CN111840353A - Preparation method and equipment of elderberry extract - Google Patents
Preparation method and equipment of elderberry extract Download PDFInfo
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- CN111840353A CN111840353A CN202010809739.2A CN202010809739A CN111840353A CN 111840353 A CN111840353 A CN 111840353A CN 202010809739 A CN202010809739 A CN 202010809739A CN 111840353 A CN111840353 A CN 111840353A
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- elderberry
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/35—Caprifoliaceae (Honeysuckle family)
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/58—Multistep processes
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B5/00—Drying solid materials or objects by processes not involving the application of heat
- F26B5/04—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum
- F26B5/06—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum the process involving freezing
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
Abstract
The invention relates to the field of elderberry extraction, in particular to a preparation method and equipment of an elderberry extract, which comprises the steps of preparing an elderberry extracting solution; obtaining an elderberry extract, and carrying out primary membrane separation treatment on the elderberry extract to obtain an elderberry extract clarified liquid; obtaining clear liquid of elderberry, and carrying out secondary membrane separation treatment on the clear liquid of elderberry to obtain ultra-filtered clear liquid of elderberry; obtaining an elderberry ultrafiltration clear liquid, and carrying out a third membrane separation treatment on the elderberry ultrafiltration clear liquid to obtain an elderberry ultrafiltration trapped fluid; the method comprises the steps of obtaining elderberry ultrafiltration trapped fluid, carrying out membrane separation treatment on the elderberry ultrafiltration trapped fluid for the fourth time, and carrying out freeze drying on a product after the membrane separation treatment for the fourth time to obtain an elderberry extract.
Description
Technical Field
The invention relates to the field of elderberry extraction, in particular to a preparation method and equipment of an elderberry extract.
Background
Elderberry is the fruit of the plant Sambucus nigra (Sambucus nigra Linn) of the Caprifoliaceae family, produced in Europe under the English name Elderberry. Elderberry plays an important role in the european history of herbs. Hippocastates, honored by the Western as "father of medicine", called elderberry as his kit because of its rich health efficacy. In modern medicine, elderberry is considered to be a sweating drug for the treatment of fever, cold or nasal mucosal disease. In modern medical and pharmacological research, flavone and polyphenol components contained in elderberry have better prevention and treatment effects on viruses such as H1N1 and the like.
The traditional production methods of the elderberry extract comprise ethanol extraction, macroporous resin purification, supercritical extraction and the like. The organic solvent is used and at the same time, the concentration and drying are carried out at a certain temperature. The anthocyanin component in elderberry is marked by cyanidin-3-O glucoside, and is unstable under illumination and high temperature. The production methods have a heating process, so that the extraction rate and the content of anthocyanin are greatly influenced.
Disclosure of Invention
In order to solve the technical problems, the technical scheme solves the problems that cyanidin-3-O glucoside is used for calibration, and anthocyanin components are unstable under illumination and high temperature, and the method and the equipment utilize the combination of low-temperature extraction, membrane separation and freeze drying, adopt a process mode of low temperature in the whole process and avoid the degradation loss of anthocyanin to the maximum extent.
In order to achieve the above purposes, the technical scheme adopted by the invention is as follows:
a preparation method of elderberry extract comprises the following steps:
preparing an elderberry extracting solution;
obtaining the elderberry extract, and carrying out primary membrane separation treatment on the elderberry extract to obtain an elderberry extract clarified liquid;
obtaining the elderberry clear liquid, and carrying out secondary membrane separation treatment on the elderberry clear liquid to obtain an elderberry ultra-filtered clear liquid;
obtaining the elderberry ultrafiltration clear liquid, and carrying out membrane separation treatment on the elderberry ultrafiltration clear liquid for the third time to obtain an elderberry ultrafiltration trapped fluid;
and (3) obtaining the elderberry ultrafiltration trapped fluid, performing fourth membrane separation treatment on the elderberry ultrafiltration trapped fluid, and freeze-drying a product after the fourth membrane separation treatment to obtain an elderberry extract with anthocyanin more than 25%.
Optionally, the preparation of the elderberry extract specifically comprises:
obtaining an elderberry raw material, wherein the elderberry raw material is one or a combination of more of fresh elderberry fruits, frozen elderberry fruits or dried elderberry fruits;
adding purified water 15-30 times of the weight of the elderberry raw material, and dissolving the elderberry raw material;
adjusting the pH value of the dissolved solution to 2-4, and stirring uniformly, wherein the dissolved solution is adjusted by using one acid solution of citric acid and ascorbic acid;
extracting the ph-adjusted solution, and filtering after extraction to obtain elderberry extractive solution, wherein the extraction temperature is 30-45 deg.C and the extraction time is 1-4 hr.
Optionally, the first membrane separation treatment is performed by using a ceramic membrane for clarification treatment, wherein the aperture of the ceramic membrane is 100-800nm, the pressure of the ceramic membrane clarification treatment is 0.04-0.13mpa, and the temperature of the clarification treatment is 20-40 ℃.
Optionally, the elderberry clear liquid is obtained, and the second membrane separation treatment is performed on the elderberry clear liquid to obtain an elderberry ultra-filtered clear liquid, which specifically comprises:
obtaining elderberry clarified liquid, and performing circulating ultrafiltration treatment through an ultrafiltration membrane with molecular weight I, wherein the molecular weight of the ultrafiltration membrane with molecular weight I is 5000-;
and (3) circularly ultrafiltering the elderberry clear liquid to the minimum circulating volume, supplementing purified water, and continuously ultrafiltering to the minimum circulating volume to obtain an elderberry ultrafiltered clear liquid, wherein the weight of the supplemented purified water is 10-20 times of the weight of the elderberry raw material.
