CN114436926A - Method for separating and purifying erythroguline from acutangular anisodus plants - Google Patents
Method for separating and purifying erythroguline from acutangular anisodus plants Download PDFInfo
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- CN114436926A CN114436926A CN202210170866.1A CN202210170866A CN114436926A CN 114436926 A CN114436926 A CN 114436926A CN 202210170866 A CN202210170866 A CN 202210170866A CN 114436926 A CN114436926 A CN 114436926A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D207/00—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom
- C07D207/02—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D207/04—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having no double bonds between ring members or between ring members and non-ring members
- C07D207/08—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having no double bonds between ring members or between ring members and non-ring members with hydrocarbon radicals, substituted by hetero atoms, attached to ring carbon atoms
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D451/00—Heterocyclic compounds containing 8-azabicyclo [3.2.1] octane, 9-azabicyclo [3.3.1] nonane, or 3-oxa-9-azatricyclo [3.3.1.0<2,4>] nonane ring systems, e.g. tropane or granatane alkaloids, scopolamine; Cyclic acetals thereof
- C07D451/02—Heterocyclic compounds containing 8-azabicyclo [3.2.1] octane, 9-azabicyclo [3.3.1] nonane, or 3-oxa-9-azatricyclo [3.3.1.0<2,4>] nonane ring systems, e.g. tropane or granatane alkaloids, scopolamine; Cyclic acetals thereof containing not further condensed 8-azabicyclo [3.2.1] octane or 3-oxa-9-azatricyclo [3.3.1.0<2,4>] nonane ring systems, e.g. tropane; Cyclic acetals thereof
- C07D451/04—Heterocyclic compounds containing 8-azabicyclo [3.2.1] octane, 9-azabicyclo [3.3.1] nonane, or 3-oxa-9-azatricyclo [3.3.1.0<2,4>] nonane ring systems, e.g. tropane or granatane alkaloids, scopolamine; Cyclic acetals thereof containing not further condensed 8-azabicyclo [3.2.1] octane or 3-oxa-9-azatricyclo [3.3.1.0<2,4>] nonane ring systems, e.g. tropane; Cyclic acetals thereof with hetero atoms directly attached in position 3 of the 8-azabicyclo [3.2.1] octane or in position 7 of the 3-oxa-9-azatricyclo [3.3.1.0<2,4>] nonane ring system
- C07D451/06—Oxygen atoms
- C07D451/10—Oxygen atoms acylated by aliphatic or araliphatic carboxylic acids, e.g. atropine, scopolamine
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Abstract
The invention provides a method for separating and purifying erythroguline from acutangular anisodus herb, and relates to the field of chemical processes. A method for separating and purifying erythroguline from acutangular anisodus plants comprises the following steps: performing primary extraction and concentration on the acutangular anisodus herb extract to obtain total alkaloids, performing secondary extraction and concentration on the total alkaloids to obtain a crude product, crystallizing and filtering the crude product to obtain crude salt, and performing tertiary extraction on the crude salt to obtain a finished product. The preparation method comprises the steps of preparing the acutangular anisodus herb into extract, removing most impurities, then carrying out multi-stage extraction on the acutangular anisodus herb extract, and separating and extracting the erythronoline contained in the acutangular anisodus herb step by step to obtain a high-purity finished erythronoline product; the method has the advantages of good extraction effect, high separation efficiency, simple process and easy production and use.
Description
Technical Field
The invention relates to the technical field of chemical processes, and particularly relates to a method for separating and purifying erythronoline from scopolia acutangula plants.
Background
Erythronoline is a pyrrolidine alkaloid found in coca. Clinically, the medicinal composition has central tranquilizing effect and peripheral anticholinergic effect, has weaker activity than atropine, and has relatively stronger effect of inhibiting gastrointestinal peristalsis and gastric juice secretion. It also has effects in dilating peripheral blood vessel, increasing coronary blood flow, and relieving asthma. Can be used for treating gastric ulcer and spasmodic pain caused by various gastrointestinal diseases, and has good medicinal value.
