Extraction equipment and extraction method of polydatin
阅读说明：本技术 一种虎杖苷的提取设备及提取方法 (Extraction equipment and extraction method of polydatin ) 是由 *** 王大为 徐丹 杨丽君 王省 于 2019-10-18 设计创作，主要内容包括：本发明公开了一种虎杖苷的提取设备及提取方法,涉及医药技术领域。设备包括工作台架,工作台架上由上至下依次固定连接有粉碎机、提取桶和锥形瓶,提取筒的一侧设有溶胀桶,锥形瓶一侧的顶部固定连接有装柱组件,锥形瓶的一侧由近至远依次设有搅拌桶和结晶桶,粉碎机的输出端固定连接有出料管,出料管的一端位于提取桶的内圈顶部,提取桶的顶部内圈中心处设有伺服电机。通过在将虎杖原料进行粉碎过滤干燥后进行预的处理,避免吸附过多杂质的树脂降低对有效成分虎杖甙的吸附效果,充分溶胀后的聚酰胺单体直径较小,有利于提高精提取操作中树脂对虎杖甙的吸附速度,且可将虎杖粗提物粉末中的纤维素杂质进行强效吸附并清洗过滤。(The invention discloses equipment and a method for extracting polydatin, and relates to the technical field of medicines. Equipment includes the workstation frame, fixedly connected with rubbing crusher from top to bottom in proper order on the workstation frame, draw bucket and erlenmeyer flask, one side of drawing a section of thick bamboo is equipped with the swelling bucket, the top fixedly connected with dress post subassembly of erlenmeyer flask one side, one side of erlenmeyer flask is by nearly to being equipped with agitator and crystallization bucket far away in proper order, rubbing crusher's output fixedly connected with discharging pipe, the one end of discharging pipe is located the inner circle top of drawing the bucket, the top inner circle center department of drawing the bucket is equipped with servo motor. Through carrying out preliminary treatment after smashing the filtration drying with giant knotweed rhizome raw materials, avoid adsorbing the resin of too much impurity and reduce the adsorption effect to effective component polydatin, polyamide monomer diameter after abundant swelling is less, is favorable to improving the adsorption rate of resin to polydatin in the extraction operation, and can carry out the strong absorption and wash the filtration with the cellulose impurity in the giant knotweed rhizome crude extract powder.)
1. The utility model provides an extraction equipment of polydatin, includes workstation frame (1), its characterized in that: the automatic extracting device is characterized in that a pulverizer (14), an extracting barrel (2) and a conical flask (31) are fixedly connected to the workbench frame (1) from top to bottom in sequence, a swelling barrel (3) is arranged on one side of the extracting barrel, a column assembling component (32) is fixedly connected to the top of one side of the conical flask (31), a stirring barrel (4) and a crystallizing barrel (5) are sequentially arranged on one side of the conical flask (31) from near to far, a discharging pipe (141) is fixedly connected to the output end of the pulverizer (14), one end of the discharging pipe (141) is located at the top of an inner ring of the extracting barrel (2), a servo motor is arranged at the center of the inner ring of the top of the extracting barrel (2) and fixedly connected to the side wall of the extracting barrel (2) through a connecting frame, a stirring shaft (21) is fixedly connected to the output end of the servo motor on the extracting barrel (2), the column assembling component (32, the bottom fixedly connected with water pipe (324) of body (321), the one end fixedly connected with precision filter screen (323) of body (321) inner wall, cup joint piston (322) with body (321) adaptation on water pipe (324).
2. The apparatus for extracting polydatin according to claim 1, wherein: the utility model discloses a conical flask, including extraction bucket (2), erlenmeyer flask (31) swelling bucket (3) opposite side is located same vertical plane, the bottom of extracting bucket (2) is equipped with the sliding seat, and the top fixedly connected with semicircular loose collar of sliding seat, all through loose axle and loose collar swing joint the front and back of extracting bucket (2).
3. The apparatus for extracting polydatin according to claim 1, wherein: the other side of the top of the extraction barrel (2) is fixedly connected with an oblique filter screen (22), and the top of the swelling barrel (3) is close to one side of the extraction barrel (2) and is fixedly connected with an oblique guide plate.
