CN113801174B - Process for recovering breviscapine from breviscapine acid precipitation waste liquid - Google Patents
Process for recovering breviscapine from breviscapine acid precipitation waste liquid Download PDFInfo
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- CN113801174B CN113801174B CN202111282868.1A CN202111282868A CN113801174B CN 113801174 B CN113801174 B CN 113801174B CN 202111282868 A CN202111282868 A CN 202111282868A CN 113801174 B CN113801174 B CN 113801174B
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- DJSISFGPUUYILV-UHFFFAOYSA-N UNPD161792 Natural products O1C(C(O)=O)C(O)C(O)C(O)C1OC(C(=C1O)O)=CC2=C1C(=O)C=C(C=1C=CC(O)=CC=1)O2 DJSISFGPUUYILV-UHFFFAOYSA-N 0.000 title claims abstract description 81
- DJSISFGPUUYILV-ZFORQUDYSA-N scutellarin Chemical compound O1[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1OC(C(=C1O)O)=CC2=C1C(=O)C=C(C=1C=CC(O)=CC=1)O2 DJSISFGPUUYILV-ZFORQUDYSA-N 0.000 title claims abstract description 81
- 239000007788 liquid Substances 0.000 title claims abstract description 64
- 239000002699 waste material Substances 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 36
- 238000003916 acid precipitation Methods 0.000 title claims abstract description 32
- 238000005406 washing Methods 0.000 claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000010805 inorganic waste Substances 0.000 claims abstract description 8
- 230000001376 precipitating effect Effects 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 39
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- 239000012065 filter cake Substances 0.000 claims description 18
- 238000001914 filtration Methods 0.000 claims description 18
- 239000003480 eluent Substances 0.000 claims description 16
- 239000002244 precipitate Substances 0.000 claims description 14
- 239000010865 sewage Substances 0.000 claims description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 12
- 239000000706 filtrate Substances 0.000 claims description 12
- 241001013934 Erigeron breviscapus Species 0.000 claims description 10
- 239000003960 organic solvent Substances 0.000 claims description 10
- 229920005654 Sephadex Polymers 0.000 claims description 9
- 239000012507 Sephadex™ Substances 0.000 claims description 8
- 238000011068 loading method Methods 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 claims description 6
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 6
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 239000000047 product Substances 0.000 claims description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 4
- 230000006837 decompression Effects 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 238000007605 air drying Methods 0.000 claims 1
- 230000007613 environmental effect Effects 0.000 abstract description 7
- 238000004134 energy conservation Methods 0.000 abstract description 4
- 239000010815 organic waste Substances 0.000 abstract description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052799 carbon Inorganic materials 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 description 8
- 239000003814 drug Substances 0.000 description 7
- 229940079593 drug Drugs 0.000 description 5
- 239000012071 phase Substances 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- NPLTVGMLNDMOQE-UHFFFAOYSA-N carthamidin Natural products C1=CC(O)=CC=C1C1OC2=CC(O)=C(O)C(O)=C2C(=O)C1 NPLTVGMLNDMOQE-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000002198 insoluble material Substances 0.000 description 2
- 238000004811 liquid chromatography Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 238000002390 rotary evaporation Methods 0.000 description 2
- 229930190376 scutellarin Natural products 0.000 description 2
- 206010002383 Angina Pectoris Diseases 0.000 description 1
- 241000208838 Asteraceae Species 0.000 description 1
- 201000006474 Brain Ischemia Diseases 0.000 description 1
- 206010008111 Cerebral haemorrhage Diseases 0.000 description 1
- 206010008120 Cerebral ischaemia Diseases 0.000 description 1
- 206010008132 Cerebral thrombosis Diseases 0.000 description 1
- 201000001429 Intracranial Thrombosis Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 206010008118 cerebral infarction Diseases 0.000 description 1
- 208000029078 coronary artery disease Diseases 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
- C07H17/06—Benzopyran radicals
- C07H17/065—Benzo[b]pyrans
- C07H17/07—Benzo[b]pyran-4-ones
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to a process for recovering breviscapine, and in particular relates to a process for recovering breviscapine from breviscapine acid precipitation waste liquid. Mainly comprises the following steps: 1) Concentrating under reduced pressure: 2) Standing and precipitating: 3) And (3) re-dissolving: 4) And (3) column passing: 5) Concentrating: 6) Washing: 7) Drying; the process is used for treating the waste liquid, recovering the breviscapine contained in the waste liquid, simultaneously converting a large amount of organic waste liquid into a small amount of inorganic waste liquid, reducing the discharge of waste, having certain economic benefit and conforming to the production concepts of energy conservation, environmental protection, green and low carbon.
