant composition draws, a high pressure circulation extraction element is related to.
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.
SUMMERY OF THE UTILITY MODEL
Problem to prior art existence, the utility model aims to provide a high pressure circulation extraction element, high pressure circulation extraction element strengthens the plant material and draws the solid-liquid extraction effect between the solvent through the mode that adopts high pressure to draw, strengthens separation effect between the two through the decompression process again to improve plant active ingredient's extraction efficiency, simplify and draw technology, reduce cost.
To achieve the purpose, the utility model adopts the following technical proposal:
the utility model provides a high-pressure circulation extraction device, which comprises a material mixing device, a high-pressure delivery pump, a high-pressure extraction device and a decompression circulation device which are connected in sequence, wherein the outlet of the decompression circulation device is connected with the inlet of the material mixing device; and an ultrasonic generating device is arranged in the material mixing device.
In the utility model, because the effective constituent often exists in cell and organelle in the plant, will draw out and need experience complicated mass transfer process, therefore draw the technique and need improve the penetrability of cell membrane and cell wall or even broken cell usually, the device utilizes the mixture of raw materials and solvent, pressure boost, draws, decompression process, accomplishes an extraction cycle, utilizes supersound, high pressure condition to destroy the integrality of cell, makes the effective constituent wherein dissolve out, still mainly exists in cell or tissue clearance, nevertheless through quick decompression, utilizes the inside and outside great pressure differential of cell, strengthens the material exchange process, better brings into the solvent main part the effective constituent that dissolves out, improves 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.
Following conduct the utility model discloses preferred technical scheme, nevertheless do not conduct the utility model provides a technical scheme's restriction, through following technical scheme, can reach and realize better the utility model discloses a technical purpose and beneficial effect.
As the utility model discloses preferred technical scheme, the inside of material mixing equipment is equipped with the stirring subassembly, and the outside is equipped with the control by temperature change and presss from both sides the cover.
The utility model discloses in, because active ingredient's difference in the plant, its suitable extraction temperature also can be different, and active ingredient's performance often receives the temperature to influence great, therefore the extraction temperature need be controlled, can control the temperature of mixing material when plant material mixes with the solvent, adopts the mode that the accuse temperature pressed from both sides the cover, and for the flash mixed, generally need stir, can accomplish preliminary extraction process.
Preferably, the ultrasound generating device comprises a focused ultrasound transducer and/or a divergent ultrasound transducer.
The utility model discloses in, utilize ultrasonic acoustic energy can broken cell, dissolve its active ingredient with higher speed, promote the diffusion of active ingredient, therefore assist the supersound condition at the material mixing in-process, can enough accelerate the dispersion of plant material and mix, also can tentatively accomplish the preliminary destruction of cell, help subsequent high pressure to draw.
The utility model discloses in, in the high pressure delivery pump carries the high pressure extraction equipment with the combined material to constantly improve the pressure in this equipment, carry out the pressurize after reaching required pressure.
Preferably, the high pressure extraction device is hermetically hollow.
Preferably, a pressure gauge is arranged on the high-pressure extraction equipment.
Preferably, a pressure reducing valve is arranged at an outlet of the high-pressure extraction device.
The utility model discloses in, in order to maintain the pressure of drawing equipment, need set up to airtight condition, and set up the pressure in the manometer real-time supervision equipment, reach high pressure and draw the time back, open the valve in exit, reduce pressure fast, utilize pressure differential can spray out the material and get into decompression circulating equipment, the great pressure differential of this process also can be utilized simultaneously reaches the purpose of further drawing.
The utility model discloses in, the material selection of high pressure extraction equipment needs can bear the high pressure condition, need be greater than maximum extraction pressure at least, according to the utility model discloses well extraction pressure's selection, the design pressure that the equipment material can tolerate 20MPa at least, for example 20MPa, 22MPa, 24MPa, 26MPa, 28MPa or 30MPa etc. but not limited only to the numerical value enumerated, other numerical values not enumerated in this numerical value range are equally suitable.
As the utility model discloses preferred technical scheme, be equipped with the circulating pump on decompression circulating equipment and material mixing apparatus's the connecting pipeline.
