CN110613751A - Method for separating and purifying ephedrine - Google Patents
Method for separating and purifying ephedrine Download PDFInfo
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- CN110613751A CN110613751A CN201911116819.3A CN201911116819A CN110613751A CN 110613751 A CN110613751 A CN 110613751A CN 201911116819 A CN201911116819 A CN 201911116819A CN 110613751 A CN110613751 A CN 110613751A
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- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/19—Preparation or pretreatment of starting material involving fermentation using yeast, bacteria or both; enzymatic treatment
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- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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- A61K2236/50—Methods involving additional extraction steps
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- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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- A—HUMAN NECESSITIES
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- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
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Abstract
The invention discloses a method for separating and purifying ephedrine, and belongs to the technical field of extraction of plant active ingredients. The invention aims at the problems of low extraction rate, low purity, easy deactivation and the like of cannabixanthin in the existing extraction method, and high-purity ephedrine is obtained by crushing hemp leaves, and then sequentially carrying out enzymolysis with cellulase, low-temperature extraction, filtration, concentration and recovery, extraction, rough filtration, membrane filtration, chromatography, concentration, crystallization, drying and other technological processes for separation and purification. The method has simple process, and the prepared cannabixanthin does not contain tetrahydrocannabinol, thereby being suitable for industrial large-scale production.
Description
Technical Field
The invention relates to the technical field of extraction of plant active ingredients, in particular to a method for separating and purifying ephedrine.
Background
Industrial hemp (Stevia rebaudiana Bertoni) is an annual plant of the genus cannabis of the family cannabinaceae, widely distributed around the world. The Cannabis plants in the world are mainly 3 species of wild Cannabis sativa (Cannabis ruderalisisch), Indian Cannabis sativa (Cannabis indica Lam) and cultivated Cannabis sativa (Cannabis sativaL), and many Cannabis varieties and subspecies are generated in the long-term biological evolution process. Cannabis sativa contains Tetrahydrocannabinol (THC), a hallucinogenic secondary metabolite, and is one of the well-known drug-source plants. For convenience of supervision and reasonable use, the varieties of cannabis with THC content of less than 0.3% in cannabis are internationally defined as industrial cannabis which does not have drug utilization value. At present, 27 countries in the world grow industrial cannabis, and 26 industrial cannabis varieties with THC content of less than 0.3% are cultivated.
The industrial hemp is also called as hemp, and the whole body of hemp is treasure and mainly has three functions of weaving, eating and medicine. The hemp skin is rich in fiber and can be used for processing clothes and various ornaments, the hemp stem core is an excellent wood substitute and can also be used for producing superfine powder, and the hemp seeds are rich in high-quality protein and fatty acid necessary for human bodies and can be applied to the fields of food, health care products and the like. More than 20 known flavonoids isolated from leaves, flowers and pollen of cannabis sativa are glycosylated, prenylated or methylated. In 2002, McPartland et al isolated a conjugated O-glycoside compound: apigenin (apigenin), luteolin (luteolin), quercetin (quercetin) and kaempferol (kaempferol); in the same year, Vanhoenantker et al isolated C-glycoside compounds: orientin (orientin), paclitaxel (vitexin), luteolin-7-O-glucoside (luteolin-7-O-glucoside) and apigenin-7-O-glucoside (apigenin-7-O-glucoside). In addition, the specific compounds of cannabis include cannabixanthin a, cannabixanthin B and cannabixanthin C. The ephedrine is a compound in the cannabis, belongs to propenyl flavonoid chemically, and has no relation with cannabinoids such as THC or CBD. Cannabixanthin a and B belong to the flavonoids and were found in 1985, and cannabixanthin C was found in 2008. It was confirmed to have anti-inflammatory effect at that time, and the efficacy of the compound is nearly 30 times stronger than that of acetylsalicylic acid (aspirin) under the same quality. The obtained product has rheumatoid inhibiting effect; the ephedrine A and the ephedrine B have the inhibition effect on prostaglandin E in vitro, so that a plurality of researches discuss the potential of the ephedrine A and the ephedrine B in the aspect of anti-inflammation. At present, the process for extracting the total flavone from the hemp leaves and the hemp pectins is reported, but the realization of industrial extraction is rare. The method adopts methanol water solution extraction and column chromatography separation and purification, optimizes the extraction process of the hemp leaf total flavonoids to search for the optimal extraction conditions of the hemp leaf total flavonoids, aims to develop a process suitable for industrial large-scale production, and aims to provide guidance for fully utilizing the bioactive components in the hemp leaves and realizing the comprehensive utilization of hemp resources and the maximization of benefits.