Optionally, the elderberry ultrafiltration clear liquid is obtained, and the third membrane separation treatment is performed on the elderberry ultrafiltration clear liquid to obtain an elderberry ultrafiltration retentate, which specifically comprises:
obtaining elderberry ultrafiltration clear liquid, and performing circulating ultrafiltration treatment through an ultrafiltration membrane with molecular weight II, wherein the molecular weight of the ultrafiltration membrane with molecular weight II is 500-;
and (3) circularly ultrafiltering the elderberry ultrafiltration clear liquid to the minimum circulating volume, supplementing purified water, and continuously ultrafiltering to the minimum circulating volume to obtain an elderberry ultrafiltration trapped fluid, wherein the weight of the supplemented purified water is 5-15 times of the weight of the elderberry raw material.
Optionally, the elderberry ultrafiltration retentate is obtained, a fourth membrane separation treatment is performed on the elderberry ultrafiltration retentate, and a product obtained after the fourth membrane separation treatment is freeze-dried, so that an elderberry extract with anthocyanin greater than 25% is obtained, and the method specifically includes the following steps:
obtaining an osteosynthesis raspberry ultrafiltration trapped fluid, and carrying out nanofiltration concentration treatment to ensure that the solid content of a solid-liquid mixture after concentration is 15-20%;
freeze drying solid-liquid mixture with solid content of 15-20% to obtain elderberry extract with anthocyanin greater than 25%, wherein the anthocyanin is cyanidin-3-glucoside as standard, and contains cyanidin-3-ramulus Mori-5-glucoside, cyanidin-3, 5-diglucoside, cyanidin-3-ramulus Mori-glucoside, and cyanidin-3-glucoside.
Further, still provide a preparation facilities of elderberry extract product, including ultrafiltration system, ultrafiltration system includes ultrafiltration apparatus, pipe-line system, rock mechanism and coordinated control mechanism, ultrafiltration apparatus includes a plurality of milipore filter filters, milipore filter sets up in the top cap, the inside of milipore filter is equipped with the milipore filter, the top and bottom of milipore filter are equipped with top cap and bottom cap respectively, milipore filter and top cap, the bottom cap all is the rotation connection, pipe-line system includes the feed liquor pipeline, the feed liquor branch pipe, backwash pipeline and backwash branch pipe, the feed liquor pipeline sets up at milipore filter top, be equipped with the feed liquor branch pipe that equals with milipore filter quantity on the feed liquor pipeline, feed liquor branch pipe and top cap one-to-one, and be connected with the top cap, the feed liquor branch pipe, the backwashing pipeline is provided with backwashing branch pipes with the same number as the ultrafiltration membrane filters, the backwashing branch pipes correspond to the bottom cover one by one and are connected with the bottom cover, the backwashing branch pipes are communicated with the inside of the ultrafiltration membrane filters, the side part of one of the ultrafiltration membrane filters is provided with a shaking mechanism, the shaking mechanism is used for controlling the ultrafiltration membrane filter to rotate along the central shaft of the ultrafiltration membrane filter, each ultrafiltration membrane filter is provided with a linkage control mechanism, and the linkage control mechanism is used for controlling the ultrafiltration membrane filter and the shaking mechanism to control the ultrafiltration membrane filter to rotate synchronously.
Optionally, the pipeline system further comprises a liquid outlet pipeline and liquid outlet branch pipes, the liquid outlet pipeline is arranged at the top of the ultrafiltration membrane filter, the liquid outlet pipeline is provided with the liquid outlet branch pipes, the number of the liquid outlet branch pipes is equal to that of the ultrafiltration membrane filter, the liquid outlet branch pipes correspond to the top cover one to one and are connected with the top cover, and the liquid outlet branch pipes are communicated with the inside of the ultrafiltration membrane filter.
Optionally, the shaking mechanism comprises a shaking driving motor, a mounting bracket, a driving shaft, a worm, a sleeve ring, a fixed rod, a first movable rod, a worm wheel and a second movable rod, wherein the mounting bracket is arranged on the side part of one ultrafiltration membrane filter, the shaking driving motor is arranged on the mounting bracket, the output shaft of the shaking driving motor is connected with the driving shaft in a transmission manner, the worm is coaxially sleeved on the driving shaft, one end of the driving shaft is connected with the shaking driving motor, the sleeve ring is arranged at the other end of the driving shaft, the sleeve ring is sleeved on the ultrafiltration membrane filter and is fixedly connected with the ultrafiltration membrane filter, the fixed rod is hinged on the mounting bracket, the fixed rod is fixed on the frame, one end of the fixed rod is hinged with the mounting bracket, the other end of the fixed rod is hinged with the first movable rod, one end of the first movable, the worm wheel is meshed with the worm, the worm wheel and the second movable rod are coaxially arranged, and the worm wheel is fixedly connected with the second movable rod.
Optionally, the linkage control mechanism includes an outer disk gear, a sleeve, a suspension, a rack, a housing, a lifting drive motor, a first shaft body, a driving drive plate, a notch wheel, a second shaft body, a driven sheave, a sliding groove, a fan-shaped tooth and a pin column, the sleeve is sleeved on each ultrafiltration membrane filter, the sleeve is positioned at the top of the sleeve ring, the sleeve is rotatably connected with the outer disk gear, the outer disk gears positioned on the same horizontal plane are mutually meshed, the suspension is fixed on the sleeve, the rack is hung on the suspension, the housing is arranged on the side portion of the rack, the lifting drive motor is arranged on the housing, the first shaft body is connected with the output shaft of the lifting drive motor in a transmission manner, the first shaft body is rotatably connected inside the housing, the driving drive plate is arranged on the housing, the notch wheel is coaxially connected with the driving drive plate, the pin column is arranged on the, the second shaft body is sleeved with a driven grooved wheel and a fan-shaped tooth, the driven grooved wheel is provided with a plurality of sliding grooves which extend along the radial direction of the driven grooved wheel, the pin column is connected with one of the sliding grooves in a sliding mode, and the fan-shaped tooth is meshed with the rack.
