CN109096131B - Process for preparing levodopa by utilizing velvet beans - Google Patents
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- CN109096131B CN109096131B CN201811136998.2A CN201811136998A CN109096131B CN 109096131 B CN109096131 B CN 109096131B CN 201811136998 A CN201811136998 A CN 201811136998A CN 109096131 B CN109096131 B CN 109096131B
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- WTDRDQBEARUVNC-LURJTMIESA-N L-DOPA Chemical compound OC(=O)[C@@H](N)CC1=CC=C(O)C(O)=C1 WTDRDQBEARUVNC-LURJTMIESA-N 0.000 title claims abstract description 79
- WTDRDQBEARUVNC-UHFFFAOYSA-N L-Dopa Natural products OC(=O)C(N)CC1=CC=C(O)C(O)=C1 WTDRDQBEARUVNC-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 229960004502 levodopa Drugs 0.000 title claims abstract description 79
- 244000111261 Mucuna pruriens Species 0.000 title claims abstract description 23
- 235000008540 Mucuna pruriens var utilis Nutrition 0.000 title claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 33
- 244000046052 Phaseolus vulgaris Species 0.000 claims abstract description 21
- 235000010627 Phaseolus vulgaris Nutrition 0.000 claims abstract description 20
- 235000012054 meals Nutrition 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000007598 dipping method Methods 0.000 claims abstract description 17
- 229920001661 Chitosan Polymers 0.000 claims abstract description 14
- 241000252233 Cyprinus carpio Species 0.000 claims abstract description 14
- 241000282326 Felis catus Species 0.000 claims abstract description 14
- 239000012535 impurity Substances 0.000 claims abstract description 14
- 238000000194 supercritical-fluid extraction Methods 0.000 claims abstract description 14
- 241000255789 Bombyx mori Species 0.000 claims abstract description 13
- 241000238557 Decapoda Species 0.000 claims abstract description 13
- 108010073771 Soybean Proteins Proteins 0.000 claims abstract description 13
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000001509 sodium citrate Substances 0.000 claims abstract description 11
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims abstract description 11
- 239000011975 tartaric acid Substances 0.000 claims abstract description 11
- 235000002906 tartaric acid Nutrition 0.000 claims abstract description 11
- 229940001941 soy protein Drugs 0.000 claims abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 30
- 238000000926 separation method Methods 0.000 claims description 30
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 27
- 238000001914 filtration Methods 0.000 claims description 22
- 238000000605 extraction Methods 0.000 claims description 21
- 239000007788 liquid Substances 0.000 claims description 20
- 239000002244 precipitate Substances 0.000 claims description 19
- 239000013078 crystal Substances 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 17
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 16
- 239000012043 crude product Substances 0.000 claims description 15
- 239000000047 product Substances 0.000 claims description 15
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 14
- 238000000746 purification Methods 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 12
- 238000000909 electrodialysis Methods 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 11
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 claims description 8
- 229930003268 Vitamin C Natural products 0.000 claims description 8
- 210000000582 semen Anatomy 0.000 claims description 8
- 239000011718 vitamin C Substances 0.000 claims description 8
- 235000019154 vitamin C Nutrition 0.000 claims description 8
- 239000001569 carbon dioxide Substances 0.000 claims description 7
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 7
- 238000002791 soaking Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 230000001376 precipitating effect Effects 0.000 claims description 6
- 235000019710 soybean protein Nutrition 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 5
- 238000010298 pulverizing process Methods 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 abstract description 5
- 238000003815 supercritical carbon dioxide extraction Methods 0.000 abstract description 4
- 239000010865 sewage Substances 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 45
- 238000002386 leaching Methods 0.000 description 7
- 235000019441 ethanol Nutrition 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- -1 phenylalanine compound Chemical class 0.000 description 3
- 150000008442 polyphenolic compounds Chemical class 0.000 description 3
- 235000013824 polyphenols Nutrition 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 description 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 2
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 2
- 239000001263 FEMA 3042 Substances 0.000 description 2
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 description 2
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 2
- 239000001099 ammonium carbonate Substances 0.000 description 2
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 2
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 2
- 235000011130 ammonium sulphate Nutrition 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 210000000078 claw Anatomy 0.000 description 2
- 239000012065 filter cake Substances 0.000 description 2
- 229930003944 flavone Natural products 0.000 description 2