4. The apparatus for extracting polydatin according to claim 1, wherein: the automatic drying device is characterized in that the workbench frame (1) is sequentially provided with a first-stage bedplate (11), a second-stage bedplate (12) and a third-stage bedplate (13) which are parallel to each other through pillars and fixedly connected from bottom to top, the extraction barrel (2) and the swelling barrel (3) are sequentially and fixedly connected to the upper surface of the second-stage bedplate (12) from left to right, and the conical bottle (31), the stirring barrel (4) and the crystallization barrel (5) are sequentially and fixedly connected to the upper surface of the first-stage bedplate (11) from left to right.
5. The extraction method of polydatin is characterized by comprising the following steps:
s1, crude extraction: the raw material adopts giant knotweed rhizome, the reagent adopts 95% ethanol, dried giant knotweed rhizome is crushed by a crusher (14), the 95% ethanol is put into an extraction barrel (2) for extraction, the extraction operation is specifically that the crushed giant knotweed rhizome is put into the extraction barrel (2) for heating to boiling and is stirred by a stirring shaft (21), the mixed solution after extraction is filtered by a filter screen (22), the filtrate is combined, and the filtrate is dried in vacuum by a vacuum drier to obtain the crude extract of the polydatin;
s2, fine extraction: soaking polyamide in 95% ethanol for 24 hr to swell polyamide after absorbing ethanol, loading the swelled polyamide mixture into column for cleaning, soaking in clear water, placing the cleaned swelled matter in a conical flask (31), reflux-extracting crude polydatin extract in S1 with 80% ethanol, filtering, combining the filtrates, concentrating under reduced pressure, adding water in an amount three times the volume of the filtrate, centrifuging to obtain a sample solution, pouring the sample solution into the conical flask (31), adsorbing in a centrifuge at room temperature for 12 hr, filtering to obtain a refined extract filtrate, and vacuum-drying to obtain a refined extract of polydatin;
s3, refining: and (3) stirring and dissolving the refined extract in the S2 by using 90% ethanol to obtain a refined solution, stirring and dissolving the refined solution by using 200-mesh and 300-mesh neutral alumina, adsorbing impurities in the refined solution by using the alumina to obtain adsorbed alumina and a refined solution after adsorption, washing and separating the adsorbed alumina to further obtain the alumina and the refined solution after adsorption, mixing the refined solution after separation and the refined solution to obtain a mixed solution, filtering to obtain a refined solution of the polydatin, standing, crystallizing and filtering to obtain the final polydatin crystal.
6. The method according to claim 5, wherein the ethanol remaining in the filtered impurities after the leaching in S1 is recovered under reduced pressure, the inside of the closed container is evacuated by a vacuum reducer to reduce the water content in the filtrate, the filtrate is heated to evaporate the water, and finally the water and the ethanol are separated.
7. The method for extracting polydatin according to claim 5, wherein said S2 column loading operation comprises fixing the organic glass tube on the operation frame, closing the top end with a dense filter net, plugging the piston (322) with a plug, adding distilled water, pouring the swollen polyamide swollen matter into the glass tube while stirring with a glass rod, continuously adding distilled water, after the water surface overflows, opening the piston (322), draining the excess water from the bottom of the glass tube, always keeping the water surface in the glass tube higher than the swollen matter before the transfer of the polyamide swollen matter is finished, continuously adding distilled water for 30 minutes after the transfer of the swollen matter is finished, wherein the volume ratio of the swollen matter to the sample liquid in S2 is 1: 20.
8. the method for extracting polydatin according to claim 5, wherein the crystallization of the refined solution in S3 comprises dissolving the refined solution in 40% ethanol, filtering to obtain refined filtrate and crude crystals, refrigerating the refined filtrate for crystallization to obtain refined crystals, and recrystallizing the crude crystals and the refined crystals to obtain the final crystals.
Technical Field
The invention relates to the technical field of chemistry and chemical engineering, in particular to equipment and a method for extracting polydatin.