Compared with the prior art, the invention has the beneficial effects that:
the method combines low-temperature extraction, membrane separation and freeze drying, adopts a whole low-temperature process mode, and avoids the degradation loss of anthocyanin to the maximum extent. Meanwhile, in the anthocyanin purification process, the membrane separation is carried out by adopting the difference between the molecular weight of the impurities and the molecular weight of the anthocyanin, so that the purification by using an organic solvent is avoided, the final product has no organic solvent residue, the content of the anthocyanin can reach more than 25 percent, and the quality of the elderberry extract is greatly improved. The whole process is carried out at low temperature, so that the breeding of microorganisms can be effectively controlled.
The whole process is designed into a mode of sealing a pipeline, the probability of polluting microorganisms is greatly reduced, and meanwhile, the microorganisms in the extracting solution can be filtered and removed by the filtering of the ceramic membrane, so that the aseptic production of the subsequent process is ensured.
The method and the equipment apply the ultrafiltration membrane separation technology to the purification of the elderberry anthocyanin, and simultaneously utilize the characteristic of the ceramic membrane for intercepting microorganisms, so that the microorganism indexes of the product can meet the standard requirements without the process conditions of irradiation, moist heat sterilization and the like. Meanwhile, the whole process of the technology is carried out at low temperature, so that the components of anthocyanin are retained to the maximum extent, and the loss of anthocyanin is avoided.
Drawings
FIG. 1 is a schematic flow diagram of the process of the present invention;
FIG. 2 is a schematic view of a detailed process of S100) in the present invention;
FIG. 3 is a schematic view of a detailed flow of step S300) in the present invention;
FIG. 4 is a schematic flow chart of S400) in the present invention;
FIG. 5 is a schematic view of a detailed flow of step S500) in the present invention;
FIG. 6 is a first schematic structural diagram of the apparatus of the present invention;
FIG. 7 is an enlarged schematic view at A of FIG. 6;
FIG. 8 is a front view of the apparatus of the present invention;
FIG. 9 is a second schematic structural view of the apparatus of the present invention;
FIG. 10 is an enlarged schematic view at B of FIG. 9;
FIG. 11 is a first schematic view of the rocking mechanism according to the present invention;
FIG. 12 is a second schematic structural view of a rocking mechanism according to the present invention;
FIG. 13 is a schematic view of the linkage control mechanism according to the present invention;
FIG. 14 is a first schematic structural view of the interior of the housing of the present invention;
fig. 15 is a second structural diagram of the interior of the housing in the present invention.
Description of reference numerals:
1-ultrafiltration equipment; 1 a-a top cover; 1 b-an ultrafiltration membrane filter; 1 c-a bottom cover; 1 d-a frame;
2-a pipeline system; 2 a-a liquid inlet pipeline; 2 b-a liquid inlet branch pipe; 2 c-backwashing the pipeline; 2 d-backwashing branch pipes; 2 e-a liquid outlet pipeline; 2 f-liquid outlet branch pipe;
3-a shaking mechanism; 3 a-shaking drive motor; 3 b-mounting a bracket; 3 c-a drive shaft; 3 d-worm; 3 e-a collar; 3 f-fixing the rod; 3 g-a first movable bar; 3 h-worm gear; 3 i-a second movable bar;
4-a linkage control mechanism; 4 a-outer disc gear; 4 b-a sleeve; 4 c-suspension; 4 d-rack; 4 e-a housing; 4 f-a lifting drive motor; 4 g-first shaft body; 4 h-driving plate; 4 i-notched wheel; 4 j-second shaft; 4 k-driven sheave; 4 m-sliding groove; 4 n-sector teeth; 4 o-pin.
Detailed Description
The following description is presented to disclose the invention so as to enable any person skilled in the art to practice the invention. The preferred embodiments in the following description are given by way of example only, and other obvious variations will occur to those skilled in the art.