- 150000002212 flavone derivatives Chemical class 0.000 description 2
- 235000011949 flavones Nutrition 0.000 description 2
- 229930003935 flavonoid Natural products 0.000 description 2
- 235000017173 flavonoids Nutrition 0.000 description 2
- 235000018102 proteins Nutrition 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 description 2
- 235000010262 sodium metabisulphite Nutrition 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 description 2
- 229940033123 tannic acid Drugs 0.000 description 2
- 235000015523 tannic acid Nutrition 0.000 description 2
- 229920002258 tannic acid Polymers 0.000 description 2
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 235000019750 Crude protein Nutrition 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 235000010469 Glycine max Nutrition 0.000 description 1
- 244000068988 Glycine max Species 0.000 description 1
- 241000122904 Mucuna Species 0.000 description 1
- 241000282376 Panthera tigris Species 0.000 description 1
- 208000018737 Parkinson disease Diseases 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 1
- 229940044197 ammonium sulfate Drugs 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 235000019784 crude fat Nutrition 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000035558 fertility Effects 0.000 description 1
- 241000411851 herbal medicine Species 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 235000021332 kidney beans Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- COLNVLDHVKWLRT-UHFFFAOYSA-N phenylalanine Natural products OC(=O)C(N)CC1=CC=CC=C1 COLNVLDHVKWLRT-UHFFFAOYSA-N 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 229940001584 sodium metabisulfite Drugs 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 1
- 239000000341 volatile oil Substances 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/38—Separation; Purification; Stabilisation; Use of additives
- C07C227/40—Separation; Purification
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01K—ANIMAL HUSBANDRY; AVICULTURE; APICULTURE; PISCICULTURE; FISHING; REARING OR BREEDING ANIMALS, NOT OTHERWISE PROVIDED FOR; NEW BREEDS OF ANIMALS
- A01K97/00—Accessories for angling
- A01K97/04—Containers for bait; Preparation of bait
- A01K97/045—Preparation of bait; Ingredients
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/07—Optical isomers
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental Sciences (AREA)
- Animal Husbandry (AREA)
- Biodiversity & Conservation Biology (AREA)
- Fodder In General (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses a process for preparing levodopa by utilizing velvet beans, which comprises the following steps: (1) pre-treating; (2) dipping and extracting: putting the cat beans into the extracting solution, performing supercritical carbon dioxide extraction by adopting ultrasonic assistance, and separating to obtain an extract I and an extract II; taking out the residue and the extract obtained in the supercritical extraction kettle, mixing with the isolated soy protein, chitosan, silkworm chrysalis meal and shrimp meal, and granulating to obtain carp bait; the extracting solution consists of citric acid, tartaric acid, sodium citrate and water; (3) concentrating; (4) removing impurities; (5) separating; (6) collecting; (7) and (5) purifying. The levodopa prepared by the levodopa preparation process has high purity which is up to more than 98.5%. According to the invention, the residue and the extracting solution after the supercritical extraction of the cat beans are utilized to prepare the carp bait, so that the resources are fully utilized, and the problem of sewage pollution is avoided.
Description
Technical Field
The invention relates to the technical field of Chinese herbal medicine processing, and in particular relates to a process for preparing levodopa by utilizing velvet beans.
Background
The catbeans, also named mucuna, velvet dragon, tiger claw beans and dog claw beans, are drought-enduring crops with strong adaptability, have a plurality of rhizobia at the roots, can improve the soil fertility, have developed root systems, climb up the leaves and tendrils, have wide coverage and are beneficial to keeping water and soil. The whole body of the cat bean is treasure, and the bean shells, the bean leaves and the bean seeds are rich in crude fat and crude protein, so that the cat bean is superior pig feed. The bean seeds are the raw material for producing levodopa. Levodopa is a main medicine for treating paralysis agitans, and is mainly extracted from plants such as kidney beans in domestic production. Levodopa is a phenylalanine compound, is easily soluble in water, is insoluble in organic solvents such as ethanol and the like, and has stable o-diphenol hydroxyl in molecules under acidic conditions, is easy to condense under neutral and alkaline conditions, and is easy to oxidize when encountering high temperature. In the prior art, levodopa is mainly extracted by an acid-water-alcohol method, a large amount of ethanol is consumed in the process, and the heating and concentrating time is long. At present, acid water extraction is mainly used, but the purity and the extraction rate of the levodopa are greatly influenced due to the fact that the levodopa contains a large amount of water-soluble impurities.