Disclosure of Invention
Aiming at the problems of low extraction rate, low purity, easy inactivation and the like of cannabixanthin in the existing extraction method, the invention provides a method for separating and purifying the ephedrine, which comprises the following steps:
1. pulverizing hemp flower and leaf into granules, adding cellulase for enzymolysis to obtain cellulase enzymolysis hemp flower and leaf.
2. Adding an ethanol aqueous solution into the enzymolysis cannabis sativa leaves obtained in the step 1, and extracting at a low temperature to obtain an extracting solution; the ethanol water solution is 20-50%, the low temperature extraction temperature is 45-58 deg.C, and the time is 30-60 min.
3. Filtering the extracting solution obtained in the step 2, filtering, and concentrating at low temperature under reduced pressure to 1/5 volumes to obtain a concentrated solution; the low-temperature reduced-pressure concentration temperature is 45-60 ℃, and the vacuum degree is 0.05-0.078 MPa.
4. Adding NaOH aqueous solution into the concentrated solution obtained in the step 3, and adjusting the pH value to 5-6; adjusting to alkalinity, adding n-hexane for extraction, combining the extract solutions, concentrating and pumping to dryness; the NaOH aqueous solution is 2-4%, the amount of n-hexane added each time is 1.6-2.4 times of the concentrated solution, and the extraction times are 2-3.
5. And (4) filtering the aqueous phase liquid obtained in the step (4) under pressure to obtain a crude filtrate.
6. And (4) filtering the rough filtrate obtained in the step (5) by using a membrane, and concentrating the obtained filtrate at low temperature under reduced pressure to 1/5 volumes to obtain the hemp flavone concentrated solution.
7. And (6) separating the hemp flavone concentrated solution obtained in the step 6 by column chromatography to obtain the ephedrine.
8. Carrying out low-temperature reduced pressure concentration and pumping drying on the cannabinoids separated in the step 7 to obtain cannabinoids crystals; the low-temperature reduced-pressure concentration temperature is 45-60 ℃, and the vacuum degree is 0.05-0.078 MPa.
9. Dissolving the cannabis sativa extract crystals obtained in the step 8 with an analytically pure ethanol aqueous solution, recovering the solvent at low temperature under reduced pressure, and crystallizing to obtain a cannabis sativa extract crystal liquid.
10. And (4) filtering the crystal liquid obtained in the step (9) to obtain high-purity ephedrine crystals, and drying the obtained crystals at low temperature in vacuum to obtain the pure product of the cannabinoid.
Further limiting, the particles prepared by crushing the hemp flowers and leaves in the step 1) are 30-50 meshes.
Further limiting, the cellulase is added in the step 1) for enzymolysis, the enzymolysis activity unit of the cellulase is 1000U/g, and the addition amount is as follows: 0.1-0.2 g/kg pulp; enzymolysis pH: 4.5-6.5, the enzymolysis temperature is 45-55 ℃, and the time is 40-50 min.
Further limiting, the feed-liquid ratio of the hemp flowers and leaves to the ethanol in the step 2) is 1g (4-6) mL.
Further limited, the pressure filtration pressure in the step 5) is 0.2MPa, and the filter screen is 1000 meshes.
Further defined, the filtration in the step 6) is that the rough filtrate is filtered through a hollow fiber membrane with the molecular weight of 1000D.
Further defined, the chromatography in step 7) refers to purification by elution through a macroporous resin column.
More particularly, the macroporous resin of step 7) is AB-8, HDX-5, X-5, or DX 101.
Further limiting, the drying in the step 10) is vacuum freeze-drying, the vacuum degree is 0.07-0.08 MPa, the vacuum freeze-drying temperature is-65-50 ℃, and the freeze-drying time is 24-28 h.
The method for extracting the ephedrine by adopting enzymolysis in combination with low-temperature alcohol extraction solves the problems of low extraction rate, inactivation, low color value and purity and the like of the ephedrine, and has the following beneficial effects:
the invention adopts a method of cellulose enzymolysis before extraction, the cellulose in the flower leaves is melted by the cellulose, the hemp yellow is released, and then the hemp yellow is fully released by extraction.
2, the traditional method for extracting the ephedrine adopts a solvent extraction method, and the extracted extracting solution often contains more cannabinoids.
Compared with the conventional method, the purity of the method is improved from 25% to 60%, and the purity is increased by 35%.
Drawings
FIG. 1 comparison of the extraction of ephedrine in the present invention with conventional methods.
