CN109081787B - Process for extracting levodopa from mucuna - Google Patents

Process for extracting levodopa from mucuna Download PDF

Info

Publication number
CN109081787B
CN109081787B CN201811137000.0A CN201811137000A CN109081787B CN 109081787 B CN109081787 B CN 109081787B CN 201811137000 A CN201811137000 A CN 201811137000A CN 109081787 B CN109081787 B CN 109081787B
Authority
CN
China
Prior art keywords
levodopa
leaching
soaking
temperature
solution
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201811137000.0A
Other languages
Chinese (zh)
Other versions
CN109081787A (en
Inventor
黎永红
陆华
黎敏护
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Napo Kangzheng Natural Plant Extract Co ltd
Original Assignee
Napo Kangzheng Natural Plant Extract Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Napo Kangzheng Natural Plant Extract Co ltd filed Critical Napo Kangzheng Natural Plant Extract Co ltd
Priority to CN201811137000.0A priority Critical patent/CN109081787B/en
Publication of CN109081787A publication Critical patent/CN109081787A/en
Application granted granted Critical
Publication of CN109081787B publication Critical patent/CN109081787B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C227/00Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
    • C07C227/28Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from natural products
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C227/00Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
    • C07C227/38Separation; Purification; Stabilisation; Use of additives
    • C07C227/40Separation; Purification

Abstract

The invention discloses a process for extracting levodopa from velvet beans, which comprises the following steps: (1) pre-treating; (2) firstly, leaching; (3) leaching; (4) leaching; (5) concentration: mixing the first leaching solution obtained in the step (2) and the second leaching solution obtained in the step (3), adjusting the pH value of the mixed solution, standing for 24 hours, performing centrifugal separation to obtain a precipitate and a supernatant, concentrating the supernatant to obtain a levodopa crude product I, mixing the precipitate and the third leaching solution obtained in the step (4), and drying to obtain a levodopa crude product II; (6) refining to obtain refined levodopa. Compared with the method adopting the alcohol-based extracting solution, the method adopting the water-based extracting solution for extraction has the advantages of low extraction cost, high extraction rate of levodopa obtained by extraction, high purity (higher than 90 percent) and high purity (higher than 98 percent), and is low in pollution and basically free of sewage treatment problem.

