CN111808103A - Clean production method for extracting tabersonine from African voacanga - Google Patents
Clean production method for extracting tabersonine from African voacanga Download PDFInfo
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Abstract
The invention provides a clean production method for extracting tabersonine from African voacanga, which comprises the following steps: (1) reflux extraction: crushing African voaca fruit raw materials, putting into an extraction tank, adding a mixed solvent of a lipophilic organic solvent containing a hydrophobic betaine derivative and a medium-polarity organic solvent, heating and refluxing, and filtering to obtain a mixed solvent extracting solution. (2) Silica gel column adsorption: and (3) passing the mixed solvent extracting solution through a silica gel chromatographic column, collecting the effluent of the silica gel chromatographic column, and concentrating until no solvent exists to obtain a brown yellow oily substance, namely the acorn volatile oil. (3) Silica gel column elution: eluting the silica gel chromatographic column with an eluant, collecting the eluent, and concentrating the eluent under reduced pressure. Cooling the concentrated solution, stirring for crystallization, performing suction filtration, and drying to obtain a tabersonine finished product. The method does not use inorganic acid, alkali and water, does not discharge sewage and waste gas, has high content and high yield of tabersonine finished products, is green and environment-friendly, and is suitable for industrial production.
Description
Technical Field
The invention relates to a separation method of active ingredients of African voacanga, in particular to a clean production method for extracting tabersonine from African voacanga.
Background
African muguet (Voacanga Africana), also known as African Voacanga, is a perennial arbor of the genus Marguet of the family Apocynaceae, and is mainly distributed between African Sagnac and Sudan, Angora, and West African, Congo, and tanzania. African lilac fruit has a long medicinal history in traditional medicine in African regions, and the whole strain can be used as a medicine and is often used for treating diseases such as leprosy, dysentery, malaria, systemic edema, epilepsy and infantile convulsion. Pharmacological activity research shows that the African voaca has the activities of resisting tumor, bacteria, inflammation and malaria, inhibiting angiogenesis, improving memory, calming, hypnotizing, giving up drugs, removing addiction and the like, and has extremely high medicinal value. At present, African Voacanga chalotiana has been introduced and domesticated by domestic scientific research units.
African strobilus custard is rich in indole alkaloids with cardiotonic, antibacterial, antiulcer, and antioxidant effects, such as: tabersonine, laojiu amine, laojiu alkali, laojiu Ling, voacangine, etc. In particular, tabersonine (tabersonine), also known as tabersonine, has the highest attention because it is a precursor of vincristine, a cancer chemotherapy drug, and has been industrially produced at present in China.
The Voacanga seed is rich in volatile oil, which has effects in repairing cell membrane, enhancing cell resistance, and preventing skin inflammation, and can be used in cosmetics and health products. The literature reports that the Voacanga seed volatile oil mainly comprises fatty acids, esters, hydrocarbons and a small amount of phenols.
In the technical scheme of extracting tabersonine from Voacanga chalotiana in the prior art, a large amount of low-boiling organic solvent is often used, and the solvent loss is large after multiple times of extraction and distillation; and a lot of needs use diluted acid aqueous solution, and the waste water that produces is more, handles waste water and further raises the cost and produces the pressure of environmental protection.
CN201010609832.5 discloses a method for extracting tabersonine from Voacanga chalotiana, which comprises the steps of crushing Voacanga chalotiana as a raw material, extracting with acid water, adjusting alkali, filtering, extracting, crystallizing and the like to obtain a tabersonine product. The yield of the alkali adjusting and precipitating process is difficult to control, and limited tabersonine is suspended or dissolved in a large amount of alkali liquor after alkali adjustment and is difficult to completely separate out and precipitate, so the yield of tabersonine prepared by the method is low.
CN201210165108.7 discloses a new technology for extracting tabersonine from Voacanga chalotiana Pierre ex Stapf based on enzymatic hydrolysis, which takes dry Voacanga chalotiana Stapf seeds as raw materials, and obtains tabersonine products through the steps of crushing, petroleum ether degreasing, enzymolysis, lower alcohol extraction, reduced pressure distillation concentration, drying crystallization and the like. In the enzymolysis process of the method, tabersonine is unstable in property and has the risk of being degraded; if the degreasing is insufficient, a large amount of fat-soluble impurities are leached in the subsequent alcohol extraction process, so that the yield and the content of tabersonine crystals are influenced.
CN201810284666.2 discloses a method for extracting tabersonine from African voacanga fruit, which takes seeds of African voacanga fruit as raw materials, and obtains tabersonine products through the steps of crushing, sulfuric acid solution soaking and percolating, filtering, macroporous resin adsorption and desorption, concentration and centrifugation and the like. The tabersonine product obtained by the method has low content, large sewage discharge and serious environmental pollution.
CN201410053307.8 discloses a novel extraction and separation technology of tabersonine hydrochloride in African plant Voacanga chalotiana, which comprises the steps of taking African Voacanga chalotiana as a raw material, extracting by alkaline methanol or ethanol, dissolving by acid water, degreasing, alkalifying, extracting by an organic solvent, concentrating, back extracting by acid water, concentrating, crystallizing and the like to obtain tabersonine hydrochloride (i.e. tabersonine hydrochloride). The method has complicated steps, and the dosage of acid, alkali and organic solvent is large, so the method is not suitable for industrial production.