Description
Technical Field
The invention belongs to a process for recovering breviscapine, and in particular relates to a process for recovering breviscapine from breviscapine acid precipitation waste liquid.
Background
The scutellarin is a flavonoid effective component extracted and separated from erigeron breviscapus (also called erigeron breviscapus) of Compositae, mainly comprises scutellarin, and is clinically used for treating diseases such as cerebral ischemia, sequelae caused by cerebral hemorrhage, hyperviscosity and lipidemia, cerebral thrombosis, coronary heart disease, angina pectoris and the like. At present, the crude drug of breviscapine is mainly purified and produced by a macroporous resin adsorption method, a large amount of acid waste liquid is generated in the production process, the waste liquid also contains approximately 50% of organic solvents such as acetone, ethanol and the like, and meanwhile, a part of breviscapine is remained in the waste liquid, so that medicinal resources are wasted when the breviscapine is directly discharged, and great pressure is brought to environmental protection.
In the prior art, chinese patent CN205974075U discloses a sewage harmless treatment system in the production process of breviscapine, which only treats waste liquid without recycling the breviscapine in the waste liquid. The Chinese patent CN103588835B uses a large amount of pure water to dilute waste liquid, so that the breviscapine precipitate is separated out, and then the breviscapine precipitate is purified by a mode of recrystallizing an organic solvent.
Disclosure of Invention
Aiming at the situation, the invention aims to provide a process for recovering the breviscapine from the breviscapine acid precipitation waste liquid, the waste liquid is treated by the process, the breviscapine contained in the waste liquid is recovered, and simultaneously, a large amount of organic waste liquid is converted into a small amount of inorganic waste liquid, so that the emission of waste is reduced, the process has certain economic benefit, and the process also accords with the production concepts of energy conservation, environmental protection and low carbon.
The technical scheme of the invention is as follows:
a process for recovering breviscapine from breviscapine acid precipitation waste liquid comprises the following steps:
1) Concentrating under reduced pressure: concentrating the acid precipitation waste liquid in the production of breviscapine under reduced pressure, and recovering the organic solvent in the waste liquid;
2) Standing and precipitating: cooling the water phase remained after the decompression concentration, standing for 12-24 hours, filtering after precipitation is completely separated out, and washing the obtained filter cake twice by pure water;
3) And (3) re-dissolving: adding 10-100 times of pure water into the precipitate according to the mass ratio, adjusting pH value to 7.0-9.0 with alkali liquor, performing ultrasonic dissolution, and filtering to remove insoluble part;
4) And (3) column passing: loading the filtrate on a sephadex column, eluting with pure water, collecting eluent, and detecting;
5) Concentrating: combining the eluents meeting the requirements, concentrating, adjusting the pH value to 1.5-2.0 by using acid, and standing for 5-24 hours until a sample is separated out;
6) Washing: filtering, and washing the obtained filter cake with pure water to neutrality;
7) And (3) drying: drying to obtain erigeron breviscapus product with purity higher than 85%.
Further, in the process for recovering breviscapine from breviscapine acid precipitation waste liquid, the organic solvent in the step 1) comprises acetone.
Further, in the process for recovering breviscapine from the breviscapine acid precipitation waste liquid, the filter cake obtained in the step 2) is washed twice by pure water, and the residual sewage does not contain organic matters, and is directly led into a sewage tank as inorganic waste liquid for sewage treatment.
Further, in the process for recovering breviscapine from the breviscapine acid precipitation waste liquid, the pure water in the step 3) is 50 times of the pure water.
Further, in the process for recovering breviscapine from the breviscapine acid precipitation waste liquid, the alkali liquor in the step 3) is selected from aqueous solution of one of sodium hydroxide, potassium hydroxide, sodium carbonate and sodium bicarbonate.
Further, in the process for recovering breviscapine from the breviscapine acid precipitation waste liquid, the pH value in the step 3) is 7.35.