Description

Process for extracting levodopa from mucuna
Technical Field
The invention relates to the technical field of Chinese herbal medicine processing, in particular to a process for extracting levodopa from velvet beans.
Background
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 due to a large amount of water-soluble impurities, the purity and the extraction rate of the levodopa are greatly influenced.
The research shows that the following acid water is used for extracting the levodopa, for example, CN201410735107.0 discloses a method for extracting the levodopa from green soybeans under the assistance of microwaves, which comprises the following steps: (1) pretreatment of raw materials: crushing the impurity-removed cat beans to 20-60 meshes, and mixing the crushed cat beans according to a solid-liquid ratio of 1: 1.5 adding deionized water, then sequentially adding 0.1%, 0.01% and 0.005-0.01% by mass of acetic acid, ascorbic acid and pectinase, mixing uniformly, and soaking for 4 h; (2) microwave-assisted extraction: adding the mixture according to the solid-liquid ratio of 1: 20, and 0.2 percent by mass of sodium thiosulfate, uniformly mixing, adding the materials into a microwave extraction device with the frequency of 2450MHz and the power of 20kw, extracting for 45-50min at the extraction temperature of 55-60 ℃, discharging the materials after the microwave extraction is finished, and separating solid from liquid by a solid-liquid separator to obtain an extracting solution; (3) fine filtering and ultrafiltration; (4) nano-filtering; (5) concentrating; (6) crystallizing; (7) separating; (8) and (5) washing and drying. Which solves the problem of environmental pollution in the traditional acid leaching extraction method. Although the problem of acid pollution of an extraction process in an acid leaching method is solved, sodium thiosulfate is added in the extraction process, and sulfur dioxide is generated to cause environmental pollution due to poor post-treatment sewage and acid reaction.
Also, for example, patent CN201611023242.8 discloses a method for extracting levodopa from velvet bean, comprising the steps of flattening the velvet bean, placing the squashed velvet bean into a reaction kettle in which an aqueous solution of ammonium bicarbonate, ammonium sulfate, tannic acid and sodium metabisulfite is dissolved, pressurizing with carbon dioxide, heating and leaching to obtain an extracting solution and velvet bean dregs; 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, and when acid-base fertilizer water is discharged, the nitrogen-ammonia content is increased, so that the difficulty of sewage treatment is increased.
Disclosure of Invention
The invention overcomes the technical problems of low purity, low extraction rate and serious pollution of levodopa extracted by an extraction process for extracting levodopa by acid water 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 extracting levodopa from velvet beans comprises the following steps:
(1) pretreatment: cleaning velvet beans, removing impurities, crushing and sieving with a 80-mesh sieve for later use;
(2) leaching: putting mucuna into the extracting solution, performing ultrasonic treatment for 40-50 min by adopting ultrasonic waves, and then soaking for 8h and filtering to obtain primary soybean soaking residues and primary leaching solution;
(3) leaching: soaking the bean dregs obtained in the step (1) in an extracting solution again, performing ultrasonic treatment for 40-50 min by adopting ultrasonic waves, soaking for 8h, and filtering to obtain secondary-soaked bean dregs and secondary-soaked leaching solution;
(4) leaching: soaking the second-soaked bean dregs in the extracting solution, performing ultrasonic treatment for 40-50 min by adopting ultrasonic waves, soaking for 4h, and filtering to obtain third-soaked bean dregs and a third-soaked leaching solution;
(5) concentration: mixing the first leaching solution obtained in the step (2) and the second leaching solution obtained in the step (3), adjusting the pH value of the mixed solution to 4.5-5.0, standing for 24 hours, performing centrifugal separation to obtain a precipitate and a supernatant, concentrating the supernatant to obtain a levodopa crude product I, mixing the precipitate and the third leaching solution obtained in the step (4), and drying to obtain a levodopa crude product II;
(6) refining: dissolving the levodopa crude product I and the levodopa crude product II in an aqueous solution with the mass being 3-5 times and the pH value being 3.5, adding the levodopa crude product I and vitamin C accounting for 0.1-0.5% of the total mass of the levodopa crude product II, heating to boil, filtering, adding 5-10% of activated carbon into the filtrate, stirring, preserving heat at 80-90 ℃ for 30-40 min, filtering to remove the activated carbon, and performing spray drying to obtain a levodopa fine product;
the extracting solutions in the step (1), the step (2) and the step (3) are all composed of the following components: the extraction liquid contains water 3-8 times of the mass of the velvet bean, 0.05-0.2% of vitamin C, 0.05-0.2% of acetic acid, 0.01-0.05% of protease, 0.01-0.05% of cellulase, 0.01-0.05% of sodium citrate and 0.01-0.05% of sodium metasilicate pentahydrate by mass of the velvet bean.
Wherein in the step (6), the concentration mode is decompression concentration, the pressure is 4.4-5.5 mpa, and the temperature is 30-40 ℃.
Wherein the power of the ultrasonic wave in the step (2) is 500W, and the irradiation temperature of the ultrasonic wave is 30-35 ℃.