Referring to fig. 1, the method includes the following steps:
s100) preparing an elderberry extract, and specifically referring to fig. 2, the method comprises the following steps:
s101) obtaining an elderberry raw material, wherein the elderberry raw material is one or a combination of more of fresh elderberry fruits, frozen elderberry fruits or dried elderberry fruits;
s102) adding purified water which is 15-30 times of the weight of the elderberry raw material, and dissolving the elderberry raw material;
s103) adjusting the pH value of the dissolved solution to 2-4, and uniformly stirring, wherein the dissolved solution is adjusted by using one acid solution of citric acid and ascorbic acid;
s104) extracting the ph-adjusted solution, and filtering after extraction to obtain an elderberry extracting solution, wherein the extracting temperature is 30-45 ℃ and the extracting time is 1-4 hours;
s200) obtaining an elderberry extract, and carrying out primary membrane separation treatment on the elderberry extract, wherein the primary membrane separation treatment adopts a ceramic membrane for clarification treatment, the aperture of the ceramic membrane is 100-800nm, the pressure of the ceramic membrane clarification treatment is 0.04-0.13mpa, and the temperature of the clarification treatment is 20-40 ℃ to obtain an elderberry extract clarified liquid;
s300) obtaining the elderberry clear liquid, and carrying out secondary membrane separation treatment on the elderberry clear liquid to obtain an elderberry ultra-filtration clear liquid, specifically referring to the figure 3, comprising the following steps:
s301) obtaining an elderberry clarified liquid, and performing circulating ultrafiltration treatment through an ultrafiltration membrane with molecular weight I, wherein the molecular weight of the ultrafiltration membrane with molecular weight I is 5000-;
s302) carrying out circulating ultrafiltration on the elderberry clear liquid to the minimum circulating volume, supplementing purified water, and continuously carrying out ultrafiltration to the minimum circulating volume to obtain an elderberry ultrafiltration clear liquid, wherein the weight of the supplemented purified water is 10-20 times of that of the elderberry raw material;
s400) obtaining elderberry ultrafiltration clear liquid, and performing a third membrane separation treatment on the elderberry ultrafiltration clear liquid to obtain elderberry ultrafiltration retentate, specifically, referring to fig. 4, comprising the following steps:
s401) obtaining elderberry ultrafiltration clear liquid, and performing circulating ultrafiltration treatment through an ultrafiltration membrane with molecular weight II, wherein the molecular weight of the ultrafiltration membrane with molecular weight II is 500-2000 daltons, and the permeation pressure is 0.5-1.2 mpa;
s402) carrying out circulating ultrafiltration on the elderberry ultrafiltration clear liquid to the minimum circulating volume, supplementing purified water, and continuing to carry out ultrafiltration to the minimum circulating volume to obtain an elderberry ultrafiltration trapped fluid, wherein the weight of the supplemented purified water is 5-15 times of the weight of the elderberry raw material;
s500) obtaining elderberry ultrafiltration trapped fluid, performing fourth membrane separation treatment on the elderberry ultrafiltration trapped fluid, and freeze-drying a product after the fourth membrane separation treatment to obtain an elderberry extract with anthocyanin more than 25%, wherein the method specifically refers to the figure 5 and comprises the following steps:
s501) obtaining an elderberry ultrafiltration trapped fluid, and carrying out nanofiltration concentration treatment to ensure that the solid content of a solid-liquid mixture after concentration is 15-20%;
s502) carrying out freeze drying treatment on the solid-liquid mixture with the solid content of 15-20% to obtain the elderberry extract with anthocyanin more than 25%, wherein the anthocyanin adopts cyanidin-3-glucoside as a standard substance and comprises the content sum of cyanidin-3-mulberry pond-5-glucoside, cyanidin-3, 5-biglucoside, cyanidin-3-mulberry pond glucoside and cyanidin-3-glucoside, no organic solvent residue exists in the whole process, the anthocyanin yield is more than 85% in the whole process, the anthocyanin purification purity is high, and the elderberry extract is very suitable for mass production.
Wherein, the organic solvent refers to one or more of ethanol, methanol and ethyl acetate.
The method combines low-temperature extraction, membrane separation and freeze drying, adopts a whole low-temperature process mode, and avoids the degradation loss of anthocyanin to the maximum extent. Meanwhile, in the anthocyanin purification process, the membrane separation is carried out by adopting the difference between the molecular weight of the impurities and the molecular weight of the anthocyanin, so that the purification by using an organic solvent is avoided, the final product has no organic solvent residue, the content of the anthocyanin can reach more than 25 percent, and the quality of the elderberry extract is greatly improved. The whole process is carried out at low temperature, so that the breeding of microorganisms can be effectively controlled.
The whole process is designed into a mode of sealing a pipeline, the probability of polluting microorganisms is greatly reduced, and meanwhile, the microorganisms in the extracting solution can be filtered and removed by the filtering of the ceramic membrane, so that the aseptic production of the subsequent process is ensured.
Referring to fig. 6, 8 and 10, the apparatus includes an ultrafiltration system, the ultrafiltration system includes an ultrafiltration apparatus 1, a pipeline system 2, a shaking mechanism 3 and a linkage control mechanism 4, the ultrafiltration apparatus 1 includes a plurality of ultrafiltration membrane filters 1b, the ultrafiltration membrane filters 1b are arranged in a top cover 1a, ultrafiltration membranes are arranged inside the ultrafiltration membrane filters 1b, a top cover 1a and a bottom cover 1c are respectively arranged at the top end and the bottom end of the ultrafiltration membrane filters 1b, the ultrafiltration membrane filters 1b are rotatably connected with the top cover 1a and the bottom cover 1c, the pipeline system 2 includes a liquid inlet pipeline 2a, liquid inlet branch pipes 2b, a backwashing pipeline 2c and backwashing branch pipes 2d, the liquid inlet pipeline 2a is arranged at the top of the ultrafiltration membrane filters 1b, the liquid inlet pipeline 2a is provided with liquid inlet branch pipes 2b having the same number as the ultrafiltration membrane filters 1b, the liquid inlet branch pipes 2, the system is characterized in that the system is connected with a top cover 1a, liquid inlet branch pipes 2b are communicated with the inside of an ultrafiltration membrane filter 1b, a backwashing pipeline 2c is arranged at the bottom of the ultrafiltration membrane filter 1b, backwashing branch pipes 2d equal to the ultrafiltration membrane filter 1b in number are arranged on the backwashing pipeline 2c, the backwashing branch pipes 2d correspond to a bottom cover 1c in a one-to-one mode and are connected with the bottom cover 1c, the backwashing branch pipes 2d are communicated with the inside of the ultrafiltration membrane filter 1b, a liquid outlet pipeline 2e and a liquid outlet branch pipe 2f are further arranged on the top of the ultrafiltration membrane filter 1b, liquid outlet branch pipes 2f equal to the ultrafiltration membrane filter 1b in number are arranged on the liquid outlet pipeline 2e, the liquid outlet branch pipes 2f correspond to the top cover 1a in a one-to-connect. The side part of one ultrafiltration membrane filter 1b is provided with a shaking mechanism 3, the shaking mechanism 3 is used for controlling the ultrafiltration membrane filter 1b to rotate along the central shaft of the ultrafiltration membrane filter 1b, each ultrafiltration membrane filter 1b is provided with a linkage control mechanism 4, and the linkage control mechanism 4 is used for controlling the ultrafiltration membrane filter 1b and the shaking mechanism 3 to synchronously rotate with the ultrafiltration membrane filter 1 b. The pipeline system 2 is a connecting pipeline of the ultrafiltration equipment 1, wherein the liquid inlet pipeline 2a, the backwashing pipeline 2c and the liquid outlet pipeline 2e are respectively a connecting pipeline for inlet, outlet and backwashing, ultrafiltration can be carried out in each ultrafiltration membrane filter 1b, in order to improve the impurity removal effect of the ultrafiltration membrane filters 1b, a shaking mechanism 3 is arranged on the side part of one ultrafiltration membrane filter 1b, the shaking mechanism 3 is responsible for controlling the ultrafiltration membrane filter 1b to shake along the central shaft of the ultrafiltration membrane filter 1b, meanwhile, a linkage control mechanism 4 is matched with the side part of each ultrafiltration membrane filter 1b, the linkage control mechanism 4 on each ultrafiltration membrane filter 1b independently controls the ultrafiltration membrane filter 1b, and the linkage control mechanism is used for controlling the ultrafiltration membrane filter 1b to shake together with the ultrafiltration membrane filter 1b controlled by the shaking mechanism 3.