Further, in the process for recovering breviscapine from the breviscapine acid precipitation waste liquid, the specification of the sephadex in the step 4) is G-10.
Further, in the process for recovering breviscapine from the breviscapine acid precipitation waste liquid, the acid in the step 5) is selected from hydrochloric acid or acetic acid.
Further, in the process for recovering breviscapine from the breviscapine acid precipitation waste liquid, the drying in the step 7) is vacuum drying or air blast drying.
Further, the process for recovering the breviscapine from the breviscapine acid precipitation waste liquid comprises the following specific steps:
1) Concentrating under reduced pressure: concentrating the acid precipitation waste liquid in the production of breviscapine under reduced pressure, and recovering an organic solvent acetone in the waste liquid;
2) Standing and precipitating: cooling the water phase remained after the decompression concentration, standing for 24 hours, filtering after precipitation is completely separated out, and washing the obtained filter cake twice by pure water; the sewage left after the washing twice does not contain organic matters, and is directly led into a sewage tank as inorganic waste liquid for sewage treatment;
3) And (3) re-dissolving: adding 50 times of pure water into the precipitate according to the mass ratio, adjusting pH to 7.35 with 10% sodium bicarbonate solution, ultrasonically dissolving at 40deg.C for 10min, and filtering to remove insoluble part;
4) And (3) column passing: loading the filtrate on G-10 sephadex column, eluting with pure water, collecting eluate, and detecting;
5) Concentrating: combining the eluents meeting the purity requirement, concentrating the combined eluents under reduced pressure at 60 ℃, regulating the ph value to 2.0 by using hydrochloric acid, and standing for 5 hours until a sample is separated out;
6) Washing: filtering, and washing the obtained filter cake with pure water to neutrality;
7) And (3) drying: vacuum drying at 50deg.C for 5 hr to obtain breviscapine product with purity of more than 85%.
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses a process for recovering breviscapine from breviscapine acid precipitation waste liquid, which is used for treating the waste liquid, recovering the breviscapine contained in the waste liquid, wherein the purity of the breviscapine is more than 85%, the breviscapine can be used as a raw material drug of the breviscapine for oral administration or used as a raw material for preparing a higher-purity raw material drug of the breviscapine, and simultaneously, a large amount of organic waste liquid is converted into a small amount of inorganic waste liquid, so that the discharge of waste is reduced, the process has certain economic benefit, and the production concepts of energy conservation, environmental protection and environmental protection are also met.
Drawings
FIG. 1 is a process flow diagram according to the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The reagents or instruments used in the examples of the present invention are conventional reagent products commercially available, without the manufacturer's knowledge.
Example 1
Taking 1000ml of acid precipitation waste liquid in the production of breviscapine, recovering the organic solvent by rotary evaporation at 50 ℃ to obtain 450ml of acetone, naturally cooling the residual water phase to room temperature by detecting the content of the acetone to be 95%, standing for 24 hours, filtering after precipitation is completely separated out, and washing the obtained filter cake twice by using a small amount of pure water to obtain 1.03g of precipitate. 50ml of pure water was added to the precipitate, ph was adjusted to 7.35 with 10% sodium bicarbonate solution, sonicated at 40℃for 10min, and insoluble material was removed by filtration.
Soaking G-10 sephadex pure water for 24 hours, removing suspended matters on the surface of the liquid after full swelling, carrying out ultrasonic degassing for 20 minutes, slowly pouring the liquid into a 10mm multiplied by 250mm glass chromatographic column, ensuring wet column packing and preventing generation of bubbles and faults, naturally settling for 1 hour, and balancing 4BV by pure water at a flow rate of 2BV/h to obtain a well-balanced chromatographic column, wherein the specification of a column bed of the chromatographic column is 10mm multiplied by 150mm.