Wherein the power of the ultrasonic wave in the step (3) is 500W, and the irradiation temperature of the ultrasonic wave is 40-45 ℃.
Wherein the power of the ultrasonic wave in the step (4) is 500W, and the irradiation temperature of the ultrasonic wave is 50-55 ℃.
Wherein in the leaching processes in the step (1), the step (2) and the step (3), the leaching temperature is 40-50 min.
Wherein, in the step (6), the spray drying conditions are that the air inlet temperature is 160 ℃, the air exhaust temperature is 90 ℃ and the spray pressure is 0.8 mpa.
The protease is composed of subtilisin and papain with the mass ratio of 1: 3-7, and the enzyme activity of the protease is not lower than 885.7U/g.
Compared with the prior art, the invention has the following beneficial effects:
(1) compared with the method adopting the alcohol-based extracting solution, the method adopting the water-based extracting solution for extraction has the advantages of low extraction cost, high extraction rate of levodopa obtained by extraction, high purity (higher than 90 percent) and high purity (higher than 98 percent), and is low in pollution and basically free of sewage treatment problem. The extracting solution disclosed by the invention consists of vitamin C, acetic acid, protease, cellulase, sodium citrate and sodium metasilicate pentahydrate, the cellulase can degrade mucuna cellulose, destroy plant cell walls and promote dissolution of levodopa, the subtilisin and the papain can degrade proteins, levodopa protein precursors in mucuna can be degraded into levodopa, and the levodopa protein precursors can be dissolved in the water-based extracting solution of the acetic acid, the vitamin C, the sodium citrate and the sodium metasilicate pentahydrate at high concentration, so that the obtained purity is high, and the extraction rate is high.
(2) According to the method, the levodopa is extracted by ultrasonic assistance, primary extraction is carried out at 30-35 ℃, the velvet beans can be efficiently enzymolyzed by the subtilisin, the papain and the cellulase at the temperature, the levodopa is quickly dissolved out under the cavitation action of the ultrasonic, the enzyme can also quickly permeate into the velvet beans, and the enzymolysis speed is greatly increased. The secondary leaching is carried out at the temperature of 40-45 ℃, the stable dissolution of the levodopa is facilitated at the temperature, the tertiary leaching is carried out at the temperature of 50-55 ℃, the enzyme is inactivated at the temperature, and the levodopa precursor is effectively dissolved out to generate the levodopa.
Detailed Description
The present invention will be further described with reference to examples and tests.
Example 1
A process for extracting levodopa from velvet beans comprises the following steps:
(1) pretreatment: cleaning velvet beans, removing impurities, crushing and sieving with a 80-mesh sieve for later use;
(2) leaching: placing mucuna in the extracting solution, performing ultrasonic treatment for 50min by adopting ultrasonic waves, soaking for 8h, and filtering to obtain primary soybean soaking residues and primary leaching solution; the power of ultrasonic waves is 500W, and the irradiation temperature of the ultrasonic waves is 30 ℃; the leaching temperature is 50 min;
(3) leaching: soaking the bean dregs obtained in the step (1) in the extracting solution again, and soaking for 8 hours after ultrasonic treatment is carried out for 40 minutes to obtain secondary-soaking bean dregs and secondary-soaking leachate; the power of the ultrasonic wave is 500W, and the irradiation temperature of the ultrasonic wave is 45 ℃; the leaching temperature is 40 min;
(4) leaching: soaking the second-soaked bean dregs in the extracting solution, performing ultrasonic treatment for 50min by adopting ultrasonic waves, soaking for 4h, and filtering to obtain third-soaked bean dregs and a third-soaked leaching solution; the power of the ultrasonic wave is 500W, and the irradiation temperature of the ultrasonic wave is 50 ℃; the leaching temperature is 50 min;
(5) concentration: mixing the first leaching solution obtained in the step (2) and the second leaching solution obtained in the step (3), adjusting the pH value of the mixed solution to 4.5, standing for 24 hours, performing centrifugal separation to obtain a precipitate and a supernatant, concentrating the supernatant to obtain a crude levodopa product I, mixing the precipitate and the third leaching solution obtained in the step (4), and drying to obtain a crude levodopa product II;
(6) refining: dissolving the levodopa crude product I and the levodopa crude product II in an aqueous solution with the mass 5 times and the pH value of 3.5, adding 0.1% of vitamin C in the total mass of the levodopa crude product I and the levodopa crude product II, heating to boil, filtering, adding 10% of active carbon into the filtrate, stirring, preserving the temperature at 80 ℃ for 40min, filtering to remove the active carbon, and performing spray drying to obtain a levodopa fine product; the concentration mode is reduced pressure concentration, the pressure is 4.4mpa, and the temperature is 40 ℃; the spray drying conditions are that the air inlet temperature is 160 ℃, the air exhaust temperature is 90 ℃ and the spray pressure is 0.8 mpa.