Referring to fig. 6, 11 and 12, the shaking mechanism 3 includes a shaking driving motor 3a, a mounting bracket 3b, a driving shaft 3c, a worm 3d, a collar 3e, a fixing rod 3f, a first movable rod 3g, a worm wheel 3h and a second movable rod 3i, wherein the side of one ultrafiltration membrane filter 1b is provided with the mounting bracket 3b, the mounting bracket 3b is provided with the shaking driving motor 3a, an output shaft of the shaking driving motor 3a is connected with the driving shaft 3c in a transmission manner, the driving shaft 3c is coaxially sleeved with the worm 3d, one end of the driving shaft 3c is connected with the shaking driving motor 3a, the other end of the driving shaft 3c is provided with the collar 3e, the collar 3e is sleeved on the ultrafiltration membrane filter 1b and fixedly connected with the ultrafiltration membrane filter 1b, the mounting bracket 3b is hinged with the fixing rod 3f, the fixing rod 3f is fixed, one end and the installing support 3b of dead lever 3f are articulated, the other end of dead lever 3f articulates there is first movable rod 3g, the one end and the dead lever 3f of first movable rod 3g are articulated, the other end of first movable rod 3g articulates there is second movable rod 3i, it is connected with worm wheel 3h to rotate on the installing support 3b, worm wheel 3h and worm 3d mesh, worm wheel 3h and the coaxial setting of second movable rod 3i and worm wheel 3h and second movable rod 3i fixed connection.
The fixed rod 3f in the shaking mechanism 3 is fixed on the frame 1d, namely the fixed rod 3f is always in a fixed state, when the shaking driving motor 3a works, the driving shaft 3c and the worm 3d are driven to rotate, when the worm 3d rotates, the worm wheel 3h meshed with the worm is driven to rotate, when the worm wheel 3h rotates, the second movable rod 3i coaxially fixed with the worm wheel 3h is driven to rotate together, when the second movable rod 3i rotates, the first movable rod 3g is driven to move, because the fixed rod 3f is always in a fixed state, the shaking driving motor 3a, the mounting bracket 3b, the driving shaft 3c, the worm 3d, the lantern ring 3e, the first movable rod 3g, the worm wheel 3h and the second movable rod 3i perform reciprocating shaking movement around the hinge point of the fixed rod 3f and the first movable rod 3g, the collar 3e is fixed to one of the ultrafiltration membrane filters 1b, and thus rotates the ultrafiltration membrane filter 1b along its central axis.
Referring to fig. 7, 10, 13, 14 and 15, the linkage control mechanism 4 includes an outer disk gear 4a, a sleeve 4b, a suspension 4c, a rack 4d, a housing 4e, a lifting driving motor 4f, a first shaft 4g, a driving dial 4h, a notch wheel 4i, a second shaft 4j, a driven sheave 4k, a sliding slot 4m, a sector gear 4n and a pin 4o, each ultrafiltration membrane filter 1b is sleeved with the sleeve 4b, the sleeve 4b is located at the top of the sleeve ring 3e, the sleeve 4b is rotatably connected with the outer disk gear 4a, the outer disk gears 4a located on the same horizontal plane are engaged with each other, the suspension 4c is fixed on the sleeve 4b, the rack 4d is hung on the suspension 4c, the housing 4e is arranged at the side of the rack 4d, the lifting driving motor 4f is arranged on the housing 4e, an output shaft of the lifting driving motor 4f is connected with the first shaft 4g, the first shaft body 4g is rotatably connected inside the shell 4e, the shell 4e is provided with a driving drive plate 4h, the driving drive plate 4h is coaxially connected with a notch wheel 4i, the side part of the notch position of the notch wheel 4i is provided with a pin 4o, the side part of the first shaft body 4g is provided with a second shaft body 4j rotatably connected inside the shell 4e, the second shaft body 4j is sleeved with a driven sheave 4k and fan-shaped teeth 4n, the driven sheave 4k is provided with a plurality of sliding grooves 4m radially extending along the driven sheave 4k, the pin 4o is slidably connected with one of the sliding grooves 4m, and the fan-shaped teeth 4n are meshed with the rack 4 d.