Slowly dripping the filtered filtrate into a chromatographic column, keeping the flow rate at 2BV/h, continuing eluting with pure water at the same flow rate after the sample is loaded, collecting the filtrate from the beginning of loading in sections, and collecting 10ml of filtrate from each section until the eluent is colorless, and collecting 240ml of eluent altogether. Detecting the eluent by adopting liquid chromatography, combining the filtrates with the purity meeting the requirement, concentrating the combined eluent under reduced pressure at 60 ℃ to obtain 15ml of concentrated solution, regulating the ph value to 2.0 by using 10% hydrochloric acid, precipitating yellow precipitate, standing for 5 hours, filtering after the precipitate is completely precipitated, washing the obtained filter cake to be neutral by using pure water, and vacuum-drying the obtained filter cake at 50 ℃ for 5 hours to obtain 0.46g of breviscapine, wherein the purity of the obtained filter cake is 87.5% by liquid phase detection, and the obtained filter cake can be used as a breviscapine raw material medicine for oral administration.
Example 2
Taking 5000ml of acid precipitation waste liquid in the production of breviscapine, recovering the organic solvent by rotary evaporation at 60 ℃ to obtain 2000ml of acetone, naturally cooling the residual water phase to room temperature after detecting the content of the acetone to be 96%, standing for 24 hours, filtering after precipitation is completely separated out, and washing the obtained filter cake twice with a small amount of pure water to obtain 5.43g of precipitate. To the precipitate was added 250ml of pure water, ph was adjusted to 7.35 with 10% sodium bicarbonate solution, sonicated at 40 ℃ for 10min, and insoluble material was removed by filtration.
And (3) taking the fully processed G-10 sephadex, slowly pouring the sephadex into a 30mm multiplied by 500mm glass chromatographic column, ensuring the wet column loading and preventing the generation of bubbles and faults, naturally settling for 1h, and balancing 4BV by using pure water at the flow rate of 2BV/h to obtain a well-balanced chromatographic column, wherein the specification of the column bed of the chromatographic column is 30mm multiplied by 350mm.
Slowly dripping the filtered filtrate into a chromatographic column, keeping the flow rate at 2BV/h, continuing to elute with pure water at the same flow rate after the sample is loaded, collecting the filtrate from the beginning of loading in sections, and collecting 100ml of filtrate from each section until the eluent is colorless, and collecting 1000ml of eluent altogether. Detecting the eluent by adopting liquid chromatography, combining the filtrates with the purity meeting the requirement, concentrating the combined eluent under reduced pressure at 60 ℃ to obtain 40ml of concentrated solution, regulating the ph value to 2.0 by using 10% hydrochloric acid, precipitating yellow precipitate, standing for 5 hours, filtering after the precipitate is completely precipitated, washing the obtained filter cake to be neutral by using pure water, and vacuum-drying the obtained filter cake at 50 ℃ for 5 hours to obtain 1.97g of breviscapine, wherein the purity of the breviscapine is 86.5% by liquid phase detection, and the breviscapine can be used as a breviscapine raw material medicine for oral administration.
According to the results of examples 1 and 2, it can be seen that the process treats the waste liquid, recovers the breviscapine contained in the waste liquid, has a purity of more than 85%, can be used as a raw material drug of the breviscapine for oral administration or as a raw material for preparing a raw material drug of the breviscapine with higher purity, and simultaneously converts a large amount of organic waste liquid into a small amount of inorganic waste liquid, thereby reducing the discharge of waste, having certain economic benefit, and conforming to the production concepts of energy conservation, environmental protection and environmental protection.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (10)
1. A process for recovering breviscapine from breviscapine acid precipitation waste liquid is characterized by comprising the following steps:
1) Concentrating under reduced pressure: concentrating the acid precipitation waste liquid in the production of breviscapine under reduced pressure, and recovering the organic solvent in the waste liquid;
2) Standing and precipitating: cooling the water phase remained after the decompression concentration, standing for 12-24 hours, filtering after precipitation is completely separated out, and washing the obtained filter cake twice by pure water;
3) And (3) re-dissolving: adding 10-100 times of pure water into the precipitate according to the mass ratio, adjusting pH value to 7.0-9.0 with alkali liquor, performing ultrasonic dissolution, and filtering to remove insoluble part;
4) And (3) column passing: loading the filtrate on a sephadex column, eluting with pure water, collecting eluent, and detecting;
5) Concentrating: combining the eluents meeting the requirements, concentrating, adjusting the pH value to 1.5-2.0 by using acid, and standing for 5-24 hours until a sample is separated out;
6) Washing: filtering, and washing the obtained filter cake with pure water to neutrality;
7) And (3) drying: drying to obtain erigeron breviscapus product with purity higher than 85%.