For example, patent CN201611023242.8 discloses a method for extracting levodopa from semen Stizolobii Cochin chinensis, comprising crushing semen Stizolobii Cochin chinensis, placing into a reaction kettle containing ammonium bicarbonate, ammonium sulfate, tannic acid and sodium pyrosulfite aqueous solution, pressurizing with carbon dioxide, heating, and leaching to obtain extractive solution and semen Stizolobii Cochin chinensis residue; precipitating the extractive solution with chitosan, filtering, primarily separating impurities, concentrating the filtrate under reduced pressure, and separating out crude product; and leaching the crude product with an ethanol solution, recovering the ethanol after leaching, taking a filter cake, purifying the filter cake by adopting a traditional refining process, standing, separating out crystals, filtering to obtain the crystals, and drying to obtain the levodopa with the content of not less than 99% and the yield of not less than 3%. The method can improve the product yield from 2.5 percent to 3 percent, reduce the discharge amount of the acid-alkali containing wastewater by over 95 percent and save 60 percent of labor force. However, the extracting solution is extracted by taking ammonium bicarbonate, ammonium sulfate, tannic acid and sodium metabisulfite as solvents, so that the ammonia nitrogen content is increased when acid-base wastewater is discharged, and the difficulty of sewage treatment is increased. The waste of the technology for extracting levodopa from the cat beans is rich in flavone and protein substances, and if the waste can be utilized, the comprehensive utilization rate of the waste resources can be further improved.
Disclosure of Invention
The invention overcomes the technical problems of low purity of levodopa obtained by a process for extracting levodopa by acid water, easy environmental pollution and the like in the prior art, and provides a process for preparing levodopa by using velvet beans.
In order to solve the problems, the invention adopts the following technical scheme:
a process for preparing levodopa by using velvet beans comprises the following steps:
(1) pretreatment: cleaning semen Stizolobii Cochinchinensis, removing impurities, pulverizing, and sieving with 80 mesh sieve;
(2) dipping and extracting: placing the cat beans in an extracting solution, soaking for 8 hours after ultrasonic treatment is carried out for 40-50 minutes, transferring the cat beans to a supercritical reaction kettle, extracting for 20-35 minutes under the conditions that the extraction pressure is 55-60 mpa, the extraction temperature is 60-75 ℃, the flow rate of carbon dioxide is 15L/min, extracting and separating at the temperature of 5-9 mpa and the temperature of 25 ℃ under the conditions that the pressure of a separation kettle I is 10-20 mpa, the temperature of 40-50 ℃ and the pressure of a separation kettle II are 10-9 mpa, and the separation kettle I is used for separating to obtain an extract I and an extract II is obtained by separating the separation kettle II; taking out the residue and the extract obtained in the supercritical extraction kettle, mixing with the isolated soy protein, chitosan, silkworm chrysalis meal and shrimp meal, and granulating to obtain carp bait; the extracting solution comprises, by mass, 1-5% of citric acid, 3-5% of tartaric acid, 10-15% of sodium citrate and the balance of water;
(3) concentration: concentrating the extract II obtained in the step (2) under reduced pressure to separate out crystals to obtain a levodopa crude product and an uncrystallized solution;
(4) removing impurities: mixing the extract I with the solution not crystallized in the step (3), adding activated carbon, heating to 40-50 ℃, preserving heat for 2-5 hours, and filtering to remove the activated carbon;
(5) separation: adjusting the pH value of the mixture obtained in the step (4) to 1-4, separating by using an electrodialysis device, controlling the operating voltage and current, detecting the material opening at intervals, stopping electrodialysis when the mixture does not show levodopa any more when the mixture does not show levodopa, and collecting the feed liquid for later use;
(6) collecting: adjusting the pH value of the feed liquid obtained in the step (5) to 4.0, placing at a high temperature of 80-90 ℃ for 20-30 h, filtering, and collecting precipitates;
(7) and (3) purification: and (3) dissolving the precipitate obtained in the step (6) and the levodopa crude product obtained in the step (3) in a leaching solution, heating to 40-50 ℃, filtering while hot, collecting filtrate, standing at a low temperature of 0-4 ℃, precipitating crystals, filtering, washing the crystals with a small amount of absolute ethyl alcohol, and drying at a temperature below 50 ℃ to obtain the finished product.