Wherein the extracting solutions in the step (1), the step (2) and the step (3) are all composed of the following components: based on the mass of the velvet beans, the extracting solution contains 8 times of the mass of the velvet beans of water, 0.05% of vitamin C, 0.2% of acetic acid, 0.01% of protease, 0.05% of cellulase, 0.01% of sodium citrate and 0.05% of sodium metasilicate pentahydrate. The protease is composed of subtilisin and papain with the mass ratio of 1: 3. The enzyme activity of the protease is 980.2U/g.
Example 2
A process for extracting levodopa from velvet beans comprises the following steps:
(1) pretreatment: cleaning velvet beans, removing impurities, crushing and sieving with a 80-mesh sieve for later use;
(2) leaching: placing mucuna in the extracting solution, performing ultrasonic treatment for 40min by adopting ultrasonic waves, soaking for 8h, and filtering to obtain primary soybean soaking residues and primary leaching solution; the power of ultrasonic waves is 500W, and the irradiation temperature of the ultrasonic waves is 35 ℃; the leaching temperature is 40 min;
(3) leaching: soaking the bean dregs obtained in the step (1) in the extracting solution again, and soaking for 8 hours after ultrasonic treatment is carried out for 50 minutes to obtain secondary-soaking bean dregs and secondary-soaking leachate; the power of the ultrasonic wave is 500W, and the irradiation temperature of the ultrasonic wave is 40 ℃; the leaching temperature is 40 min;
(4) leaching: soaking the second-soaked bean dregs in the extracting solution, performing ultrasonic treatment for 50min by adopting ultrasonic waves, soaking for 4h, and filtering to obtain third-soaked bean dregs and a third-soaked leaching solution; the power of the ultrasonic wave is 500W, and the irradiation temperature of the ultrasonic wave is 50 ℃; the leaching temperature is 50 min;
(5) concentration: mixing the first leaching solution obtained in the step (2) and the second leaching solution obtained in the step (3), adjusting the pH value of the mixed solution to 4.5, standing for 24 hours, performing centrifugal separation to obtain a precipitate and a supernatant, concentrating the supernatant to obtain a crude levodopa product I, mixing the precipitate and the third leaching solution obtained in the step (4), and drying to obtain a crude levodopa product II;
(6) refining: dissolving the levodopa crude product I and the levodopa crude product II in an aqueous solution with the mass 5 times and the pH value of 3.5, adding 0.1% of vitamin C in the total mass of the levodopa crude product I and the levodopa crude product II, heating to boil, filtering, adding 10% of active carbon into the filtrate, stirring, preserving the temperature at 80 ℃ for 40min, filtering to remove the active carbon, and performing spray drying to obtain a levodopa fine product; the concentration mode is reduced pressure concentration, the pressure is 4.4mpa, and the temperature is 40 ℃; the spray drying conditions are that the air inlet temperature is 160 ℃, the air exhaust temperature is 90 ℃ and the spray pressure is 0.8 mpa.
Wherein the extracting solutions in the step (1), the step (2) and the step (3) are all composed of the following components: the extract contains water 3 times of the weight of the velvet bean, vitamin C0.2%, acetic acid 0.05%, protease 0.05%, cellulase 0.01%, sodium citrate 0.05%, and sodium metasilicate pentahydrate 0.01%. The protease consists of subtilisin and papain in a mass ratio of 1: 7. The enzyme activity of the protease is 890.0U/g.
Example 3
A process for extracting levodopa from velvet beans comprises the following steps:
(1) pretreatment: cleaning velvet beans, removing impurities, crushing and sieving with a 80-mesh sieve for later use;
(2) leaching: placing mucuna in the extracting solution, performing ultrasonic treatment for 42min by adopting ultrasonic waves, soaking for 8h, and filtering to obtain primary soybean soaking residues and primary leaching solution; the power of ultrasonic waves is 500W, and the irradiation temperature of the ultrasonic waves is 32 ℃; the leaching temperature is 45 min;
(3) leaching: soaking the bean dregs obtained in the step (1) in the extracting solution again, and soaking for 8 hours after ultrasonic treatment is carried out for 48 minutes to obtain secondary-soaking bean dregs and secondary-soaking leachate; the power of the ultrasonic wave is 500W, and the irradiation temperature of the ultrasonic wave is 42 ℃; the leaching temperature is 48 min;
(4) leaching: soaking the second-soaked bean dregs in the extracting solution, performing ultrasonic treatment for 45min by adopting ultrasonic waves, soaking for 4h, and filtering to obtain third-soaked bean dregs and a third-soaked leaching solution; the power of the ultrasonic wave is 500W, and the irradiation temperature of the ultrasonic wave is 52 ℃; the leaching temperature is 45 min;
(5) concentration: mixing the first leaching solution obtained in the step (2) and the second leaching solution obtained in the step (3), adjusting the pH value of the mixed solution to 4.8, standing for 24 hours, performing centrifugal separation to obtain a precipitate and a supernatant, concentrating the supernatant to obtain a crude levodopa product I, mixing the precipitate and the third leaching solution obtained in the step (4), and drying to obtain a crude levodopa product II;