Each lifting driving motor 4f works independently, when the lifting driving motor 4f works, the lifting driving motor 4f drives the first shaft body 4g to rotate, and simultaneously the driving dial 4h, the notched wheel 4i and the pin 4o also synchronously rotate along the central axis of the first shaft body 4g, wherein the pin 4o is eccentrically arranged on the driving dial 4h, when the driving dial 4h rotates, the pin 4o on the driving dial 4h does not enter one driven sheave 4k of the sliding grooves 4m, because the inward concave locking arc of the driven sheave 4k is clamped by the outward concave locking arc of the notched wheel 4i, at the moment, the driven sheave 4k is not moved, and then the driven sheave 4k also continues to rotate, the pin 4o enters one of the sliding grooves 4m, and when the pin 4o enters the sliding groove 4m, the locking arc of the driven sheave 4k is just loosened, thereafter, the driven sheave 4k is driven by the pin 4o to rotate, and when the pin 4o leaves the sliding groove 4m during continuous rotation, the locking arc of the driven sheave 4k is again locked, and the driven sheave 4k is still. This movement is repeated until the pin 4o enters again the other sliding groove 4m of the driven sheave 4k, and therefore, the driven sheave 4k is intermittently rotated while being moved.
When the driven sheave 4k performs intermittent rotary motion, the fan-shaped teeth 4n coaxially connected with the driven sheave 4k also perform intermittent rotary motion of moving and stopping at the same time synchronously, the fan-shaped teeth 4n are meshed with the rack 4d corresponding to the linkage control mechanism 4, and the fan-shaped teeth 4n are fan-shaped, so that the rack 4d, the suspension 4c, the sleeve 4b and the outer disk gear 4a can be driven to perform intermittent lifting motion along the central shaft of the ultrafiltration membrane filter 1b, and the lifting height of each time is equal. The linkage control mechanism 4 of the ultrafiltration membrane filter 1b controlled by the shaking mechanism 3 is responsible for playing a role in position calibration, after the calibration is finished, the linkage control mechanism 4 does not act any more, the outer disc gear 4a and the sleeve 4b on the ultrafiltration membrane filter 1b controlled by the shaking mechanism 3 are fixed at a certain height, and when the outer disc gears 4a on other ultrafiltration membrane filters 1b lift along the central shaft of the ultrafiltration membrane filter 1b, the mutual outer disc gears 4a can be controlled to complete meshing, so that the ultrafiltration membrane filters 1b controlled by the shaking mechanism 3 can shake together.
The equipment realizes the functions of the invention through the following steps, thereby solving the technical problems provided by the invention:
step one, after the elderberry clear liquid is obtained through preparation, introducing the elderberry clear liquid into a liquid inlet pipeline 2a, allowing the elderberry clear liquid to enter each ultrafiltration membrane filter 1b along a liquid inlet branch pipe 2b, performing secondary membrane separation treatment on the elderberry clear liquid in the ultrafiltration membrane filters 1b to obtain elderberry ultrafiltration clear liquid, and allowing the elderberry ultrafiltration clear liquid to flow out along a backwashing pipeline 2c and a backwashing branch pipe 2 d;
step two, starting the shaking driving motor 3a, driving the driving shaft 3c and the worm 3d to rotate when the shaking driving motor 3a works, when the worm 3d rotates, the worm wheel 3h engaged with the worm is driven to rotate, when the worm wheel 3h rotates, the second movable rod 3i coaxially fixed with the worm wheel is driven to rotate together, when the second movable rod 3i rotates, the first movable rod 3g is driven to move, because the fixed rod 3f is always in a fixed state, the shaking driving motor 3a, the mounting bracket 3b, the driving shaft 3c, the worm 3d, the lantern ring 3e, the first movable rod 3g, the worm wheel 3h and the second movable rod 3i perform reciprocating swing motion around a hinge point of the fixed rod 3f and the first movable rod 3g, so that the ultrafiltration membrane filter 1b is driven to rotate along the central axis thereof;
and step three, the coordinated control mechanism 4 of each ultrafiltration membrane filter 1b works independently, when the lifting drive motor 4f corresponding to the ultrafiltration membrane filter 1b works, the driven sheave 4k is driven to do intermittent rotary motion, the fan-shaped teeth 4n coaxially connected with the driven sheave 4k synchronously do intermittent rotary motion of stopping at the same time, the fan-shaped teeth 4n are meshed with the rack 4d corresponding to the coordinated control mechanism 4, and the fan-shaped teeth 4n are fan-shaped, so that the rack 4d, the suspension 4c, the sleeve 4b and the outer disk gear 4a can be driven to do intermittent lifting motion along the central shaft of the ultrafiltration membrane filter 1b, the meshing of the outer disk gears 4a can be controlled, and the ultrafiltration membrane filter 1b controlled by the shaking mechanism 3 can be shaken together.
The working principle of the invention is as follows: the method combines low-temperature extraction, membrane separation and freeze drying, adopts a whole low-temperature process mode, and avoids the degradation loss of anthocyanin to the maximum extent. Meanwhile, in the anthocyanin purification process, the membrane separation is carried out by adopting the difference between the molecular weight of the impurities and the molecular weight of the anthocyanin, so that the purification by using an organic solvent is avoided, the final product has no organic solvent residue, the content of the anthocyanin can reach more than 25 percent, and the quality of the elderberry extract is greatly improved. The whole process is carried out at low temperature, so that the breeding of microorganisms can be effectively controlled.
The whole process is designed into a mode of sealing a pipeline, the probability of polluting microorganisms is greatly reduced, and meanwhile, the microorganisms in the extracting solution can be filtered and removed by the filtering of the ceramic membrane, so that the aseptic production of the subsequent process is ensured.