In the patent US3758478, a tabersonine extraction and separation method is reported, which adopts the steps of organic solvent extraction, multiple acid water washing, alkalization, organic solvent extraction, recrystallization and the like to separate and purify tabersonine, the method has the disadvantages of complex operation process, low tabersonine yield, difficult industrial production, and great harm to production personnel due to the adoption of toxic solvents such as benzene, chloroform and the like.
CN201310613225.X discloses a clean process for extracting tabersonine from Voacanga chalotiana, which comprises husking seed of Voacanga chalotiana, micronizing, reflux-extracting with ethyl acetate, concentrating, adding TritonX-114 water solution, stirring under heat preservation, and standing for several times. The method needs expensive equipment investment such as superfine grinding, ultrasonic extraction and the like, the steps are relatively complicated, and a large amount of TritonX-114 residues possibly exist in the product, so that the method is not suitable for industrial production. In addition, the method uses concentrated hydrochloric acid and water, and waste water is discharged, so that the method cannot be called as a real cleaning process. In addition, the detection method of the patent for the product is not an external standard method, but a normalization method. The purity of the product tested by the normalization method is still very defective, and moisture, inorganic salt and impurity components which cannot be displayed under the liquid phase condition cannot be reflected by the normalization method. Therefore, the product tabersonine obtained by the patent method has the purity of 99 percent, and the actual purity has defects.
Therefore, a clean production method for extracting tabersonine from African voacanga fruit, which is green and environment-friendly, does not use inorganic acid, alkali and water, does not discharge three wastes, has high purity and high yield, and is suitable for industrial production, is urgently needed.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects in the prior art, provides a green and environment-friendly method for extracting tabersonine from various African voacanga seeds, and the method has the advantages of coherent and simple process, strong operability, low production cost, high content and high yield of tabersonine finished products, no use of inorganic acid, alkali and water, no discharge of three wastes and suitability for industrial production.
The technical scheme adopted by the invention for solving the technical problems is as follows: a clean production method for extracting tabersonine from African voacanga comprises the following steps:
(1) reflux extraction: crushing African voaca fruit raw materials, putting into an extraction tank, adding a mixed solvent of a lipophilic organic solvent containing a hydrophobic betaine derivative and a medium-polarity organic solvent, heating and refluxing, and filtering to obtain a mixed solvent extracting solution;
(2) silica gel column adsorption: passing the mixed solvent extractive solution through silica gel chromatographic column, collecting silica gel chromatographic column effluent, and concentrating until no solvent is present to obtain brown yellow oily substance, i.e. Voacanga seed volatile oil;
(3) silica gel column elution: eluting the silica gel chromatographic column with an eluant, collecting the eluent, and concentrating the eluent under reduced pressure. Cooling the concentrated solution, stirring for crystallization, performing suction filtration, and drying to obtain a tabersonine finished product.
Preferably, in the step (1), the hydrophobic betaine derivative is selected from at least one of dodecyl dimethyl betaine, tetradecyl dimethyl betaine, hexadecyl dimethyl betaine, castor oil betaine, tall oil betaine, and dialkyl phosphate betaine.
Further preferably, the amount of the hydrophobic betaine derivative is 6-10 per mill of the weight of the African voaca fruit raw material.
The hydrophobic betaine derivative is an amphoteric surfactant, and the inventor finds that when the hydrophobic betaine derivative is heated and refluxed for extraction, a small amount of the hydrophobic betaine derivative can be added to reduce the surface tension of a solvent, increase the extraction rate of the solvent on tabersonine, protect tabersonine molecular structures from being oxidized and decomposed in the heating process, effectively protect the tabersonine molecular structures and improve the yield of tabersonine products.
Preferably, in the step (1), the lipophilic organic solvent is at least one of diethyl ether, petroleum ether, n-hexane, cyclohexane, 6# solvent oil and 120# solvent oil; the medium polarity organic solvent is at least one selected from ethyl acetate, methyl acetate, propyl acetate, butyl acetate, dichloromethane and chloroform.
The ratio (V/V) of the lipophilic organic solvent to the ethyl acetate is 15-20: 1.
preferably, in the step (1), the total amount of the mixed solvent of the lipophilic organic solvent and the ethyl acetate is 15-20 times (L/kg) of the weight of the African strobilus Linnaeus raw material. The purpose of heating, refluxing and extracting twice by using a mixed solvent of a lipophilic organic solvent and ethyl acetate is to fully leach tabersonine in the African voacanga fruit raw material.
Preferably, in the step (1), the heating reflux of the mixed solvent of the lipophilic organic solvent and the ethyl acetate is divided into more than two times, the amount of the mixed solvent added in each time is gradually reduced according to 10-30%, and the extraction time is gradually reduced according to 20-50%. The advantage of multiple reflux extractions is that the desired product tabersonine can be fully leached.