(6) refining: dissolving the levodopa crude product I and the levodopa crude product II in an aqueous solution with the mass being 4 times and the pH value being 3.5, adding 0.3% of vitamin C in the total mass of the levodopa crude product I and the levodopa crude product II, heating to boiling, filtering, adding 8% of active carbon into the filtrate, stirring, preserving the temperature at 85 ℃ for 35min, filtering to remove the active carbon, and performing spray drying to obtain a levodopa fine product; the concentration mode is reduced pressure concentration, the pressure is 5.0mpa, and the temperature is 35 ℃; the spray drying conditions are that the air inlet temperature is 160 ℃, the air exhaust temperature is 90 ℃ and the spray pressure is 0.8 mpa.
Wherein the extracting solutions in the step (1), the step (2) and the step (3) are all composed of the following components: the extractive solution contains water 6 times of the weight of the velvet bean, vitamin C0.1%, acetic acid 0.1%, protease 0.03%, cellulase 0.03%, sodium citrate 0.03%, and sodium metasilicate pentahydrate 0.03%. The protease consists of subtilisin and papain in a mass ratio of 1: 5. The enzyme activity of the protease is 888.7U/g.
To illustrate the technical effect set of the present invention, the following control groups were set up:
control group 1
The extraction process of the control 1 is substantially the same as that of the levodopa of example 1, except that the extraction solution of the control 1 is: adding 10% ammonium bicarbonate, 10% ammonium sulfate, 10% tannic acid and 3% sodium pyrosulfite by weight and volume ratio according to the weight of mucuna and 10 times of water by mass based on the total volume of the added water.
Control group 1
The extraction process of the control 1 is substantially the same as that of the levodopa of example 1, except that the extraction solution of the control 1 is: adding 10% ammonium bicarbonate, 10% ammonium sulfate, 10% tannic acid and 3% sodium pyrosulfite by weight and volume ratio according to the weight of mucuna and 10 times of water by mass based on the total volume of the added water.
Control group 2
The extraction process of the control group 2 was substantially the same as that of the levodopa of example 1, except that the extraction solution of the control group 2 was: according to the mass of the mucuna, the weight ratio of solid to liquid is 1: 21.5 adding deionized water, and then sequentially adding 0.1%, 0.01%, 0.005-0.01% and 0.2% by mass of acetic acid, ascorbic acid, pectinase and sodium thiosulfate.
Control group 3
The extraction process of control 3 was substantially the same as that of example 1 except that the extract of control 3 did not contain vitamin C.
Control group 4
The extraction process of control 4 was substantially the same as that of example 1 except that the extract of control 4 contained no cellulase.
Control group 5
The extraction process of control 5 was substantially the same as that of example 1 except that the extract of control 5 did not contain sodium citrate.
Control group 6
The extraction process of control 6 was substantially the same as that of levodopa of example 1, except that the extract of control 6 did not contain sodium metasilicate pentahydrate.
Control group 7
The extraction process of control 7 was substantially the same as that of example 1 except that the extract of control 7 contained no protease.
Control group 8
The extraction process of the control group 8 was substantially the same as that of the levodopa of example 1, except that the protease in the extract of the control group 8 was subtilisin only.
Control group 9
The extraction process of the control group 9 was substantially the same as that of the levodopa of example 1, except that the power of the ultrasonic waves in step (2), step (3) and step (4) of the control group 9 was 500W, and the irradiation temperature of the ultrasonic waves was 35 ℃.
Control group 10
The extraction process of the control group 10 was substantially the same as that of the levodopa of example 1 except that the power of the ultrasonic wave in step (2) of the control group 10 was 500W, the ultrasonic wave irradiation temperature was 55 ℃, the power of the ultrasonic wave in step (3) was 500W, the ultrasonic wave irradiation temperature was 45 ℃, the power of the ultrasonic wave in step (4) was 500W, and the ultrasonic wave irradiation temperature was 30 ℃.
Experimental detection
The extraction rate is as follows: the extraction rates of levodopa for examples 1 to 3 and controls 1 to 10 were as follows in table 1.
TABLE 1
Figure GDA0002682851300000071
Figure GDA0002682851300000081
As is clear from Table 1, the extraction yield and purity of examples 1 to 3 were slightly higher than those of control 1 and control 2, and it was found that the extract solutions used in the present invention were more effective than those of control 1 to control 2. Examples 1 to 3 showed that the extraction yield and purity were higher than those of control 3 to 8, and that the extract liquid of the present invention comprises vitamin C0.1, acetic acid, protease, cellulase, sodium citrate, sodium metasilicate pentahydrate, and water, and by combining them, the extract liquid was able to dissolve levodopa and its precursor, and the extraction yield and purity were high. The extraction rate and purity of the examples 1 to 3 are higher than those of the control group 9 and the control group 10, especially the extraction rate of the invention is high, which shows that the dissolution rate of levodopa is influenced after the ultrasonic extraction temperature is changed, and the extraction rate of levodopa is not as high as that of the invention by adopting isothermal extraction or high-temperature to low-temperature gradient extraction.
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 (4)