Radix Anisodi Acutangulus C.Y.Wu et C.Chen is a plant of the genus anisodamia of the family Solanaceae. Perennial herbs with height of 1-1.5 m and no hair in the whole plant; the main root is thick, there are few hypertrophic lateral roots, the root bark is yellow brown, and the section is light yellow. As a traditional Chinese medicinal material, the traditional Chinese medicine has the effects of relieving spasm and pain, dispelling wind and removing dampness and the like, and can treat diseases such as stomachache, biliary colic, renal colic, rheumatic arthralgia, lumbocrural pain, traumatic injury and the like; the whole herb and root of the medicine contain alkaloid such as anisodine, and the medicine has high medicinal value, and how to extract the anisodine becomes the problem to be solved.
Disclosure of Invention
The invention aims to provide a method for separating and purifying erythronoline from acutangular anisodus herb, which can effectively separate and extract the erythronoline contained in acutangular anisodus herb and has high extraction efficiency.
The technical problem to be solved by the invention is realized by adopting the following technical scheme.
First, the embodiment of the invention provides a method for separating and purifying erythronoline from scopolia acutangula plants, which comprises the following steps: performing primary extraction and concentration on the acutangular anisodus herb extract to obtain total alkaloids, performing secondary extraction and concentration on the total alkaloids to obtain a crude product, crystallizing and filtering the crude product to obtain crude salt, and performing tertiary extraction on the crude salt to obtain a finished product.
Further, in some embodiments of the present invention, the acutangular anisodus herb extract is prepared by the following method: pulverizing and sieving radix Anisodi Acutanguli, leaching with methanol, filtering, and concentrating the filtrate to obtain radix Anisodi Acutanguli plant extract.
Further, in some embodiments of the present invention, the mesh number of the screen is 80 to 120 mesh; concentrating the filtrate to relative density of 1.1-1.2 to obtain radix Anisodi Acutanguli plant extract.
Further, in some embodiments of the present invention, in the first-stage extraction, chloroform is used to perform isovolumetric extraction on the acutangular anisodus herb extract, and then the chloroform is concentrated under reduced pressure and recovered to obtain total alkaloids.
Further, in some embodiments of the present invention, in the second-stage extraction, the pH is adjusted to 8 to 10, then carbon tetrachloride is used for extraction, and then the pH of the obtained extract is adjusted to 6 to 7, and then the extract is concentrated under reduced pressure to obtain a crude product.
Further, in some embodiments of the invention, ammonia is added to adjust the pH to 8-10; adding dilute sulfuric acid to adjust the pH to 6-7.
Further, in some embodiments of the invention, the crystallization is filtered by adding 10-20 times of acetone to the crude product, followed by stirring and adding hydrobromic acid, cooling for crystallization and filtering to obtain the crude salt.
Further, in some embodiments of the invention, hydrobromic acid is added to a pH of 3.
Further, in some embodiments of the present invention, in the third-stage extraction, water is added to the crude salt to dissolve the crude salt, the pH is adjusted to 8 to 10, chloroform is used for extraction, and the chloroform is dehydrated and recovered to obtain the finished product.
Further, in some embodiments of the invention, ammonia is added to adjust the pH to 8-10; dehydration was carried out with anhydrous sodium sulfate.
Compared with the prior art, the embodiment of the invention has at least the following advantages or beneficial effects:
in view of the above, the embodiment of the present invention provides a method for separating and purifying erythronoline from scopolia acutangula plants, which comprises the following steps: performing primary extraction and concentration on the acutangular anisodus root plant extract through chloroform to obtain total alkaloids, performing secondary extraction and concentration on the total alkaloids through carbon tetrachloride to obtain a crude product, crystallizing and filtering the crude product to obtain crude salt, dissolving the crude salt, and performing tertiary extraction through chloroform to obtain a finished product.