FIG. 2 compares the purity of the ephedrine of the present invention with that of the conventional method.
FIG. 3 comparison of cannabinoids in extracts of the present invention and conventional processes.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
The specific implementation mode adopts the following technical scheme:
example 1
Method for separating and purifying ephedrine
1. 1000g of hemp flower and leaf are taken and crushed by a high-speed crusher with the granularity of 40 meshes to obtain hemp flower and leaf particles.
2. Then the ratio of 1g: adding ethanol water solution with volume fraction of 30% into 4mL of the feed liquid, and stirring and extracting to obtain an extracting solution. The extraction temperature is 48 deg.C, the extraction time is 40min, and the extraction time is 2 times.
3. Filtering the extracting solution after extraction is finished, removing filter residues, putting the filtrate into a concentrator, recovering the solvent, and concentrating the extracting solution to 20% of the original volume after the solvent is recovered; the vacuum concentration temperature is 52 ℃, and the vacuum degree is 0.072 MPa.
4. Standing and cooling the concentrated solution obtained in the step 3, adding a 2% NaOH aqueous solution, and adjusting the pH value to 5-6; adding n-hexane for extraction, mixing the extractive solutions, concentrating, and draining; the amount of n-hexane added each time is 2 times of the concentrated solution, and the extraction times are 2 times.
5. Pouring the extracted water phase into a 1000-mesh filter tank, pressurizing to 0.2MPa, and filtering to obtain a crude filtrate.
6. Filtering the obtained coarse filtrate with hollow fiber membrane with molecular weight of 1000D, and concentrating the obtained filtrate at low temperature under reduced pressure to 1/5 volume to obtain hemp flavone concentrated solution.
7. Separating the obtained hemp flavone concentrated solution by column chromatography to obtain ephedrine; the used filler is macroporous resin AB-8.
8. Concentrating the separated cannabis sativa extract solution at low temperature under reduced pressure, and draining to obtain cannabis sativa extract crystal; the low-temperature reduced pressure concentration temperature is 52 ℃, and the vacuum degree is 0.072 MPa.
9. Adding ethanol water solution according to the material ratio of 1:3 for dissolving, recovering solvent at low temperature under reduced pressure after complete dissolution, concentrating until cannabis yellow crystals are separated out, standing and cooling to obtain cannabis yellow crystal liquid.
10. Filtering the crystallization liquid by using a glass sand funnel to obtain high-purity ephedrine crystals, and putting the obtained crystals into a drying oven, wherein the vacuum degree is 0.08 MPa, the vacuum freeze-drying temperature is-65 ℃, and the freeze-drying time is 28 hours, so that the finished product of the ephedrine is obtained.
Example 2
Method for separating and purifying ephedrine
1. Taking 1000g of hemp flowers and leaves, crushing the hemp flowers and leaves by a high-speed crusher to 40 meshes, adding cellulase with the activity unit of 1000U/g, adding the cellulase with the addition amount of 0.1 g/kg of hemp flowers and leaves, stirring the mixture for 40min for enzymolysis at the pH value of 4.5 and the temperature of 45 ℃ and the rotation number of a stirring paddle of 20 r/min, and obtaining the cellulase enzymatic hydrolysis flowers and leaves.
2. Then the ratio of 1g: adding ethanol water solution with volume fraction of 30% into 4mL of the feed liquid, and stirring and extracting to obtain an extracting solution. The extraction temperature is 48 deg.C, the extraction time is 40min, and the extraction time is 2 times.
3. Filtering the extracting solution after extraction is finished, removing filter residues, putting the filtrate into a concentrator, recovering the solvent, and concentrating the extracting solution to 20% of the original volume after the solvent is recovered; the vacuum concentration temperature is 52 ℃, and the vacuum degree is 0.072 MPa.
4. Standing and cooling the concentrated solution obtained in the step 3, adding a 2% NaOH aqueous solution, and adjusting the pH value to 5-6; adding n-hexane for extraction, mixing the extractive solutions, concentrating, and draining; the amount of n-hexane added each time is 2 times of the concentrated solution, and the extraction times are 2 times.
5. Pouring the extracted water phase into a 1000-mesh filter tank, pressurizing to 0.2MPa, and filtering to obtain a crude filtrate.
6. Filtering the obtained coarse filtrate with hollow fiber membrane with molecular weight of 1000D, and concentrating the obtained filtrate at low temperature under reduced pressure to 1/5 volume to obtain hemp flavone concentrated solution.
7. Separating the obtained hemp flavone concentrated solution by column chromatography to obtain ephedrine; the used filler is macroporous resin HDX-5.