Background
Polydatin is an extract of a plant giant knotweed, can be used for relieving cough, regulating blood fat, reducing cholesterol and resisting shock, is white needle-shaped crystal powder, is easily soluble in methanol and ethanol, is slightly soluble in water and ethyl acetate, and has the effects of dispelling rheumatism, promoting blood circulation to remove blood stasis, relieving cough and reducing sputum, the polydatin is extracted from the giant knotweed, and the giant knotweed contains resveratrol and polydatin, wherein the polydatin is ten to twenty times of the resveratrol.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides equipment and a method for extracting polydatin, which aim to solve the problems in the background art.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: the extraction equipment of the polydatin comprises a workbench frame, wherein a pulverizer, an extraction barrel and a conical flask are fixedly connected on the workbench frame from top to bottom in sequence, a swelling barrel is arranged on one side of the extraction barrel, a column assembly component is fixedly connected to the top of one side of the conical flask, a stirring barrel and a crystallization barrel are sequentially arranged on one side of the conical flask from near to far, a discharge pipe is fixedly connected to the output end of the pulverizer, one end of the discharge pipe is positioned at the top of an inner ring of the extraction barrel, a servo motor is arranged at the center of the inner ring at the top of the extraction barrel and is fixedly connected with the side wall of the extraction barrel through a connecting frame, a stirring shaft is fixedly connected to the output end of the servo motor on the extraction barrel, the column assembly component comprises a pipe body with two communicated ends, a water pipe is fixedly connected to the bottom of the pipe body, and a piston matched with the pipe body is sleeved on the water pipe.
The column assembly can combine with colloidal polyamide, and the polyamide can adsorb effective components and make water flow through the colloid, so that the cellulose impurities in the giant knotweed rhizome are washed out.
Further optimize this technical scheme, erlenmeyer flask and swelling bucket opposite side are located same vertical plane, the bottom of drawing the bucket is equipped with the sliding seat, and the top fixedly connected with semicircular loose ring of sliding seat, draw the front and back of bucket all through loose axle and loose ring swing joint.
This sets up the sliding seat, combines the loose loop, can incline the extraction bucket, is convenient for pour out the content slope in the bucket in order to carry out operation on next step.
Further optimize this technical scheme, the opposite side fixedly connected with diagonal filter screen of extraction bucket top, the top of swelling bucket is close to extraction bucket one side fixedly connected with diagonal baffle.
This set up deflector, make the raw materials poured into the swelling bucket carry out the rapid direction.
Further optimizing the technical scheme, the workbench frame is fixedly connected with a first-stage bedplate, a second-stage bedplate and a third-stage bedplate which are parallel to each other from bottom to top through pillars, the extraction barrel and the swelling barrel are fixedly connected to the upper surface of the second-stage bedplate from left to right in sequence, and the conical flask, the stirring barrel and the crystallization barrel are fixedly connected to the upper surface of the first-stage bedplate from left to right in sequence.
The work bench is configured to allow for the flow-through operation of the equipment components on the primary, secondary, and tertiary platens.
A method for extracting polydatin comprises the following steps:
s1: coarse extraction: pulverizing dried rhizoma Polygoni Cuspidati with a pulverizer, extracting with 95% ethanol in an extraction barrel, heating to boil, stirring with a stirring shaft, filtering with a filter screen, mixing filtrates, and vacuum drying with a vacuum drier to obtain crude polydatin extract;
s2: fine extraction: soaking polyamide in 95% ethanol for 24 hr to swell polyamide after absorbing ethanol, loading the swelled polyamide mixture into column for cleaning, soaking in clear water, placing the cleaned swelled matter in a conical flask, reflux-extracting crude polydatin extract in S1 with 80% ethanol, filtering, combining the filtrates, concentrating under reduced pressure, adding water in an amount three times the volume of the filtrate, centrifuging to obtain a sample solution, pouring the sample solution into the conical flask, placing in a centrifuge for adsorption at room temperature for 12 hr, filtering to obtain a refined extract filtrate, and vacuum-drying to obtain a refined polydatin extract;
s3: refining: and (3) stirring and dissolving the refined extract in the S2 by using 90% ethanol to obtain a refined solution, stirring and dissolving the refined solution by using 200-mesh and 300-mesh neutral alumina, adsorbing impurities in the refined solution by using the alumina to obtain adsorbed alumina and a refined solution after adsorption, washing and separating the adsorbed alumina to further obtain the alumina and the refined solution after adsorption, mixing the refined solution after separation and the refined solution to obtain a mixed solution, filtering to obtain a refined solution of the polydatin, standing, crystallizing and filtering to obtain the final polydatin crystal.
Further optimizing the technical scheme, the residual ethanol in the filtered impurities after leaching in the S1 is subjected to decompression recovery, the inside of the closed container is vacuumized by adopting a vacuum decompressor so that the water in the filtrate is reduced, the water is evaporated by heating, and finally the water and the ethanol are separated.