1. A process for extracting levodopa from velvet beans is characterized by comprising the following steps:
(1) pretreatment: cleaning velvet beans, removing impurities, crushing and sieving with a 80-mesh sieve for later use;
(2) leaching: putting mucuna into the extracting solution, performing ultrasonic treatment for 40-50 min by adopting ultrasonic waves, and then soaking for 8h and filtering to obtain primary soybean soaking residues and primary leaching solution; the power of the ultrasonic wave is 500W, and the irradiation temperature of the ultrasonic wave is 30-35 ℃;
(3) leaching: soaking the bean dregs obtained in the step (1) in an extracting solution again, performing ultrasonic treatment for 40-50 min by adopting ultrasonic waves, soaking for 8h, and filtering to obtain secondary-soaked bean dregs and secondary-soaked leaching solution; the power of the ultrasonic wave is 500W, and the irradiation temperature of the ultrasonic wave is 40-45 ℃;
(4) leaching: soaking the second-soaked bean dregs in the extracting solution, performing ultrasonic treatment for 40-50 min by adopting ultrasonic waves, soaking for 4h, and filtering to obtain third-soaked bean dregs and a third-soaked leaching solution; the power of the ultrasonic wave is 500W, and the irradiation temperature of the ultrasonic wave is 50-55 ℃;
(5) concentration: mixing the first leaching solution obtained in the step (2) and the second leaching solution obtained in the step (3), adjusting the pH value of the mixed solution to 4.5-5.0, standing for 24 hours, performing centrifugal separation to obtain a precipitate and a supernatant, concentrating the supernatant to obtain a levodopa crude product I, mixing the precipitate and the third leaching solution obtained in the step (4), and drying to obtain a levodopa crude product II;
(6) refining: dissolving the levodopa crude product I and the levodopa crude product II in an aqueous solution with the mass being 3-5 times and the pH value being 3.5, adding the levodopa crude product I and vitamin C accounting for 0.1-0.5% of the total mass of the levodopa crude product II, heating to boil, filtering, adding 5-10% of activated carbon into the filtrate, stirring, preserving heat at 80-90 ℃ for 30-40 min, filtering to remove the activated carbon, and performing spray drying to obtain a levodopa fine product;
the extracting solutions in the step (1), the step (2) and the step (3) are all composed of the following components: the mass of the velvet bean is taken as a reference, and the extracting solution contains 3-8 times of the mass of the velvet bean, 0.05-0.2% of vitamin C, 0.05-0.2% of acetic acid, 0.01-0.05% of protease, 0.01-0.05% of cellulase, 0.01-0.05% of sodium citrate and 0.01-0.05% of sodium metasilicate pentahydrate; the protease is composed of subtilisin and papain with the mass ratio of 1: 3-7.
2. The process of claim 1, wherein the levodopa is extracted from velvet bean, the process comprising: in the step (5), the concentration mode is reduced pressure concentration, the pressure is 4.4-5.5 MPa, and the temperature is 30-40 ℃.
3. The process of claim 1, wherein the levodopa is extracted from velvet bean, the process comprising: in the leaching processes in the step (1), the step (2) and the step (3), the leaching temperature is 40-50 min.
4. The process of claim 1, wherein the levodopa is extracted from velvet bean, the process comprising: in the step (6), the spray drying conditions are that the air inlet temperature is 160 ℃, the air exhaust temperature is 90 ℃ and the spray pressure is 0.8 mpa.
CN201811137000.0A 2018-09-28 2018-09-28 Process for extracting levodopa from mucuna Active CN109081787B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811137000.0A CN109081787B (en) 2018-09-28 2018-09-28 Process for extracting levodopa from mucuna