8. Concentrating the separated cannabis sativa extract solution at low temperature under reduced pressure, and draining to obtain cannabis sativa extract crystal; the low-temperature reduced pressure concentration temperature is 52 ℃, and the vacuum degree is 0.072 MPa.
9. Adding ethanol water solution according to the material ratio of 1:3 for dissolving, recovering solvent at low temperature under reduced pressure after complete dissolution, concentrating until cannabis yellow crystals are separated out, standing and cooling to obtain cannabis yellow crystal liquid.
10. Filtering the crystallization liquid by using a glass sand funnel to obtain high-purity ephedrine crystals, and putting the obtained crystals into a drying oven, wherein the vacuum degree is 0.08 MPa, the vacuum freeze-drying temperature is-65 ℃, and the freeze-drying time is 28 hours, so that the finished product of the ephedrine is obtained.
Example 3
Method for separating and purifying ephedrine
1. Taking 1000g of hemp flowers and leaves, crushing the hemp flowers and leaves by a high-speed crusher to 40 meshes, adding cellulase with the activity unit of 1000U/g, adding the cellulase with the addition amount of 0.1 g/kg of hemp flowers and leaves, stirring the mixture for 40min for enzymolysis at the pH value of 4.5 and the temperature of 45 ℃ and the rotation number of a stirring paddle of 20 r/min, and obtaining the cellulase enzymatic hydrolysis flowers and leaves.
2. Then the ratio of 1g: adding ethanol water solution with volume fraction of 30% into 4mL of the feed liquid, and stirring and extracting to obtain an extracting solution. The extraction temperature is 48 deg.C, the extraction time is 40min, and the extraction time is 2 times.
3. Filtering the extracting solution after extraction is finished, removing filter residues, putting the filtrate into a concentrator, recovering the solvent, and concentrating the extracting solution to 20% of the original volume after the solvent is recovered; the vacuum concentration temperature is 52 ℃, and the vacuum degree is 0.072 MPa.
4. Pouring the concentrated solution obtained in the step 3 into a 1000-mesh filter tank, pressurizing to 0.2MPa, and filtering to obtain a crude filtrate.
5. Filtering the obtained coarse filtrate with hollow fiber membrane with molecular weight of 1000D, and concentrating the obtained filtrate at low temperature under reduced pressure to 1/5 volume to obtain hemp flavone concentrated solution.
6. Separating the obtained hemp flavone concentrated solution by column chromatography to obtain ephedrine; the used filler is macroporous resin HDX-5.
7. Concentrating the separated cannabis sativa extract solution at low temperature under reduced pressure, and draining to obtain cannabis sativa extract crystal; the low-temperature reduced pressure concentration temperature is 52 ℃, and the vacuum degree is 0.072 MPa.
8. Adding ethanol water solution according to the material ratio of 1:3 for dissolving, recovering solvent at low temperature under reduced pressure after complete dissolution, concentrating until cannabis yellow crystals are separated out, standing and cooling to obtain cannabis yellow crystal liquid.
9. Filtering the crystallization liquid by using a glass sand funnel to obtain high-purity ephedrine crystals, and putting the obtained crystals into a drying oven, wherein the vacuum degree is 0.08 MPa, the vacuum freeze-drying temperature is-65 ℃, and the freeze-drying time is 28 hours, so that the finished product of the ephedrine is obtained.
Example 1 compared to example 2:
the method of example 1 is ethanol aqueous solution extraction combined with macroporous resin chromatography to extract the ephedrine, which is different from the present application in that the hemp flower and leaf are not subjected to enzymolysis treatment.
Example 3 compared to example 2:
the method of example 3 is an aqueous ethanol extraction coupled with macroporous resin chromatography to extract the ephedrine, which differs from the present application in that the extract is subjected to column chromatography without extraction.
The comparative analysis of the above examples gives: the method has the advantages of high extraction rate, high purity of the obtained cannabinoids, no cannabinoid and the like.