Further optimizing the technical scheme, the S2 column filling operation comprises the steps of fixing the organic glass tube on an operation frame, covering a high-density filter screen at the bottom end of the organic glass tube, plugging a piston, adding distilled water, pouring the swelled polyamide swelled substances into the glass tube while stirring by using a glass rod, continuously adding distilled water in the process, opening the piston after the water surface overflows, discharging the redundant water from the bottom of the glass tube, always keeping the water surface in the glass tube higher than the swelled substances before the polyamide swelled substances are transferred, continuously adding distilled water for 30 minutes after the transfer of the swelled substances is finished, wherein the volume ratio of the swelled substances to the sample liquid in S2 is 1: 20.
further optimizing the technical scheme, the crystallization operation of the refined solution in the step S3 is to add 40% ethanol into the refined solution for dissolving and filtering, obtain refined filtrate and crude crystals after the refined crystals are filtered, obtain refined crystals after the refined filtrate is refrigerated and crystallized, and obtain the final finished product crystals after the crude crystals and the refined crystals are recrystallized.
(III) advantageous effects
Compared with the prior art, the invention provides equipment and a method for extracting polygonin, which have the following beneficial effects:
1. according to the extraction equipment and the extraction method of the polydatin, the polydatin raw material is subjected to pretreatment after being crushed, filtered and dried, so that the reduction of the adsorption effect of the resin for adsorbing excessive impurities on the polydatin serving as an effective component is avoided, the diameter of the polyamide monomer after full swelling is small, the adsorption speed and the adsorption effect of the resin on the polydatin in the high-precision extraction operation are favorably improved, and the cellulose impurities in the polydatin crude extract powder can be strongly adsorbed, cleaned and filtered.
2. According to the extraction equipment and the extraction method of the polydatin, neutral alumina is used, and alumina with fine particle size is adopted, so that the contact area is large, the impurity removal effect is good, the diameter of an alumina monomer is small, the impurity adsorption efficiency is improved, the large-scale production of the polydatin is facilitated, and the corrosion to the inner wall of the preparation equipment due to the overhigh or overlow pH value is avoided by adopting the neutral alumina.
Drawings
FIG. 1 is a schematic view of a device for extracting polydatin according to the present invention;
FIG. 2 is a schematic view of a column assembly of an extraction apparatus for polydatin according to the present invention;
FIG. 3 is a flow chart of the refining operation of a method for extracting polydatin according to the present invention.
In the figure: 1. a working bench; 11. a primary platen; 12. a secondary bedplate; 13. a third stage platen; 14. a pulverizer; 141. a discharge pipe; 2. an extraction barrel; 21. a stirring shaft; 22. a filter screen; 3. a swelling barrel; 31. a conical flask; 32. assembling a column assembly; 321. a pipe body; 322. a piston; 323. a precise filter screen; 324. a water pipe; 4. a stirring barrel; 5. and (5) a crystallizing barrel.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1-2, an extraction apparatus for polygonin comprises a work bench 1, wherein a
Specifically, the
Specifically, the other side of the top of the extraction barrel 2 is fixedly connected with an
Specifically, the work bench 1 is fixedly connected with a first-
Referring to fig. 3, a method for extracting polydatin includes the following steps:
s1: coarse extraction: the raw material adopts giant knotweed rhizome, the reagent adopts 95% ethanol, the dried giant knotweed rhizome is crushed by a
s2: fine extraction: soaking polyamide in 95% ethanol for 24 hours to make the polyamide absorb ethanol and swell, loading the swelled polyamide mixture into a column for cleaning, soaking in clear water, placing the cleaned swelled matter in a
s3: refining: and (3) stirring and dissolving the refined extract in the S2 by using 90% ethanol to obtain a refined solution, stirring and dissolving the refined solution by using 200-mesh and 300-mesh neutral alumina, adsorbing impurities in the refined solution by using the alumina to obtain adsorbed alumina and a refined solution after adsorption, washing and separating the adsorbed alumina to further obtain the alumina and the refined solution after adsorption, mixing the refined solution after separation and the refined solution to obtain a mixed solution, filtering to obtain a refined solution of the polydatin, standing, crystallizing and filtering to obtain the final polydatin crystal.
Specifically, the ethanol remaining in the leached filtered impurities in S1 is recovered under reduced pressure, the inside of the closed container is vacuumized by a vacuum pressure reducer to reduce the water content in the filtrate, and the filtrate is heated to evaporate the water, so that the water and the ethanol are finally separated.