The method and the equipment apply the ultrafiltration membrane separation technology to the purification of the elderberry anthocyanin, and simultaneously utilize the characteristic of the ceramic membrane for intercepting microorganisms, so that the microorganism indexes of the product can meet the standard requirements without the process conditions of irradiation, moist heat sterilization and the like. Meanwhile, the whole process of the technology is carried out at low temperature, so that the components of anthocyanin are retained to the maximum extent, and the loss of anthocyanin is avoided.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. The preparation method of the elderberry extract is characterized by comprising the following steps:
preparing an elderberry extracting solution;
obtaining the elderberry extract, and carrying out primary membrane separation treatment on the elderberry extract to obtain an elderberry extract clarified liquid;
obtaining the elderberry clear liquid, and carrying out secondary membrane separation treatment on the elderberry clear liquid to obtain an elderberry ultra-filtered clear liquid;
obtaining the elderberry ultrafiltration clear liquid, and carrying out membrane separation treatment on the elderberry ultrafiltration clear liquid for the third time to obtain an elderberry ultrafiltration trapped fluid;
and (3) obtaining the elderberry ultrafiltration trapped fluid, performing fourth membrane separation treatment on the elderberry ultrafiltration trapped fluid, and freeze-drying a product after the fourth membrane separation treatment to obtain an elderberry extract with anthocyanin more than 25%.
2. The preparation method of the elderberry extract according to claim 1, wherein the preparation of the elderberry extract comprises:
obtaining an elderberry raw material, wherein the elderberry raw material is one or a combination of more of fresh elderberry fruits, frozen elderberry fruits or dried elderberry fruits;
adding purified water 15-30 times of the weight of the elderberry raw material, and dissolving the elderberry raw material;
adjusting the pH value of the dissolved solution to 2-4, and stirring uniformly, wherein the dissolved solution is adjusted by using one acid solution of citric acid and ascorbic acid;
extracting the ph-adjusted solution, and filtering after extraction to obtain elderberry extractive solution, wherein the extraction temperature is 30-45 deg.C and the extraction time is 1-4 hr.
3. The method for preparing the elderberry extract according to claim 2, wherein the first membrane separation treatment is performed by ceramic membrane clarification treatment, the pore diameter of the ceramic membrane is 100-800nm, the pressure of the ceramic membrane clarification treatment is 0.04-0.13mpa, and the temperature of the clarification treatment is 20-40 ℃.
4. The preparation method of the elderberry extract according to claim 3, wherein the elderberry clear solution is obtained and subjected to a second membrane separation treatment to obtain an elderberry ultrafiltered clear solution, and the method specifically comprises the following steps:
obtaining elderberry clarified liquid, and performing circulating ultrafiltration treatment through an ultrafiltration membrane with molecular weight I, wherein the molecular weight of the ultrafiltration membrane with molecular weight I is 5000-;
and (3) circularly ultrafiltering the elderberry clear liquid to the minimum circulating volume, supplementing purified water, and continuously ultrafiltering to the minimum circulating volume to obtain an elderberry ultrafiltered clear liquid, wherein the weight of the supplemented purified water is 10-20 times of the weight of the elderberry raw material.
5. The preparation method of the elderberry extract according to claim 4, wherein the obtaining of the elderberry ultrafiltration clear liquid and the third membrane separation treatment of the elderberry ultrafiltration clear liquid to obtain the elderberry ultrafiltration retentate specifically comprises:
obtaining elderberry ultrafiltration clear liquid, and performing circulating ultrafiltration treatment through an ultrafiltration membrane with molecular weight II, wherein the molecular weight of the ultrafiltration membrane with molecular weight II is 500-;
and (3) circularly ultrafiltering the elderberry ultrafiltration clear liquid to the minimum circulating volume, supplementing purified water, and continuously ultrafiltering to the minimum circulating volume to obtain an elderberry ultrafiltration trapped fluid, wherein the weight of the supplemented purified water is 5-15 times of the weight of the elderberry raw material.
6. The preparation method of the elderberry extract according to claim 5, wherein the elderberry ultrafiltration retentate is obtained, and the fourth membrane separation treatment is performed on the elderberry ultrafiltration retentate, and the freeze drying is performed on the product after the fourth membrane separation treatment to obtain the elderberry extract with anthocyanin greater than 25%, specifically comprising:
obtaining an osteosynthesis raspberry ultrafiltration trapped fluid, and carrying out nanofiltration concentration treatment to ensure that the solid content of a solid-liquid mixture after concentration is 15-20%;
freeze drying solid-liquid mixture with solid content of 15-20% to obtain elderberry extract with anthocyanin greater than 25%, wherein the anthocyanin is cyanidin-3-glucoside as standard, and contains cyanidin-3-ramulus Mori-5-glucoside, cyanidin-3, 5-diglucoside, cyanidin-3-ramulus Mori-glucoside, and cyanidin-3-glucoside.