The foregoing shows and describes the general principles and features of the present invention, together with the advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. A method for separating and purifying the ephedrine is characterized by comprising the following steps:
step 1, enzymolysis: pulverizing hemp leaves into granules, and adding cellulase for enzymolysis;
step 2, extraction: adding ethanol water solution, and extracting at low temperature;
and step 3, concentrating: collecting extractive solution, filtering, and concentrating under reduced pressure at low temperature;
and 4, extraction: adjusting the concentrated solution to be alkaline, and adding n-hexane for extraction;
and 5, filtering: filtering the water phase liquid obtained in the step 4 under pressure;
and 6, membrane filtration: filtering the coarse filtrate obtained in the step 5 by using a membrane, and concentrating the obtained filtrate at low temperature under reduced pressure;
and 7, column chromatography: separating the hemp flavone concentrated solution obtained in the step 6 by column chromatography to obtain the ephedrine;
step 8, concentration: 7, concentrating and drying the separated cannabifolin at low temperature under reduced pressure;
step 9, crystallization: dissolving the cannabifolin crystal obtained in the step 8 by using an analytically pure grade ethanol water solution, and crystallizing;
step 10, drying: drying the obtained crystal at low temperature in vacuum to obtain pure cannabifolin.
2. The method for separating and purifying ephedrine according to claim 1, wherein in step 1, the hemp flower and leaf is pulverized into particles of 30-50 meshes, and cellulase is added for enzymolysis, wherein the enzymolysis activity unit of the cellulase is 1000U/g, and the addition amount is as follows: 0.1-0.2 g/kg pulp; enzymolysis pH: 4.5-6.5, the enzymolysis temperature is 45-55 ℃, and the time is 40-50 min.
3. The method for separating and purifying ephedrine according to claim 1, wherein the ethanol aqueous solution in step 2 is (20-50%), the low temperature extraction temperature is 45-58 deg.C, and the time is 30-60 min.
4. The method for separating and purifying ephedrine according to claim 1, wherein the low temperature vacuum concentration in step 3 is 45-60 deg.C, and the vacuum degree is 0.05-0.078 MPa.
5. The method for separating and purifying ephedrine according to claim 1, wherein the amount of NaOH aqueous solution in step 4 is 2-4%, the amount of n-hexane added in each time is 1.6-2.4 times of the concentrate, and the extraction times are 2-3.
6. The method for separating and purifying ephedrine according to claim 1, wherein the pressure filtration pressure in step 5 is 0.2MPa, and the filter screen is 1000 mesh.
7. The method for separating and purifying ephedrine according to claim 1, wherein the filtration in step 6 is performed by filtering the crude filtrate through a hollow fiber membrane with a molecular weight of 1000D.
8. The method for separating and purifying ephedrine according to claim 1, wherein the step 7 of chromatography is performed by eluting through macroporous resin column, wherein the macroporous resin column is AB-8, HDX-5, X-5 or DX 101.
9. The method for separating and purifying ephedrine according to claim 1, wherein the low temperature vacuum concentration in step 8 is 45-60 deg.C, and the vacuum degree is 0.05-0.078 MPa.
10. The method for separating and purifying ephedrine according to claim 1, wherein the drying in step 10 is vacuum freeze-drying under a vacuum degree of 0.07-0.08 MPa at a temperature of-65 deg.C to-50 deg.C for 24-28 h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111481479A (en) * | 2020-04-20 | 2020-08-04 | 中国农业科学院麻类研究所 | Method for extracting antioxidant component from cannabis sativa leaves and application of antioxidant component |
| CN111961021A (en) * | 2019-12-30 | 2020-11-20 | 云南汉盟制药有限公司 | Separation and purification process of high-purity geranylflavonoid A |
| CN114133335A (en) * | 2020-09-03 | 2022-03-04 | 中国科学院大连化学物理研究所 | A continuous preparation method for extracting ephedrine from herba Ephedrae |
-
2019
- 2019-11-15 CN CN201911116819.3A patent/CN110613751A/en not_active Withdrawn
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111961021A (en) * | 2019-12-30 | 2020-11-20 | 云南汉盟制药有限公司 | Separation and purification process of high-purity geranylflavonoid A |
| WO2021134965A1 (en) * | 2019-12-30 | 2021-07-08 | 云南汉盟制药有限公司 | Separation and purification process for cannflavin a |
| CN111961021B (en) * | 2019-12-30 | 2021-08-03 | 云南汉盟制药有限公司 | Separation and purification process of geranylflavone A |
| CN111481479A (en) * | 2020-04-20 | 2020-08-04 | 中国农业科学院麻类研究所 | Method for extracting antioxidant component from cannabis sativa leaves and application of antioxidant component |
| CN111481479B (en) * | 2020-04-20 | 2023-02-07 | 中国农业科学院麻类研究所 | Method for extracting antioxidant component from cannabis sativa leaves and application of antioxidant component |
| CN114133335A (en) * | 2020-09-03 | 2022-03-04 | 中国科学院大连化学物理研究所 | A continuous preparation method for extracting ephedrine from herba Ephedrae |
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