Wherein, the purification liquid in the step (7) is: by taking the total mass of the precipitate and the crude levodopa product as a reference, 0.05-0.2% of vitamin C, 0.05-0.2% of acetic acid and 3-8 times of water of the total mass of the precipitate and the crude levodopa product.
Wherein the solid-to-liquid ratio of the catbeans to the extracting solution is 1 kg: 0.5 to 1L.
And (3) adding the activated carbon in the step (4) in an amount which is 3-5% of the total mass of the extract I and the uncrystallized solution in the step (3) after mixing.
Wherein the power of the ultrasonic wave in the step (2) is 500W, and the irradiation temperature of the ultrasonic wave is 50-55 ℃.
Wherein in the dipping process in the step (2), the dipping temperature is 40-50 ℃.
The carp bait is prepared by mixing the following raw materials in parts by mass: 1-3 parts of residue and extracting solution obtained in the supercritical extraction kettle, 20-30 parts of soybean protein isolate, 5-8 parts of chitosan, 3-7 parts of silkworm chrysalis powder and 1-6 parts of shrimp powder.
Compared with the prior art, the invention has the following beneficial effects:
(1) the method comprises the steps of firstly carrying out ultrasonic irradiation dipping on an extracting solution composed of citric acid, tartaric acid, sodium citrate and water, then carrying out supercritical carbon dioxide extraction separation to obtain an extract I and an extract II, wherein the extract I contains high-purity levodopa such as polyphenol, flavone and volatile oil, the extract II contains high-purity levodopa, the extract II can directly separate out a levodopa crude product, the extract I and the extract II separate out levodopa crystals, then mixing the obtained solution with an uncrystallized solution, removing impurities, carrying out electrodialysis separation and purification, and finally mixing the obtained product with the levodopa crude product, and then carrying out dissolution and purification by using a purifying solution composed of water, vitamin C and acetic acid, so that the prepared levodopa has high purity which is more than 98.5%, and the extraction rate of the levodopa is high and can be more than 85.0%. According to the invention, the residue and the extracting solution after the supercritical extraction of the cat beans are utilized and mixed with the isolated soy protein, the chitosan, the silkworm chrysalis meal and the shrimp meal to obtain the carp bait, and resources are fully utilized. The process for preparing levodopa by utilizing the velvet beans does not cause the problem of sewage pollution.
(2) According to the invention, the carp bait is obtained by mixing the residue and the extracting solution obtained after the green soy beans are extracted in the supercritical extraction kettle, the soybean protein isolate, the chitosan, the silkworm chrysalis meal and the shrimp meal, wherein the residue contains rich unsaturated fatty acid, protein and various mineral substances, the extracting solution contains polyphenol, flavonoid compounds, citric acid and tartaric acid, the polyphenol, the flavonoid compounds, the citric acid and the tartaric acid can soften the silkworm chrysalis meal and the shrimp meal, the oxidative deterioration of the soybean protein isolate is prevented, and the chitosan can improve the agglomeration of the carp bait.
Detailed Description
The present invention will be further described with reference to examples and tests.