7. The preparation equipment of the elderberry extract comprises an ultrafiltration system, and is characterized in that the ultrafiltration system comprises ultrafiltration equipment (1), a pipeline system (2), a shaking mechanism (3) and a linkage control mechanism (4), the ultrafiltration equipment (1) comprises a plurality of ultrafiltration membrane filters (1b), the ultrafiltration membrane filters (1b) are arranged in a top cover (1a), ultrafiltration membranes are arranged inside the ultrafiltration membrane filters (1b), the top end and the bottom end of the ultrafiltration membrane filters (1b) are respectively provided with a top cover (1a) and a bottom cover (1c), the ultrafiltration membrane filters (1b) are rotatably connected with the top cover (1a) and the bottom cover (1c), the pipeline system (2) comprises a liquid inlet pipeline (2a), a liquid inlet branch pipe (2b), a backwashing pipeline (2c) and a backwashing branch pipe (2d), the liquid inlet pipeline (2a) is arranged at the top of the ultrafiltration membrane filters (1b), liquid inlet branch pipes (2b) with the same number as that of the ultrafiltration membrane filters (1b) are arranged on the liquid inlet pipeline (2a), the liquid inlet branch pipes (2b) correspond to the top cover (1a) one by one and are connected with the top cover (1a), the liquid inlet branch pipes (2b) are communicated with the inside of the ultrafiltration membrane filters (1b), the backwashing pipeline (2c) is arranged at the bottom of the ultrafiltration membrane filters (1b), backwashing branch pipes (2d) with the same number as that of the ultrafiltration membrane filters (1b) are arranged on the backwashing pipeline (2c), the backwashing branch pipes (2d) correspond to the bottom cover (1c) one by one and are connected with the bottom cover (1c), the backwashing branch pipes (2d) are communicated with the inside of the ultrafiltration membrane filters (1b), a shaking mechanism (3) is arranged on the side of one of the ultrafiltration membrane filters (1b), and is used for controlling the ultrafiltration membrane filters (1b) to rotate along, each ultrafiltration membrane filter (1b) is provided with a linkage control mechanism (4), and the linkage control mechanism (4) is used for controlling the ultrafiltration membrane filter (1b) and the shaking mechanism (3) to control the ultrafiltration membrane filter (1b) to synchronously rotate.
8. The preparation equipment of the elderberry extract according to claim 7, wherein the pipeline system (2) further comprises a liquid outlet pipeline (2e) and liquid outlet branch pipes (2f), the liquid outlet pipeline (2e) is arranged at the top of the ultrafiltration membrane filter (1b), the liquid outlet pipeline (2e) is provided with the liquid outlet branch pipes (2f) which are equal to the ultrafiltration membrane filter (1b) in number, the liquid outlet branch pipes (2f) are in one-to-one correspondence with the top cover (1a) and are connected with the top cover (1a), and the liquid outlet branch pipes (2f) are communicated with the inside of the ultrafiltration membrane filter (1 b).
9. The preparation device of the elderberry extract according to claim 8, wherein the shaking mechanism (3) comprises a shaking driving motor (3a), a mounting bracket (3b), a driving shaft (3c), a worm (3d), a ring (3e), a fixed rod (3f), a first movable rod (3g), a worm wheel (3h) and a second movable rod (3i), wherein the mounting bracket (3b) is arranged at the side part of one ultrafiltration membrane filter (1b), the shaking driving motor (3a) is arranged on the mounting bracket (3b), the driving shaft (3c) is connected with an output shaft of the shaking driving motor (3a) in a transmission way, the worm (3d) is coaxially sleeved on the driving shaft (3c), one end of the driving shaft (3c) is connected with the shaking driving motor (3a), the ring (3e) is arranged at the other end of the driving shaft (3c), the lantern ring (3e) is sleeved on the ultrafiltration membrane filter (1b) and is fixedly connected with the ultrafiltration membrane filter (1b), a fixing rod (3f) is hinged to the mounting support (3b), the fixing rod (3f) is fixed to the rack (1d), one end of the fixing rod (3f) is hinged to the mounting support (3b), the other end of the fixing rod (3f) is hinged to a first movable rod (3g), one end of the first movable rod (3g) is hinged to the fixing rod (3f), the other end of the first movable rod (3g) is hinged to a second movable rod (3i), a worm wheel (3h) is rotatably connected to the mounting support (3b), the worm wheel (3h) is meshed with the worm (3d), the worm wheel (3h) and the second movable rod (3i) are coaxially arranged, and the worm wheel (3h) is fixedly connected with the second movable rod (3 i).
10. The preparation equipment of the elderberry extract according to claim 9, wherein the linkage control mechanism (4) comprises an outer disk gear (4a), a sleeve (4b), a suspension (4c), a rack (4d), a housing (4e), a lifting drive motor (4f), a first shaft body (4g), a driving dial (4h), a notch wheel (4i), a second shaft body (4j), a driven sheave (4k), a sliding groove (4m), a sector gear (4n) and a pin (4o), each ultrafiltration membrane filter (1b) is sleeved with the sleeve (4b), the sleeve (4b) is positioned at the top of the sleeve ring (3e), the sleeve (4b) is rotatably connected with the outer disk gear (4a), the outer disk gears (4a) positioned on the same horizontal plane are engaged with each other, a suspension (4c) is fixed on the sleeve (4b), a rack (4d) is hung on the suspension (4c), a shell (4e) is arranged on the side portion of the rack (4d), a lifting driving motor (4f) is arranged on the shell (4e), an output shaft of the lifting driving motor (4f) is connected with a first shaft body (4g) in a transmission manner, the first shaft body (4g) is rotatably connected inside the shell (4e), a driving dial (4h) is arranged on the shell (4e), a notch wheel (4i) is coaxially connected on the driving dial (4h), a pin column (4o) is arranged on the side portion of the notch position of the notch wheel (4i), a second shaft body (4j) rotatably connected inside the shell (4e) is arranged on the side portion of the first shaft body (4g), a driven sheave (4k) and a fan-shaped tooth (4n) are sleeved on the second shaft body (4j), a plurality of sliding grooves (4m) are arranged on the driven sheave (4k) and, the pin (4o) is connected with one sliding groove (4m) in a sliding mode, and the sector-shaped teeth (4n) are meshed with the rack (4 d).
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| CN202010809739.2A CN111840353A (en) | 2020-08-13 | 2020-08-13 | Preparation method and equipment of elderberry extract |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| EP4190341A1 (en) * | 2021-12-06 | 2023-06-07 | Iprona AG/SpA | Elderberry extract for use in a method of preventing or treating sars-cov-2 infection |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| EP4190341A1 (en) * | 2021-12-06 | 2023-06-07 | Iprona AG/SpA | Elderberry extract for use in a method of preventing or treating sars-cov-2 infection |
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