The method for separating and purifying the erythroguline from the acutangular anisodus root plants comprises the steps of firstly extracting most of effective components contained in the acutangular anisodus root plants by a leaching process to prepare extract, removing impurities, then carrying out primary extraction on the obtained acutangular anisodus root plant extract, extracting alkaloid components in the acutangular anisodus root plant extract by the primary extraction, removing other components, and concentrating to obtain acutangular anisodus root total alkaloids containing the erythroguline; then, performing secondary extraction on the obtained total alkaloids, and separating and extracting the erythroguline from the total alkaloids by the secondary extraction to obtain a crude erythroguline product; then crystallizing the crude product, adding acid to form the salt of the erythrogulinic acid, crystallizing and filtering to obtain crude salt; and carrying out three-stage extraction on the obtained crude salt, dissolving the obtained crude salt by adding a solvent during the three-stage extraction to form a solution of the salt of the erythroguline, then adding alkali liquor to free the erythroguline, and further extracting the erythroguline by extraction operation to finally obtain an erythroguline finished product.
The preparation method comprises the steps of preparing the acutangular anisodus herb into extract, removing most impurities, then carrying out multi-stage extraction on the acutangular anisodus herb extract, and separating and extracting the erythronoline contained in the acutangular anisodus herb step by step to obtain a high-purity finished erythronoline product; the method has the advantages of good extraction effect, high separation efficiency, simple process and easy production and use.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail below with reference to specific examples.
The embodiment of the invention provides a method for separating and purifying erythronoline from acutangular anisodus herb, which comprises the following steps: performing primary extraction and concentration on the acutangular anisodus herb extract by chloroform to obtain total alkaloids, performing secondary extraction and concentration on the total alkaloids by carbon tetrachloride to obtain a crude product, crystallizing and filtering the crude product to obtain crude salt, dissolving the crude salt, and performing tertiary extraction by chloroform to obtain a finished product.
In the embodiment, most of effective components contained in the acutangular anisodus acutangular plant are extracted and prepared into extract through an extraction process, impurities are removed, then primary extraction is carried out on the obtained acutangular anisodus acutangular plant extract, alkaloid components in the acutangular anisodus acutangular plant extract are extracted through the primary extraction, other components are removed, and the total alkaloids contain erythroguline; then, performing secondary extraction on the obtained total alkaloids, and separating and extracting the erythroguline from the total alkaloids by the secondary extraction to obtain a crude erythroguline product; then crystallizing the crude product, adding acid to form the salt of the erythrogulinic acid, crystallizing and filtering to obtain crude salt; and carrying out three-stage extraction on the obtained crude salt, dissolving the obtained crude salt by adding a solvent during the three-stage extraction to form a solution of the salt of the erythroguline, then adding alkali liquor to free the erythroguline, and further extracting the erythroguline by extraction operation to finally obtain an erythroguline finished product.
The preparation method comprises the steps of preparing the acutangular anisodus herb into extract, removing most impurities, then carrying out multi-stage extraction on the acutangular anisodus herb extract, and separating and extracting the erythronoline contained in the acutangular anisodus herb step by step to obtain a high-purity finished erythronoline product; the method has the advantages of good extraction effect, high separation efficiency, simple process and easy production and use.
Further, in some embodiments of the present invention, the acutangular anisodus herb extract is prepared by the following method: pulverizing and sieving radix Anisodi Acutanguli, leaching with methanol, filtering, and concentrating the filtrate to obtain radix Anisodi Acutanguli plant extract.
In the embodiment, the particle size of the three-thirds powder particles after being crushed can be effectively controlled by crushing and sieving the three-thirds plants, so that the effective ingredients contained in the three-thirds powder particles can be fully extracted through subsequent leaching operation, the waste loss is avoided, and the leaching efficiency is improved; three fens three after will smashing are leached and are filtered through methyl alcohol, detach impurity, then concentrate the filtrating and retrieve methyl alcohol, reduce the wasting of resources to promote the concentration of active ingredient through the concentration, get rid of unnecessary moisture, thereby make things convenient for going on of follow-up step, be favorable to improving follow-up extraction separation operation's efficiency, more be favorable to the use of producing.
Further, in some embodiments of the present invention, the mesh size of the screen is 80-120 mesh; concentrating the filtrate to relative density of 1.1-1.2 to obtain radix Anisodi Acutanguli plant extract.