Example 1
A process for preparing levodopa by using velvet beans comprises the following steps:
(1) pretreatment: cleaning semen Stizolobii Cochinchinensis, removing impurities, pulverizing, and sieving with 80 mesh sieve;
(2) dipping and extracting: placing the cat beans in an extracting solution, performing ultrasonic treatment for 50min by adopting ultrasonic waves, soaking for 8h, transferring to a supercritical reaction kettle, extracting for 20min at the extraction pressure of 55mpa and the extraction temperature of 75 ℃ and at the flow rate of 15L/min of carbon dioxide, extracting and separating at the temperature of 25 ℃ and the pressure of 20mpa in a separation kettle I at the temperature of 40 ℃ and the pressure of 9mpa in a separation kettle II, separating in the separation kettle I to obtain an extract I, and separating in the separation kettle II to obtain an extract II; taking out the residue and the extract obtained in the supercritical extraction kettle, mixing with the isolated soy protein, chitosan, silkworm chrysalis meal and shrimp meal, and granulating to obtain carp bait; the extracting solution comprises, by mass, 5% of citric acid, 3% of tartaric acid, 15% of sodium citrate and the balance of water; the solid-liquid ratio of the catbeans to the extracting solution is 1 kg: 0.5L; the power of the ultrasonic wave is 500W, and the irradiation temperature of the ultrasonic wave is 55 ℃; in the dipping process in the step (2), the dipping temperature is 40 ℃.
(3) Concentration: concentrating the extract II obtained in the step (2) under reduced pressure to separate out crystals to obtain a levodopa crude product and an uncrystallized solution;
(4) removing impurities: mixing the extract I with the uncrystallized solution obtained in the step (3), adding activated carbon, heating to 50 ℃, keeping the temperature for 2 hours, and filtering to remove the activated carbon; the adding amount of the activated carbon is 5% of the total mass of the extract I and the non-crystallized solution in the step (3);
(5) separation: adjusting the pH value of the mixture obtained in the step (4) to 1, separating by using an electrodialysis device, controlling the operating voltage and current, detecting the material opening at intervals, stopping electrodialysis when the mixture does not show levodopa reaction any more, and collecting the feed liquid for later use;
(6) collecting: adjusting the pH value of the feed liquid obtained in the step (5) to 4.0, standing at a high temperature of 90 ℃ for 20h, filtering, and collecting precipitates;
(7) and (3) purification: dissolving the precipitate obtained in the step (6) and the levodopa crude product obtained in the step (3) in a leaching solution, heating to 50 ℃, filtering while hot, collecting filtrate, standing at a low temperature of 0 ℃, precipitating crystals, filtering, washing the crystals with a small amount of absolute ethyl alcohol, and drying at a temperature below 50 ℃ to obtain a finished product; the purification liquid is as follows: based on the total mass of the precipitate and the crude levodopa product, 0.05 percent of vitamin C, 0.2 percent of acetic acid and 8 times of water are used as the total mass of the precipitate and the crude levodopa product.
Example 2
A process for preparing levodopa by using velvet beans comprises the following steps:
(1) pretreatment: cleaning semen Stizolobii Cochinchinensis, removing impurities, pulverizing, and sieving with 80 mesh sieve;
(2) dipping and extracting: placing the cat beans in an extracting solution, soaking for 8 hours after ultrasonic treatment is carried out for 40 minutes by ultrasonic waves, transferring the cat beans to a supercritical reaction kettle, extracting for 35 minutes under the conditions that the extracting pressure is 60mpa, the extracting temperature is 60 ℃, the flow rate of carbon dioxide is 15L/min, extracting and separating at the temperature of 25 ℃ under the conditions that the pressure of a separation kettle I is 10mpa, the temperature is 50 ℃, the pressure of a separation kettle II is 5mpa, and extracting and separating are carried out in the separation kettle I to obtain an extract I, and separating in the separation kettle II to obtain an extract II; taking out the residue and the extract obtained in the supercritical extraction kettle, mixing with the isolated soy protein, chitosan, silkworm chrysalis meal and shrimp meal, and granulating to obtain carp bait; the extracting solution comprises 1% of citric acid, 5% of tartaric acid, 10% of sodium citrate and the balance of water by mass percentage; the solid-liquid ratio of the catbeans to the extracting solution is 1 kg: 1L; the power of the ultrasonic wave is 500W, and the irradiation temperature of the ultrasonic wave is 50 ℃; in the dipping process in the step (2), the dipping temperature is 50 ℃.