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811137000.0A CN109081787B (en) 2018-09-28 2018-09-28 Process for extracting levodopa from mucuna

Publications (2)

Publication Number Publication Date
CN109081787A CN109081787A (en) 2018-12-25
CN109081787B true CN109081787B (en) 2021-01-15

Family

ID=64842631

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201811137000.0A Active CN109081787B (en) 2018-09-28 2018-09-28 Process for extracting levodopa from mucuna

Country Status (1)

Country Link
CN (1) CN109081787B (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112110826B (en) * 2019-06-19 2023-05-16 吴基 Method for extracting levodopa from cat beans
CN113975850B (en) * 2021-10-26 2022-11-25 广西甙元植物制品有限公司 Automatic production equipment and process for producing levodopa based on chenopodium quinoa

Citations (23)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3253023A (en) * 1963-09-27 1966-05-24 Dow Chemical Co Recovery of 3-(3, 4-dihydroxyphenyl)-l-alanine from velvet beans
US3941835A (en) * 1970-03-19 1976-03-02 Bio-Derivatives Corporation Recovery of L-Dopa from R-dopa containing materials
CN1042703A (en) * 1988-11-14 1990-06-06 广西东兰县制药厂 Water diacolation-ion exchange method is extracted the levodopa novel process
CN1045969A (en) * 1989-03-28 1990-10-10 张宪德 Method with cat beans or multitude's beans production levodopa
CA2504201A1 (en) * 2002-10-30 2004-05-13 Phytrix Ag Mucuna pruriens and extracts thereof for the treatment of neurological diseases
WO2005092359A1 (en) * 2004-03-04 2005-10-06 Scott & White Memorial Hospital Extract of mucuna species and the use thereof as anti-parkinsons’s disease pharmaceutical
BRPI0901077A2 (en) * 2009-03-13 2010-11-16 Univ Fed Do Parana production of standardized dry extract of mucuna pruriens for use in treatment of parkinson's disease
CN102267919A (en) * 2011-05-31 2011-12-07 南宁市一锋生物科技有限公司 Preparation method of L-dopa from Mucuna pruriens
CN202124582U (en) * 2011-07-01 2012-01-25 安徽普朗膜技术有限公司 Membrane treatment system capable of extracting levodopa from velvet beans
CN102600229A (en) * 2012-03-22 2012-07-25 福建省农业科学院作物研究所 Method for improving content of levodopa of broad bean flower
CN102885815A (en) * 2011-07-20 2013-01-23 上海中医药大学附属曙光医院 Application of stizolobium cochinchinensis seed extract to preparation of medicament for treating Parkinson's disease accompanied by sleep disorder
CN103467328A (en) * 2013-09-30 2013-12-25 桂林茗兴生物科技有限公司 Method for extracting L-DOPA from velvet beans
CN103641730A (en) * 2013-12-19 2014-03-19 隆玉杰 Method for preparing levodopa
CN103664669A (en) * 2012-09-05 2014-03-26 李叶华 Process method for preparing high-purity levodopa
CN104311440A (en) * 2014-11-05 2015-01-28 桂林三宝生物科技有限公司 Method for extracting levodopa from velvet beans
CN104402748A (en) * 2014-12-05 2015-03-11 南宁知本康业生物技术有限公司 Microwave-assisted method for extracting levodopa from cat beans
CN104480171A (en) * 2014-11-21 2015-04-01 南宁知本康业生物技术有限公司 Method for extracting polypeptide from velvet bean residue
CN104610080A (en) * 2015-01-29 2015-05-13 黄振忠 Method for preparing levodopa by using Mucuna pruriens
CN105055494A (en) * 2015-08-31 2015-11-18 桂林茗兴生物科技有限公司 Method for preparing catbean extract
CN106631853A (en) * 2016-11-21 2017-05-10 广西邦尔药业有限公司 Method for extracting levodopa from cat beans
CN106946721A (en) * 2017-03-30 2017-07-14 湖南华诚生物资源股份有限公司 A kind of method for extracting high-purity tyrosine and levodopa in the beans from cat simultaneously
CN108033893A (en) * 2017-12-25 2018-05-15 北京颐方生物科技有限公司 The method that continuous flow upstream ultrasonic technique extracts levodopa from cat beans
CN108546237A (en) * 2018-06-15 2018-09-18 那坡康正天然植物提取有限责任公司 A method of extracting levodopa by raw material of cat beans