In the embodiment, the particle size of the three thirds of powder after being crushed can be better controlled by limiting the mesh number of the sieve, so that the adverse effect on the leaching efficiency of subsequent leaching caused by too large or too small particles is avoided, and the effective components contained in the three thirds of powder can be fully extracted into the extract; through controlling the extract relative density after the concentration, can remove unnecessary moisture through the concentration more effectively, promote the active ingredient concentration, help improving follow-up extraction separation efficiency, more be favorable to the production and use.
Further, in some embodiments of the present invention, in the first-stage extraction, chloroform is used to perform isovolumetric extraction on the acutangular anisodus herb extract, and then the chloroform is concentrated under reduced pressure and recovered to obtain total alkaloids.
In the embodiment, alkaloids such as erythrosine contained in the acutangular anisodus root can be dissolved in chloroform, most of the alkaloids contained in the acutangular anisodus root can be effectively extracted by using the chloroform, and other impurities are removed, so that the subsequent separation and extraction of the erythrosine are facilitated; decompression concentration and recovery chloroform can effectively reduce the wasting of resources, and decompression concentration can effectively prevent that the alkaloid of drawing from suffering from the loss at the in-process of concentration simultaneously, helps further promoting extraction, separation efficiency.
Further, in some embodiments of the present invention, in the second-stage extraction, the pH is adjusted to 8 to 10, then carbon tetrachloride is used for extraction, and then the pH of the obtained extract is adjusted to 6 to 7, and then the extract is concentrated under reduced pressure to obtain a crude product.
In the embodiment, the extracted alkaloids can be dissociated out by adjusting the pH value to be alkaline, and then are extracted by carbon tetrachloride, so that the method is favorable for further separating and extracting the erythrosine contained in the raw material, further removing other components and improving the extraction efficiency; then, the pH value is adjusted and the pressure is reduced for concentration, so that a crude product is obtained, and the subsequent steps can be conveniently and smoothly carried out.
Further, in some embodiments of the invention, ammonia is added to adjust the pH to 8-10; adding dilute sulfuric acid to adjust the pH to 6-7.
In the above embodiment, adjust solution pH through using ammonia water and dilute sulfuric acid, can follow-up extraction efficiency that separates the extraction to the erythrodocaine through carbon tetrachloride of more effectual improvement, more be favorable to the use of producing.
Further, in some embodiments of the invention, the crystallization is filtered by adding 10-20 times of acetone to the crude product, followed by stirring and adding hydrobromic acid, cooling for crystallization and filtering to obtain the crude salt.
In the above embodiment, acetone is added to dissolve the obtained crude erythronoline, and then hydrobromic acid is added while stirring, so that the hydrobromic acid and the erythronoline are fully reacted to generate the erythronoline hydrobromide, and the obtained erythronoline is cooled, crystallized and filtered to obtain crude salt with the component of the crystalline erythronoline hydrobromide, so that the erythronoline which is insoluble in the raw material and difficult to extract and separate forms soluble salt crystals, thereby further improving the extraction and separation efficiency of the erythronoline in the raw material, being more beneficial to the subsequent steps, and being more beneficial to production and use.
Further, in some embodiments of the invention, hydrobromic acid is added to a pH of 3.
In the above embodiment, by controlling the addition of hydrobromic acid to a pH of 3, the amount of added hydrobromic acid can be effectively controlled, so that the added hydrobromic acid can fully react with the erythrosine to form erythrosine hydrobromide, thereby enabling the erythrosine in the raw material to be extracted and separated more fully, further improving the extraction and separation efficiency, and facilitating the smooth proceeding of the subsequent steps.
Further, in some embodiments of the present invention, in the third-stage extraction, water is added to the crude salt to dissolve the crude salt, the pH is adjusted to 8 to 10, chloroform is used for extraction, and the chloroform is dehydrated and recovered to obtain the finished product.
In the above embodiment, the crude salt is dissolved by adding water to form a salt solution of erythrosine hydrobromide, then adding alkali to adjust the pH to 8-10 to free the erythrosine in the salt solution, then using chloroform to extract and separate the free erythrosine, and finally dehydrating and recovering the chloroform to save resources and finally obtain the finished erythrosine. Can effectually extract the separation to red gulonic alkali like this, extract efficiently.
Further, in some embodiments of the invention, ammonia is added to adjust the pH to 8-10; dehydration was carried out with anhydrous sodium sulfate.