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 utility model, the pressure reduction circulation equipment is in a normal pressure environment, the surface of the equipment is provided with the sight glass, and the internal condition is observed, and the pressure reduction circulation equipment has the functions of temporarily storing the 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.
The utility model discloses in, it has a pipeline still directly to link between the export of high-pressure delivery pump and the export of decompression circulating equipment, is equipped with the valve on it, and through the material circulation among the material mixing apparatus, can realize that the circulation under the ordinary pressure state draws.
As the utility model discloses preferred technical scheme, high pressure circulation extraction element still includes integrated control ware, integrated control ware independently links to each other with material mixing apparatus, high-pressure delivery pump, high pressure extraction equipment and decompression circulating equipment.
The utility model discloses in, integrated control ware is as the holistic control module of device, carries out integrated control to processes such as the switching of the operation of pressing from both sides cover temperature control, delivery pump, valve.
The utility model also provides an application method of above-mentioned high pressure circulation extraction element, application method includes:
mixing the plant material and the extraction solvent, pressurizing by a high-pressure delivery pump, performing high-pressure extraction, and performing cyclic extraction or discharge after pressure reduction and injection.
As a preferred technical solution 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, but not limited to the values recited, and other values not recited within this range 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 the preferred technical scheme of the utility model, the mixing of plant material and extraction solvent is carried out in material mixing equipment.
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.
The utility model discloses in, many-sided factor is synthesized to material mixing temperature's control needs, treats to extract plant and active ingredient's kind, solvent kind's selection etc. other each side condition, also should satisfy the temperature requirement like equipment, material, heat transfer medium etc. makes this operation can normally go on.
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 values listed, and other values not listed in the numerical 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 utility model discloses preferred technical scheme, the material decompression after the high pressure is drawed is sprayed and is got into decompression circulating equipment.
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.
The utility model discloses in, the extract is followed high pressure and is drawed equipment to decompression circulating equipment, becomes the ordinary pressure from the high pressure condition, utilizes the quick pressure differential change further to draw effective constituent from the plant material to strengthen the material and draw the separation effect of solvent.
Compared with the prior art, the utility model discloses following beneficial effect has:
(1) the high-pressure circulation extraction device of the utility model improves the dissolution rate of 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;
(2) the decompression process after the high-pressure extraction of the utility model can strengthen the material exchange process, and the dissolved effective components are better brought into the main body of the solvent, thereby further strengthening the solid-liquid extraction process and realizing the purpose of efficiently extracting the effective components;
(3) device simple structure, technology is easy and simple to handle, and green is favorable to the popularization of scale production.
Drawings
Fig. 1 is a schematic structural connection diagram of a high-pressure circulation extraction device provided in embodiment 1 of the present invention;
fig. 2 is a schematic structural diagram of a material mixing device provided in embodiment 1 of the present invention;
fig. 3 is a schematic structural diagram of a high-pressure extraction device provided in embodiment 1 of the present invention;
fig. 4 is a schematic structural diagram of a pressure reduction cycle apparatus provided in embodiment 1 of the present invention;
fig. 5 is a schematic structural diagram of a material mixing device 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 high-pressure delivery pump 2, a high-pressure extraction device 3, a pressure gauge 31, a pressure reduction circulating device 4, a sight glass 41, an integrated controller 5 and a circulating pump 6.
Detailed Description
To better explain the utility model, the technical proposal of the utility model is convenient to understand, and the utility model is further explained in detail below. However, the following embodiments 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 appended claims.
The utility model discloses embodiment mode part provides a high pressure circulation extraction element, high pressure circulation extraction element is including the material mixing apparatus 1, high-pressure delivery pump 2, the 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 following are typical but non-limiting examples of the present invention:
example 1:
the embodiment provides a high-pressure circulation extraction device, the structural schematic diagram of which is shown in fig. 1, and the high-pressure circulation extraction device comprises a material mixing device 1, a high-pressure delivery pump 2, a high-pressure extraction device 3 and a pressure reduction circulation device 4 which are connected in sequence, wherein an outlet of the pressure reduction circulation device 4 is connected with an inlet of the material mixing device 1; the structural schematic diagram of the material mixing device 1 is shown in fig. 2, and a cumulative ultrasonic transducer 12 is arranged inside the device.