2. The process for recovering breviscapine from erigeron breviscapus acid precipitation waste liquid according to claim 1, wherein said organic solvent in step 1) comprises acetone.
3. The process for recovering breviscapine from breviscapine acid precipitation waste liquid as claimed in claim 1, wherein said filter cake obtained in said step 2) is washed twice with pure water, and the residual sewage does not contain organic matters, and is directly introduced into a sewage tank as an inorganic waste liquid for sewage treatment.
4. The process for recovering breviscapine from erigeron breviscapus acid precipitation waste liquid as claimed in claim 1, wherein the amount of pure water in said step 3) is 50 times.
5. The process for recovering breviscapine from erigeron breviscapus acid precipitation waste liquid as claimed in claim 1, wherein said alkali solution in said step 3) is selected from aqueous solution of one of sodium hydroxide, potassium hydroxide, sodium carbonate and sodium bicarbonate.
6. The process for recovering breviscapine from erigeron breviscapus acid precipitation waste liquid as claimed in claim 1, wherein the pH value in said step 3) is 7.35.
7. The process for recovering breviscapine from breviscapine acid precipitation waste liquid as claimed in claim 1, wherein the dextran gel specification in said step 4) is G-10.
8. The process for recovering breviscapine from erigeron breviscapus acid precipitation waste liquid according to claim 1, wherein the acid in said step 5) is selected from hydrochloric acid and acetic acid.
9. The process for recovering breviscapine from erigeron breviscapus acid precipitation waste liquid as claimed in claim 1, wherein said drying in step 7) is vacuum drying or air drying.
10. The process for recovering breviscapine from breviscapine acid precipitation waste liquid as claimed in claim 1, comprising the following specific steps:
1) Concentrating under reduced pressure: concentrating the acid precipitation waste liquid in the production of breviscapine under reduced pressure, and recovering an organic solvent acetone in the waste liquid;
2) Standing and precipitating: cooling the water phase remained after the decompression concentration, standing for 24 hours, filtering after precipitation is completely separated out, and washing the obtained filter cake twice by pure water; the sewage left after the washing twice does not contain organic matters, and is directly led into a sewage tank as inorganic waste liquid for sewage treatment;
3) And (3) re-dissolving: adding 50 times of pure water into the precipitate according to the mass ratio, adjusting pH to 7.35 with 10% sodium bicarbonate solution, ultrasonically dissolving at 40deg.C for 10min, and filtering to remove insoluble part;
4) And (3) column passing: loading the filtrate on G-10 sephadex column, eluting with pure water, collecting eluate, and detecting;
5) Concentrating: combining the eluents meeting the purity requirement, concentrating the combined eluents under reduced pressure at 60 ℃, regulating the ph value to 2.0 by using hydrochloric acid, and standing for 5 hours until a sample is separated out;
6) Washing: filtering, and washing the obtained filter cake with pure water to neutrality;
7) And (3) drying: vacuum drying at 50deg.C for 5 hr to obtain breviscapine product with purity of more than 85%.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005085255A1 (en) * | 2004-03-04 | 2005-09-15 | Nihon University | The extract of bulbophgllum radiatum lindl and the preparation and the use |
| CN101747395A (en) * | 2009-12-25 | 2010-06-23 | 中国医药集团总公司四川抗菌素工业研究所 | Method for preparing high-purity scutellarin |
| CN103588835A (en) * | 2013-11-14 | 2014-02-19 | 昆明理工大学 | Method for recycling scutellarin from waste liquid of acid sediment |
-
2021
- 2021-11-01 CN CN202111282868.1A patent/CN113801174B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005085255A1 (en) * | 2004-03-04 | 2005-09-15 | Nihon University | The extract of bulbophgllum radiatum lindl and the preparation and the use |
| CN101747395A (en) * | 2009-12-25 | 2010-06-23 | 中国医药集团总公司四川抗菌素工业研究所 | Method for preparing high-purity scutellarin |
| CN103588835A (en) * | 2013-11-14 | 2014-02-19 | 昆明理工大学 | Method for recycling scutellarin from waste liquid of acid sediment |
Non-Patent Citations (1)
| Title |
|---|
| 叶萌.灯盏花：预防和治疗心脑血管病的天赐良药.云南科学技术出版社,2007,116. * |
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