In the embodiment, the ammonia water is used, so that the erythrosine in the crude salt solution can be more effectively dissociated, and the subsequent extraction and separation of the dissociated erythrosine by the chloroform are facilitated; through using anhydrous sodium sulfate, can effectively get rid of unnecessary moisture, help improving the quality of the product red guqin that obtains, more be favorable to the use of producing.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The embodiment provides a method for separating and purifying erythroguline from acutangular anisodus plants, which comprises the following steps:
pulverizing radix Anisodi Acutanguli, sieving with 100 mesh sieve, leaching with methanol, filtering, and concentrating the filtrate to relative density of 1.1 to obtain radix Anisodi Acutanguli plant extract;
extracting the acutangular anisodus root and the acutangular anisodus root extract by chloroform in an isometric manner, and then concentrating under reduced pressure and recovering the chloroform to obtain total alkaloids;
adding ammonia water into the total alkaloids to adjust pH to 10, extracting with carbon tetrachloride, adding dilute sulfuric acid into the obtained extract to adjust pH to 6, and concentrating under reduced pressure to obtain crude product;
adding acetone 10 times of the crude product, then stirring and adding hydrobromic acid until the pH value is 3, cooling, crystallizing and filtering to obtain crude salt;
and adding water to the crude salt for dissolving, adding ammonia water to adjust the pH value to 10, extracting by using chloroform, dehydrating by using anhydrous sodium sulfate, and recovering the chloroform to obtain a finished product.
Example 2
The embodiment provides a method for separating and purifying erythroguline from acutangular anisodus plants, which comprises the following steps:
pulverizing radix Anisodi Acutanguli, sieving with 80 mesh sieve, leaching with methanol, filtering, and concentrating the filtrate to relative density of 1.2 to obtain radix Anisodi Acutanguli extract;
extracting the acutangular anisodus root and the acutangular anisodus root extract by chloroform in an isometric manner, and then concentrating under reduced pressure and recovering the chloroform to obtain total alkaloids;
adding ammonia water into the total alkaloids to adjust pH to 10, extracting with carbon tetrachloride, adding dilute sulfuric acid into the obtained extract to adjust pH to 6, and concentrating under reduced pressure to obtain crude product;
adding 20 times of acetone into the crude product, then stirring and adding hydrobromic acid until the pH value is 3, cooling, crystallizing and filtering to obtain a crude salt;
and adding water to the crude salt for dissolving, adding ammonia water to adjust the pH value to 10, extracting by using chloroform, dehydrating by using anhydrous sodium sulfate, and recovering the chloroform to obtain a finished product.
Example 3
The embodiment provides a method for separating and purifying erythroguline from acutangular anisodus plants, which comprises the following steps:
pulverizing radix Anisodi Acutanguli, sieving with 90 mesh sieve, leaching with methanol, filtering, and concentrating the filtrate to relative density of 1.18 to obtain radix Anisodi Acutanguli plant extract;
extracting the acutangular anisodus root and the acutangular anisodus root extract by chloroform in an isometric manner, and then concentrating under reduced pressure and recovering the chloroform to obtain total alkaloids;
adding ammonia water into the total alkaloids to adjust pH to 9, extracting with carbon tetrachloride, adding dilute sulfuric acid into the obtained extract to adjust pH to 6, and concentrating under reduced pressure to obtain crude product;
adding 18 times of acetone into the crude product, then stirring and adding hydrobromic acid until the pH value is 3, cooling, crystallizing and filtering to obtain a crude salt;
and adding water to the crude salt for dissolving, adding ammonia water to adjust the pH value to 8, extracting by using chloroform, dehydrating by using anhydrous sodium sulfate, and recovering the chloroform to obtain a finished product.