(3) Concentration: concentrating the extract II obtained in the step (2) under reduced pressure to separate out crystals to obtain a levodopa crude product and an uncrystallized solution;
(4) removing impurities: mixing the extract I with the uncrystallized solution obtained in the step (3), adding activated carbon, heating to 40 ℃, keeping the temperature for 5 hours, and filtering to remove the activated carbon; the adding amount of the activated carbon is 3% of the total mass of the extract I and the non-crystallized solution in the step (3);
(5) separation: adjusting the pH value of the mixture obtained in the step (4) to 4, separating by using an electrodialysis device, controlling the operating voltage and current, detecting the material opening at intervals, stopping electrodialysis when the mixture does not show levodopa reaction any more, and collecting the feed liquid for later use;
(6) collecting: adjusting the pH value of the feed liquid obtained in the step (5) to 4.0, standing at the high temperature of 80 ℃ for 30h, filtering, and collecting precipitates;
(7) and (3) purification: dissolving the precipitate obtained in the step (6) and the levodopa crude product obtained in the step (3) in a leaching solution, heating to 40 ℃, filtering while hot, collecting filtrate, standing at a low temperature of 4 ℃, precipitating crystals, filtering, washing the crystals with a small amount of absolute ethyl alcohol, and drying at a temperature below 50 ℃ to obtain a finished product; the purification liquid is as follows: based on the total mass of the precipitate and the crude levodopa product, 0.2 percent of vitamin C, 0.05 percent of acetic acid and 3 times of water of the total mass of the precipitate and the crude levodopa product.
In the step (2), in the soaking and extracting, the carp bait is prepared by mixing the following raw materials in parts by mass: 3 parts of residue and extract obtained in the supercritical extraction kettle, 20 parts of soybean protein isolate, 8 parts of chitosan, 3 parts of silkworm chrysalis powder and 6 parts of shrimp meal.
Example 3
A process for preparing levodopa by using velvet beans comprises the following steps:
(1) pretreatment: cleaning semen Stizolobii Cochinchinensis, removing impurities, pulverizing, and sieving with 80 mesh sieve;
(2) dipping and extracting: placing the cat beans in an extracting solution, performing ultrasonic treatment for 45min by adopting ultrasonic waves, soaking for 8h, transferring to a supercritical reaction kettle, extracting for 30min at the extraction pressure of 58mpa and the extraction temperature of 70 ℃ and at the flow rate of 15L/min of carbon dioxide, performing extraction and separation at the temperature of 25 ℃ and the pressure of 15mpa and the temperature of 45 ℃ in a separation kettle I, separating in the separation kettle I to obtain an extract I, and separating in the separation kettle II to obtain an extract II; taking out the residue and the extract obtained in the supercritical extraction kettle, mixing with the isolated soy protein, chitosan, silkworm chrysalis meal and shrimp meal, and granulating to obtain carp bait; the extracting solution comprises 3% of citric acid, 4% of tartaric acid, 12% of sodium citrate and the balance of water by mass percentage; the solid-liquid ratio of the catbeans to the extracting solution is 1 kg: 0.8L; the power of the ultrasonic wave is 500W, and the irradiation temperature of the ultrasonic wave is 52 ℃; in the dipping process of the step (2), the dipping temperature is 45 ℃.