The material mixing equipment 1 is internally provided with a stirring assembly, and is externally provided with a temperature control jacket 11.
The structural schematic diagram of the high-pressure extraction device 3 is shown in fig. 3, and the interior is closed and hollow; a pressure gauge 31 is arranged on the high-pressure extraction equipment 3; and a pressure reducing valve is arranged at an outlet of the high-pressure extraction equipment 3.
The structure schematic diagram of the decompression circulating equipment 4 is shown in fig. 4, and a circulating pump 6 is arranged on a connecting pipeline of the decompression 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 decompression circulation device 4 is provided with a sight glass 41.
A washing pipeline is arranged between the outlet of the high-pressure delivery pump 2 and the outlet of the decompression circulating equipment 4.
The high-pressure circulation extraction device also comprises an integrated controller 5, wherein the integrated controller 5 is independently connected with the material mixing equipment 1, the high-pressure delivery pump 2, the high-pressure extraction equipment 3 and the decompression circulation equipment 4.
Example 2:
the embodiment provides a high-pressure circulation extraction device, which comprises a material mixing device 1, a high-pressure delivery pump 2, a high-pressure extraction device 3 and a reduced-pressure circulation device 4 which are sequentially connected, wherein an outlet of the reduced-pressure circulation device 4 is connected with an inlet of the material mixing device 1; the structural schematic diagram of the material mixing device 1 is shown in fig. 5, and a dispersive ultrasonic transducer 13 is arranged inside the device.
The material mixing equipment 1 is internally provided with a stirring assembly, and is externally provided with a temperature control jacket 11.
The interior of the high-pressure extraction equipment 3 is closed and hollow; a pressure gauge 31 is arranged on the high-pressure extraction equipment 3; and a pressure reducing valve is arranged at an outlet of the high-pressure extraction equipment 3.
And a circulating pump 6 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.
The high-pressure circulation extraction device also comprises an integrated controller 5, wherein the integrated controller 5 is independently connected with the material mixing equipment 1, the high-pressure delivery pump 2, the high-pressure extraction equipment 3 and the decompression circulation equipment 4.
Application example 1:
this application example provides a method for extracting anthocyanin from lycium ruthenicum by using the high-pressure circulation 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:
in the formula, delta A is an absorbance difference; mw is cyanidin-3-glucoside molecular weight (449.2); DF is the dilution factor; epsilon is the molar extinction coefficient (26900L/(mol cm)) of cyanidin-3-glucoside; 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
As can be seen from Table 1, according to the horizontal contrast between the same experiment serial numbers, the utility model provides a high pressure circulation draws technique's extraction effect will be superior to the technique that the supersound was drawed.
Application example 2:
the application example provides a method for extracting phenylethanoid glycosides from cistanche deserticola by adopting the high-pressure circulating 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
As can be seen from Table 2, according to the horizontal contrast between the same experiment serial numbers, the utility model provides a technique is drawed in the effect of drawing of high pressure circulation extraction technique will be superior to the technique that hot reflux drawed.
Application example 3:
the present application example provides a method of extracting cannabidiol from industrial cannabis using the high pressure cycle 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
As can be seen from Table 3, according to the horizontal contrast between the same experiment serial numbers, the utility model provides a technique is drawed in the effect of drawing of high pressure circulation extraction technique will be superior to the technique that hot reflux drawed.
Application example 4:
the present application example provides a method of extracting cannabis polysaccharide from industrial cannabis using the high pressure loop 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
As can be seen from table 4, according to the horizontal contrast between the same experiment serial numbers, the utility model provides a technique is drawed in the effect of drawing of high pressure circulation extraction technique will be superior to the technique that hot reflux drawed.
Application example 5:
this application example provides a method for extracting phillyrin from forsythia suspensa using the high-pressure circulation 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
As can be seen from table 5, according to the horizontal contrast between the same experiment serial numbers, the utility model provides a technique is drawed in the effect of drawing of high pressure circulation extraction technique will be superior to the technique that hot reflux drawed.