Example 4
The embodiment provides a method for separating and purifying erythroguline from acutangular anisodus plants, which comprises the following steps:
pulverizing radix Anisodi Acutanguli, sieving with 110 mesh sieve, leaching with methanol, filtering, and concentrating the filtrate to relative density of 1.15 to obtain radix Anisodi Acutanguli plant extract;
extracting the acutangular anisodus root and the acutangular anisodus root extract by chloroform in an isometric manner, and then concentrating under reduced pressure and recovering the chloroform to obtain total alkaloids;
adding ammonia water into the total alkaloids to adjust pH to 10, extracting with carbon tetrachloride, adding dilute sulfuric acid into the obtained extract to adjust pH to 6, and concentrating under reduced pressure to obtain crude product;
adding acetone 15 times of the crude product, then stirring and adding hydrobromic acid until the pH value is 3, cooling, crystallizing and filtering to obtain crude salt;
and adding water to the crude salt for dissolving, adding ammonia water to adjust the pH value to 8, extracting by using chloroform, dehydrating by using anhydrous sodium sulfate, and recovering the chloroform to obtain a finished product.
Example 5
The embodiment provides a method for separating and purifying erythronoline from acutangular anisodus root plants, which comprises the following steps:
pulverizing radix Anisodi Acutanguli, sieving with 80 mesh sieve, leaching with methanol, filtering, and concentrating the filtrate to relative density of 1.12 to obtain radix Anisodi Acutanguli plant extract;
performing isovolumetric extraction on the acutangular anisodus root plant extract by chloroform, and then performing reduced pressure concentration and chloroform recovery to obtain total alkaloids;
adding ammonia water into the total alkaloids to adjust pH to 10, extracting with carbon tetrachloride, adding dilute sulfuric acid into the obtained extract to adjust pH to 6, and concentrating under reduced pressure to obtain crude product;
adding 14 times of acetone into the crude product, then stirring and adding hydrobromic acid until the pH value is 3, cooling, crystallizing and filtering to obtain a crude salt;
and adding water to the crude salt for dissolving, adding ammonia water to adjust the pH value to 10, extracting by using chloroform, dehydrating by using anhydrous sodium sulfate, and recovering the chloroform to obtain a finished product.
Example 6
The embodiment provides a method for separating and purifying erythroguline from acutangular anisodus plants, which comprises the following steps:
pulverizing radix Anisodi Acutanguli, sieving with 100 mesh sieve, leaching with methanol, filtering, and concentrating the filtrate to relative density of 1.18 to obtain radix Anisodi Acutanguli extract;
performing isovolumetric extraction on the acutangular anisodus root plant extract by chloroform, and then performing reduced pressure concentration and chloroform recovery to obtain total alkaloids;
adding ammonia water into the total alkaloids to adjust pH to 10, extracting with carbon tetrachloride, adding dilute sulfuric acid into the obtained extract to adjust pH to 6, and concentrating under reduced pressure to obtain crude product;
adding 20 times of acetone into the crude product, then stirring and adding hydrobromic acid until the pH value is 3, cooling, crystallizing and filtering to obtain a crude salt;
and adding water to the crude salt for dissolving, adding ammonia water to adjust the pH value to 8, extracting by using chloroform, dehydrating by using anhydrous sodium sulfate, and recovering the chloroform to obtain a finished product.
Test examples
Taking the finished products of the erythronoline of examples 1-6 as samples, numbering 1-6, performing high performance liquid chromatography, preparing another erythronoline standard, performing high performance liquid chromatography under the same conditions to obtain a chromatographic chart of the samples 1-6 and the standard, and calculating the purity of the erythronoline in the samples 1-6 by peak area, wherein the results are shown in table 1:
TABLE 1
| Numbering | 1 | 2 | 3 | 4 | 5 | 6 |
| Purity/%) | 86 | 90 | 88 | 91 | 92 | 92 |
According to results, the method for separating and purifying the erythronoline from the acutangular anisodus plants provided by the invention can effectively separate and extract the erythronoline, and the obtained product has high purity; among them, the effects of examples 4 to 6 are preferable.