(3) Concentration: concentrating the extract II obtained in the step (2) under reduced pressure to separate out crystals to obtain a levodopa crude product and an uncrystallized solution;
(4) removing impurities: mixing the extract I with the uncrystallized solution obtained in the step (3), adding activated carbon, heating to 48 ℃, keeping the temperature for 4 hours, and filtering to remove the activated carbon; the adding amount of the activated carbon is 4% of the total mass of the extract I and the non-crystallized solution in the step (3);
(5) separation: adjusting the pH value of the mixture obtained in the step (4) to 3, separating by using an electrodialysis device, controlling the operating voltage and current, detecting the material opening at intervals, stopping electrodialysis when the mixture does not show levodopa reaction any more, and collecting the feed liquid for later use;
(6) collecting: adjusting the pH value of the feed liquid obtained in the step (5) to 4.0, standing at 85 ℃ for 25h, filtering, and collecting precipitates;
(7) and (3) purification: dissolving the precipitate obtained in the step (6) and the levodopa crude product obtained in the step (3) in a leaching solution, heating to 45 ℃, filtering while hot, collecting filtrate, standing at a low temperature of 2 ℃, precipitating crystals, filtering, washing the crystals with a small amount of absolute ethyl alcohol, and drying at a temperature below 50 ℃ to obtain a finished product; the purification liquid is as follows: based on the total mass of the precipitate and the crude levodopa product, 0.1 percent of vitamin C, 0.1 percent of acetic acid and 6 times of water of the total mass of the precipitate and the crude levodopa product.
In the step (2), in the soaking and extracting, the carp bait is prepared by mixing the following raw materials in parts by mass: 2 parts of residue and extracting solution obtained in the supercritical extraction kettle, 25 parts of soybean protein isolate, 6 parts of chitosan, 6 parts of silkworm chrysalis powder and 5 parts of shrimp meal.
To illustrate the technical effect set of the present invention, the following control groups were set up:
control group 1
The method for preparing levodopa using velvet beans in control 1 was substantially the same as in example 1, except that the extract of control 1 did not contain sodium citrate.
Control group 2
The method for preparing levodopa by using the velvet beans in the comparison group 2 is basically the same as that in the example 1, except that the extracting solution of the comparison group 2 consists of acetic acid, sodium citrate and water, the mass percentage content of the acetic acid is the same as that of the total mass percentage content of citric acid and tartaric acid in the example 1, and the mass percentage content of the sodium citrate is the same as that in the example 1.
Control group 3
The method for preparing levodopa using velvet beans in control 3 was substantially the same as in example 1, except that the purified solution of control 3 did not contain vitamin C.
Control group 4
The method for preparing levodopa by using velvet beans in the control group 4 is basically the same as that in the example 1, except that the velvet beans in the control group 4 are extracted at the supercritical extraction pressure of 25mpa, the extraction temperature of 30 ℃ and the flow rate of carbon dioxide of 15L/min for 30 min.
Control group 5
The method for preparing levodopa using velvet beans in control 5 was substantially the same as in example 1, except that the supercritical reaction tank in control 5 had a separation tank I pressure of 25mpa and a temperature of 65 ℃.
Control group 6
The method for preparing levodopa using velvet beans in control 6 was substantially the same as in example 1 except that the pressure of the ultra-separation tank II in control 6 was 15mpa and the temperature was 35 ℃.
The purity and extraction rate of levodopa obtained by the preparation of examples 1 to 3 and controls 1 to 6 are shown in table 1 below.
TABLE 1
As is clear from table 1, examples 1 to 3 showed high purity and extraction rate, particularly high extraction rate of levodopa as compared with control 1 to 2, indicating that the present invention showed high extraction rate of levodopa obtained by immersing an extract solution composed of citric acid, tartaric acid, sodium citrate and water and then performing supercritical carbon dioxide extraction, and examples 1 to 3 showed high purity and extraction rate, particularly high purity, as compared with control 3, indicating that the present invention showed high purity of levodopa obtained by purifying with a purification solution composed of water, vitamin C and acetic acid. Examples 1 to 3 show that the purity and extraction rate of levodopa are high, especially the extraction rate is relatively high, compared with the control groups 4 to 6, which indicates that the levodopa prepared by extraction under supercritical carbon dioxide extraction conditions and separation conditions adopted by the invention has high content, and can improve the extraction rate of levodopa.
The above description is intended to describe in detail the preferred embodiments of the present invention, but the embodiments are not intended to limit the scope of the claims of the present invention, and all equivalent changes and modifications made within the technical spirit of the present invention should fall within the scope of the claims of the present invention.