Patent Citations (24)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3253023A (en) * 1963-09-27 1966-05-24 Dow Chemical Co Recovery of 3-(3, 4-dihydroxyphenyl)-l-alanine from velvet beans
US3941835A (en) * 1970-03-19 1976-03-02 Bio-Derivatives Corporation Recovery of L-Dopa from R-dopa containing materials
CN1042703A (en) * 1988-11-14 1990-06-06 广西东兰县制药厂 Water diacolation-ion exchange method is extracted the levodopa novel process
CN1028225C (en) * 1988-11-14 1995-04-19 广西东兰县制药厂 New process for extracting levodopa by use of water percolation-ion exchange method
CN1045969A (en) * 1989-03-28 1990-10-10 张宪德 Method with cat beans or multitude's beans production levodopa
CA2504201A1 (en) * 2002-10-30 2004-05-13 Phytrix Ag Mucuna pruriens and extracts thereof for the treatment of neurological diseases
WO2005092359A1 (en) * 2004-03-04 2005-10-06 Scott & White Memorial Hospital Extract of mucuna species and the use thereof as anti-parkinsons’s disease pharmaceutical
BRPI0901077A2 (en) * 2009-03-13 2010-11-16 Univ Fed Do Parana production of standardized dry extract of mucuna pruriens for use in treatment of parkinson's disease
CN102267919A (en) * 2011-05-31 2011-12-07 南宁市一锋生物科技有限公司 Preparation method of L-dopa from Mucuna pruriens
CN202124582U (en) * 2011-07-01 2012-01-25 安徽普朗膜技术有限公司 Membrane treatment system capable of extracting levodopa from velvet beans
CN102885815A (en) * 2011-07-20 2013-01-23 上海中医药大学附属曙光医院 Application of stizolobium cochinchinensis seed extract to preparation of medicament for treating Parkinson's disease accompanied by sleep disorder
CN102600229A (en) * 2012-03-22 2012-07-25 福建省农业科学院作物研究所 Method for improving content of levodopa of broad bean flower
CN103664669A (en) * 2012-09-05 2014-03-26 李叶华 Process method for preparing high-purity levodopa
CN103467328A (en) * 2013-09-30 2013-12-25 桂林茗兴生物科技有限公司 Method for extracting L-DOPA from velvet beans
CN103641730A (en) * 2013-12-19 2014-03-19 隆玉杰 Method for preparing levodopa
CN104311440A (en) * 2014-11-05 2015-01-28 桂林三宝生物科技有限公司 Method for extracting levodopa from velvet beans
CN104480171A (en) * 2014-11-21 2015-04-01 南宁知本康业生物技术有限公司 Method for extracting polypeptide from velvet bean residue
CN104402748A (en) * 2014-12-05 2015-03-11 南宁知本康业生物技术有限公司 Microwave-assisted method for extracting levodopa from cat beans
CN104610080A (en) * 2015-01-29 2015-05-13 黄振忠 Method for preparing levodopa by using Mucuna pruriens
CN105055494A (en) * 2015-08-31 2015-11-18 桂林茗兴生物科技有限公司 Method for preparing catbean extract
CN106631853A (en) * 2016-11-21 2017-05-10 广西邦尔药业有限公司 Method for extracting levodopa from cat beans
CN106946721A (en) * 2017-03-30 2017-07-14 湖南华诚生物资源股份有限公司 A kind of method for extracting high-purity tyrosine and levodopa in the beans from cat simultaneously
CN108033893A (en) * 2017-12-25 2018-05-15 北京颐方生物科技有限公司 The method that continuous flow upstream ultrasonic technique extracts levodopa from cat beans
CN108546237A (en) * 2018-06-15 2018-09-18 那坡康正天然植物提取有限责任公司 A method of extracting levodopa by raw material of cat beans

Also Published As

Publication number Publication date
CN109081787A (en) 2018-12-25

Similar Documents

Publication Publication Date Title
CN108383886B (en) Method for extracting hesperidin from immature bitter orange by continuous countercurrent method and hesperidin obtained by extraction
CN110684128B (en) Method for extracting and refining polygonatum sibiricum polysaccharide
CN102146144B (en) Method for extracting and refining inulin
CN102924544B (en) Method for preparing stevioside and chlorogenic acid from stevia step by step
CN103755822A (en) Brasenia schreberi polysaccharide preparation method
CN109081787B (en) Process for extracting levodopa from mucuna
CN106349405A (en) Method for extracting pectin from shaddock peel through enzymolysis and ultrasonic waves
CN107337934A (en) A kind of extracting method of vaccinium bracteatum thunb leaf pigment
CN104987434B (en) A kind of method that water at low temperature extracts inulin in use
CN103087144A (en) Diosgenin production method
CN115322241B (en) Method for extracting tea saponin from oil tea meal
CN103602649A (en) Purification method for papain
CN104983778B (en) Method for continuously and comprehensively extracting liquorice components under high pressure
CN102174052B (en) Method for extracting and refining ginkgolide
CN114391657B (en) Method for extracting active ingredients from agaricus bisporus stems
CN110615857A (en) Method for recycling waste in orange can processing production
CN106883312A (en) A kind of extracting method of silkworm excrement pectin
CN108552370A (en) A method of extraction tea polyphenols
CN109467580B (en) Extraction process of naringin
CN109096131B (en) Process for preparing levodopa by utilizing velvet beans
CN112812144A (en) Method for extracting gastrodin extract
CN106188210A (en) A kind of technique extracting high-purity tea saponin from Semen Camelliae grouts
CN106866836A (en) A kind of method that pectin is extracted from pear skin
CN110938103A (en) Method for extracting food-grade tannin from persimmons
CN105754373B (en) A kind of method of application fruits and vegetables vegetables pigment, vegetable beverage and Vegetable powder

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
PE01 Entry into force of the registration of the contract for pledge of patent right
PE01 Entry into force of the registration of the contract for pledge of patent right

Denomination of invention: A process for extracting levodopa from Li Dou

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