In summary, according to the method for separating and purifying erythronoline from acutangular anisodus root provided by the embodiments of the present invention, the extraction process is performed on acutangular anisodus root to extract most of the effective components contained therein and prepare the extract, impurities are removed, the obtained acutangular anisodus root extract is subjected to primary extraction, alkaloid components in the acutangular anisodus root extract are extracted by the primary extraction, other components are removed, and the concentration is performed to obtain acutangular anisodus root total alkaloids containing erythronoline; then, performing secondary extraction on the obtained total alkaloids, and separating and extracting the erythroguline from the total alkaloids by the secondary extraction to obtain a crude erythroguline product; then crystallizing the crude product, adding acid to form the salt of the erythrogulinic acid, crystallizing and filtering to obtain crude salt; and carrying out three-stage extraction on the obtained crude salt, dissolving the obtained crude salt by adding a solvent during the three-stage extraction to form a solution of the salt of the erythroguline, then adding alkali liquor to free the erythroguline, and further extracting the erythroguline by extraction operation to finally obtain an erythroguline finished product.
The preparation method comprises the steps of preparing the acutangular anisodus herb into extract, removing most impurities, then carrying out multi-stage extraction on the acutangular anisodus herb extract, and separating and extracting the erythronoline contained in the acutangular anisodus herb step by step to obtain a high-purity finished erythronoline product; the method has the advantages of good extraction effect, high separation efficiency, simple process and easy production and use.
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (10)
1. A method for separating and purifying erythroguline from scopolia acutangula plants is characterized by comprising the following steps: performing primary extraction and concentration on the acutangular anisodus herb extract by chloroform to obtain total alkaloids, performing secondary extraction and concentration on the total alkaloids by carbon tetrachloride to obtain a crude product, crystallizing and filtering the crude product to obtain crude salt, dissolving the crude salt, and performing tertiary extraction by chloroform to obtain a finished product.
2. The method for separating and purifying erythroguline from acutangular anisodus herb as claimed in claim 1, wherein the acutangular anisodus herb extract is prepared by the following steps: pulverizing and sieving radix Anisodi Acutanguli, leaching with methanol, filtering, and concentrating the filtrate to obtain radix Anisodi Acutanguli plant extract.
3. The method for separating and purifying anisodine from acutangular anisodine plants as claimed in claim 2, wherein the mesh number of said sieve is 80-120 meshes; concentrating the filtrate to relative density of 1.1-1.2 to obtain radix Anisodi Acutanguli plant extract.
4. The method for separating and purifying anisodine from acutangular anisodine as claimed in claim 1, wherein the anisodine is obtained by extracting the acutangular anisodine extract with chloroform at the same volume during the first-stage extraction, then concentrating under reduced pressure and recovering chloroform.
5. The method of claim 1, wherein the secondary extraction is performed by adjusting pH to 8-10, extracting with carbon tetrachloride, adjusting pH of the obtained extract to 6-7, and concentrating under reduced pressure to obtain crude anisodine.
6. The method for separating and purifying anisodine from the trisection plant as claimed in claim 5, wherein the pH is adjusted to 8-10 by adding ammonia water; adding dilute sulfuric acid to adjust the pH to 6-7.
7. The method for separating and purifying anisodine from acutangular anisodine as claimed in claim 1, wherein the crude salt is obtained by adding acetone 10-20 times of the crude product, stirring and adding hydrobromic acid, cooling and crystallizing, and filtering.
8. The method of claim 7, wherein hydrobromic acid is added to a pH of 3.
9. The method for separating and purifying anisodine from acutangular anisodine as claimed in claim 1, wherein the crude salt is dissolved in water, the pH is adjusted to 8-10, and then chloroform is used for extraction, dehydration and recovery of chloroform to obtain the final product.
10. The method for separating and purifying anisodine from acutangular anisodine as claimed in claim 9, wherein ammonia is added to adjust pH to 8-10; dehydration was carried out with anhydrous sodium sulfate.
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| CN202210170866.1A CN114436926A (en) | 2022-02-23 | 2022-02-23 | Method for separating and purifying erythroguline from acutangular anisodus plants |
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| CN202210170866.1A CN114436926A (en) | 2022-02-23 | 2022-02-23 | Method for separating and purifying erythroguline from acutangular anisodus plants |
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| CN202210170866.1A Withdrawn CN114436926A (en) | 2022-02-23 | 2022-02-23 | Method for separating and purifying erythroguline from acutangular anisodus plants |
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| CN (1) | CN114436926A (en) |
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Application publication date: 20220506 |