Claims (6)
1. A process for preparing levodopa by utilizing velvet beans is characterized by comprising the following steps:
(1) pretreatment: cleaning semen Stizolobii Cochinchinensis, removing impurities, pulverizing, and sieving with 80 mesh sieve;
(2) dipping and extracting: placing the cat beans in an extracting solution, soaking for 8 hours after ultrasonic treatment is carried out for 40-50 minutes, transferring the cat beans to a supercritical reaction kettle, extracting for 20-35 minutes under the conditions that the extraction pressure is 55-60 mpa, the extraction temperature is 60-75 ℃, the flow rate of carbon dioxide is 15L/min, extracting and separating at the temperature of 5-9 mpa and the temperature of 25 ℃ under the conditions that the pressure of a separation kettle I is 10-20 mpa, the temperature of 40-50 ℃ and the pressure of a separation kettle II are 10-9 mpa, and the separation kettle I is used for separating to obtain an extract I and an extract II is obtained by separating the separation kettle II; taking out the residue and the extract obtained in the supercritical extraction kettle, mixing with the isolated soy protein, chitosan, silkworm chrysalis meal and shrimp meal, and granulating to obtain carp bait; the extracting solution comprises, by mass, 1-5% of citric acid, 3-5% of tartaric acid, 10-15% of sodium citrate and the balance of water;
(3) concentration: concentrating the extract II obtained in the step (2) under reduced pressure to separate out crystals to obtain a levodopa crude product and an uncrystallized solution;
(4) removing impurities: mixing the extract I with the solution not crystallized in the step (3), adding activated carbon, heating to 40-50 ℃, preserving heat for 2-5 hours, and filtering to remove the activated carbon;
(5) separation: adjusting the pH value of the mixture obtained in the step (4) to 1-4, separating by using an electrodialysis device, controlling the operating voltage and current, detecting the discharge hole at intervals, stopping electrodialysis when the mixture does not show levodopa any more in reaction, and collecting feed liquid for later use;
(6) collecting: adjusting the pH value of the feed liquid obtained in the step (5) to 4.0, placing at a high temperature of 80-90 ℃ for 20-30 h, filtering, and collecting precipitates;
(7) and (3) purification: dissolving the precipitate obtained in the step (6) and the levodopa crude product obtained in the step (3) in a purification solution, heating to 40-50 ℃, filtering while hot, collecting filtrate, standing at a low temperature of 0-4 ℃, precipitating crystals, filtering, washing the crystals with a small amount of absolute ethyl alcohol, and drying at a temperature below 50 ℃ to obtain a finished product; the purification liquid is as follows: 0.05-0.2% of vitamin C, 0.05-0.2% of acetic acid and 3-8 times of water in the total mass of the precipitate and the levodopa crude product.
2. The process for preparing levodopa by using velvet beans according to claim 1, wherein the levodopa comprises: the solid-liquid ratio of the catbeans to the extracting solution is 1 kg: 0.5 to 1L.
3. The process for preparing levodopa by using velvet beans according to claim 1, wherein the levodopa comprises: and (3) in the step (4), the adding amount of the activated carbon is 3-5% of the total mass of the extract I and the uncrystallized solution in the step (3) after mixing.
4. The process for preparing levodopa by using velvet beans according to claim 1, wherein the levodopa comprises: in the step (2), the power of the ultrasonic wave is 500W, and the irradiation temperature of the ultrasonic wave is 50-55 ℃.
5. The process for preparing levodopa by using velvet beans according to claim 1, wherein the levodopa comprises: in the dipping process in the step (2), the dipping temperature is 40-50 ℃.
6. The process for preparing levodopa by using velvet beans according to claim 1, wherein the levodopa comprises: the carp bait is prepared by mixing the following raw materials in parts by mass: 1-3 parts of residue and extracting solution obtained in the supercritical extraction kettle, 20-30 parts of soybean protein isolate, 5-8 parts of chitosan, 3-7 parts of silkworm chrysalis powder and 1-6 parts of shrimp powder.
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Denomination of invention: A process for preparing levodopa from cat beans Effective date of registration: 20230922 Granted publication date: 20210115 Pledgee: Guangxi Napo Rural Commercial Bank Co.,Ltd. Pledgor: NAPO KANGZHENG NATURAL PLANT EXTRACT Co.,Ltd. Registration number: Y2023980057174 |