Application example 6:
the present application example provides a method for extracting phillyrin from forsythia suspense leaves using the high-pressure circulation 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
As can be seen from table 6, according to the horizontal contrast between the same experiment serial numbers, the utility model provides a technique is drawed in the effect of drawing of high pressure circulation extraction technique will be superior to the technique that hot reflux drawed.
Application example 7:
this application example provides a method for extracting lycium barbarum polysaccharides from lycium barbarum with the high-pressure circulation extraction device of embodiment 2, which includes:
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
As can be seen from Table 7, according to the horizontal contrast between the same experiment serial numbers, the utility model provides a high pressure circulation draws the technique to extract the effect and will be superior to the technique that hot reflux extracted.
Application example 8:
this application example provides a method for extracting jasminoidin and crocin from gardenia jasminoides by using the high-pressure circulation extraction device of embodiment 2, which comprises:
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
As can be seen from Table 8, according to the horizontal contrast between the same experiment serial numbers, the utility model provides a technique is drawed in the effect of drawing of high pressure circulation extraction technique will be superior to the technique that hot reflux drawed.
Application example 9:
the present application example provides a method of extracting curcumin from turmeric using the high pressure cycle extraction apparatus 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
As can be seen from Table 9, according to the horizontal contrast between the same experiment serial numbers, the utility model provides a high pressure circulation draws the technique to extract the effect and will be superior to the technique that hot reflux extracted.
Application example 10:
the present application example provides a method for extracting asparagus saponin from asparagus by using the high-pressure circulation 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
As can be seen from Table 10, according to the horizontal contrast between the same experiment numbers, the utility model provides a high pressure circulation draws the technique to extract the effect and will be superior to the technique that hot reflux extracted.
By integrating the above embodiments and application examples, the high pressure circulation extraction device of the present invention improves the dissolution rate of the effective components in the plant material by adopting a high pressure extraction mode, and enhances the solid-liquid extraction effect between the plant material 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 described in the above embodiments, but the present invention is not limited to the above detailed device, i.e. the present invention must not be implemented by relying on the above detailed device. It should be clear to those skilled in the art that any improvement of the present invention, to the addition of the equivalent replacement and auxiliary devices of the present invention, the selection of the specific mode, etc., all fall within the scope of protection and disclosure of the present invention.
Claims (10)
1. A high-pressure circulation extraction device is characterized by comprising material mixing equipment, a high-pressure delivery pump, high-pressure extraction equipment and reduced-pressure circulation equipment which are sequentially connected, wherein an outlet of the reduced-pressure circulation equipment is connected with an inlet of the material mixing equipment;
and an ultrasonic generating device is arranged in the material mixing device.
2. The high pressure extraction apparatus of claim 1, wherein the material mixing device is provided with a stirring component inside and a temperature control jacket outside.
3. The high pressure loop extraction apparatus of claim 1, wherein the ultrasound generating device comprises a focused ultrasound transducer and/or a diverging ultrasound transducer.
4. The high pressure loop extraction apparatus of claim 1, wherein the high pressure extraction device is hermetically hollow.
5. The high pressure extraction apparatus of claim 1, wherein the high pressure extraction device is provided with a pressure gauge.
6. The high pressure loop extraction apparatus of claim 1, wherein a pressure relief valve is provided at an outlet of the high pressure extraction device.
7. The high-pressure circulation extraction device according to claim 1, wherein a circulation pump is arranged on a circulation pipeline between the decompression circulation device and the material mixing device.
8. The high pressure loop extraction apparatus of claim 7, wherein an outlet line is connected in parallel with the recirculation line.
9. The high pressure cycle extraction apparatus of claim 1, wherein the pressure reducing cycle device is provided with a sight glass.
10. The high pressure loop extraction apparatus of claim 1, further comprising an integrated controller independently connected to the material mixing device, the high pressure transfer pump, the high pressure extraction device, and the pressure reduction circulation device.
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| CN117782412B (en) * | 2024-02-23 | 2024-05-24 | 中国农业大学 | Pressure indicator and application thereof |
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