Specifically, the S2 column packing operation is to fix the organic glass tube on the operation frame, cover the top end with a dense filter screen, plug the
specifically, the crystallization operation of the refined solution in S3 is to add 40% ethanol to the refined solution to dissolve and filter, and filter the refined crystal to obtain a refined filtrate and a crude crystal, cool and crystallize the refined filtrate to obtain a refined crystal, and recrystallize the crude crystal and the refined crystal to obtain a final crystal product.
The invention has the beneficial effects that: through carrying out preliminary treatment after smashing the filtration drying with the giant knotweed rhizome raw materials, avoid adsorbing the resin of too much impurity and reduce the adsorption effect to effective component polydatin, polyamide monomer diameter after abundant swelling is less, be favorable to improving resin to polydatin adsorption rate and effect in the high-precision extraction operation, and can carry out the strong effect with the cellulose impurity in the giant knotweed rhizome crude extract powder and adsorb and wash the filtration, through using neutral alumina, and adopt the alumina of fine grain diameter, make area of contact big, it is effectual to remove impurity, alumina monomer diameter is little, make adsorption impurity efficiency improve, be convenient for the large-scale production of polydatin, through adopting neutral alumina, avoid the PH value too high or low and to the corruption that causes the preparation facilities inner wall.
The using method comprises the following steps: coarse extraction: the raw material adopts giant knotweed rhizome, the reagent adopts 95% ethanol, dried giant knotweed rhizome is crushed by a crusher 14, the 95% ethanol is put into an extraction barrel 2 for extraction, the extraction operation is specifically that the crushed giant knotweed rhizome is put into the extraction barrel 2 to be heated to boiling and is stirred by a stirring shaft 21, the mixed solution after extraction is filtered by a filter screen 22, after filtrate is combined, the filtrate is subjected to vacuum drying by a vacuum drier to obtain crude extract of polydatin, the residual ethanol in the filtered impurities after extraction is subjected to reduced pressure recovery, the interior of a closed container is vacuumized by a vacuum pressure reducer to reduce the water in the filtrate, the filtrate is heated to evaporate the water, and finally the water and the ethanol are separated; fine extraction: soaking polyamide in 95% ethanol for 24 hours to enable the polyamide to absorb the ethanol to swell, performing column filling operation on a swelled polyamide mixture to clean the polyamide mixture, and soaking the polyamide mixture in clear water, wherein the column filling operation is to fix an organic glass tube on an operation frame, cover a dense filter screen at the bottom end of the organic glass tube, plug a piston 322, add distilled water, pour a swelled polyamide swelled substance into the glass tube while stirring the polyamide mixture by using a glass rod, continuously add the distilled water during the stirring period, open the piston 322 after the water surface overflows, discharge excess water from the bottom of the glass tube, always keep the water surface in the glass tube higher than the swelled substance before the polyamide swelled substance is transferred, and continuously add the distilled water for 30 minutes after the swelled substance is transferred, wherein the volume ratio of the swelled substance to a sample liquid in S2 is 1: 20, placing the washed swelling substance in an erlenmeyer flask 31, adding 80% ethanol into the crude polydatin extract in the S1 for reflux extraction, filtering and combining the filtrates, concentrating under reduced pressure, adding water with the volume being three times of the filtrate, carrying out centrifugal operation to obtain a sample liquid, pouring the sample liquid into the erlenmeyer flask 31, placing the sample liquid in a centrifugal machine for adsorption for 12 hours at room temperature, filtering to obtain a fine extract filtrate, and carrying out vacuum drying to obtain a fine polydatin extract; refining: taking the refined extract in S2, stirring and dissolving the refined extract by 90% ethanol to obtain refined solution, stirring and dissolving neutral alumina with 200-mesh particle size and 300-mesh particle size, adsorbing impurities in the refined solution by the alumina to obtain adsorbed alumina and adsorbed refined solution, washing and separating the adsorbed alumina to further obtain alumina and adsorbed refined solution, dissolving and filtering the refined solution by 40% ethanol, carrying out refined crystal suction filtration to obtain refined filtrate and crude crystals, refrigerating and crystallizing the refined filtrate to obtain refined crystals, recrystallizing the crude crystals and the refined crystals to obtain final finished crystals, mixing the separated refined solution and the refined solution to obtain mixed solution, filtering to obtain refined solution of polydatin, standing, and carrying out suction filtration to obtain the final polydatin crystals.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
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