For example, the heating reflux of the mixed solvent in the step (1) is divided into two times of extraction, the amount of the mixed solvent used in the first extraction is 8-12 times of the weight of the African fringed lily fruit raw material, and the extraction time is 2-3 hours; the dosage of the mixed solvent in the second extraction is 6-8 times of the weight of the African voaca fruit raw material, and the extraction time is 1-2 hours.
Preferably, in the step (2), the volume consumption of the silica gel for column chromatography is 0.2-0.5 times (L/kg) of the weight of the African voacanthus fruit raw material, the height-diameter ratio of the silica gel chromatographic column is 5-8: 1, and the flow rate of the silica gel chromatographic column is 0.5-1.0 BV/h. The purpose of enabling the mixed solvent extracting solution to pass through a silica gel chromatographic column is to separate tabersonine and volatile oil in the mixed solvent extracting solution by utilizing the characteristic that silica gel can adsorb tabersonine but does not adsorb Voacanga chalotiana volatile oil, so that tabersonine is enriched in the silica gel chromatographic column.
Preferably, in the step (3), the eluent is a mixed solvent of a lipophilic organic solvent and a medium-polarity organic solvent, wherein the lipophilic organic solvent is at least one selected from diethyl ether, petroleum ether, n-hexane, cyclohexane, 6# solvent oil and 120# solvent oil; the medium-polarity organic solvent is selected from at least one of ethyl acetate, methyl acetate, propyl acetate, butyl acetate, dichloromethane and chloroform; the ratio (V/V) of the lipophilic organic solvent to the medium polar solvent is 8-12: 1.
preferably, in the step (3), the eluent contains 0.1-1% of acetic acid (V/V). The purpose of adding a small amount of acetic acid into the eluent is to moderately increase the polarity of the eluent, increase the concentrated elution capacity of the eluent on the tabersonine and simultaneously reduce the dosage of the eluent.
Further preferably, in the step (3), the eluent contains 0.2% to 0.5% of acetic acid (V/V).
Preferably, in the step (3), the dosage of the eluent is 2-4 BV, and the elution flow rate is 0.5-1.0 BV/hour. The purpose of eluting the silica gel chromatographic column with an eluent is to desorb the tabersonine adsorbed in the silica gel resin column.
Preferably, in the step (3), the concentration of the solid in the concentrated solution is 20-25%, the temperature for cooling is 5-10 ℃, the stirring speed is 30-90 r/min, and the time for crystallization is 12-24 hours.
In the present invention, 1BV is 1 packed column volume.
The principle of the method of the invention is as follows:
after the African voaca fruit raw material is crushed, the mixed solvent of lipophilic organic solvent and ethyl acetate is used for heating reflux extraction, so that tabersonine and volatile oil in the African voaca fruit raw material can be fully leached out. The tabersonine can be adsorbed by silica gel and the volatile oil can not be adsorbed by silica gel after separation by silica gel chromatographic column, thereby realizing separation of the tabersonine and the volatile oil. Eluting with eluent, desorbing tabersonine from silica gel chromatographic column, concentrating, and crystallizing to obtain tabersonine product with high content.
The method has the following beneficial effects:
(1) the method provided by the invention is a green and environment-friendly method for extracting tabersonine from African voacanga fruit, and has the advantages of coherent and simple process, strong operability, low production cost, high content of tabersonine finished products, high yield and suitability for industrial production.
(2) In the production process, inorganic acid, alkali and water are not used, and no sewage or waste gas is discharged; the solvent in the extraction residue can be recovered to be clean, and can be used as a good raw material for extracting active ingredients such as tabersonine polysaccharide, flavone and the like, and can also be used as feed or organic fertilizer and the like, and basically no waste residue is discharged.
(3) In the invention, a small amount of hydrophobic betaine derivatives are added during heating reflux extraction, so that the extraction rate of tabersonine can be increased in the heating process, the molecular structure of the extracted tabersonine can be effectively protected from being damaged (oxidized or decomposed) at high temperature, and the yield of tabersonine is further improved.
(4) In the production process, the recovered mixed solvent can be used for reflux extraction of the next batch, the recovered eluent can be used for elution of the next batch, and the silica gel can be recycled after regeneration, so that clean production can be really realized.
Detailed Description
The present invention will be further described with reference to the following examples.
The African voaca fruit seed raw material used in the embodiment of the invention is purchased from African gardner, wherein the content of tabersonine is 2.35%; the column chromatography silica gel used in the embodiment of the invention is purchased from Qingdao ocean chemical Co., Ltd; tetradecyl betaine (BS-14), a castor oil betaine procurement from Shanghai Chuxing chemical Co., Ltd; the adjuvants or chemicals used in the examples of the present invention are commercially available in the usual manner unless otherwise specified.
In the embodiment of the invention, the content of tabersonine is detected by adopting a High Performance Liquid Chromatography (HPLC) external standard method.
Example 1
(1) Reflux extraction: taking 100kg of African voaca seed raw material, crushing the raw material until the particle size is 1-2 mm, putting the crushed raw material into an extraction tank, and adding a mixed solvent of petroleum ether and ethyl acetate, wherein the weight ratio of the petroleum ether: ethyl acetate 18: 1, (V/V), wherein the mixed solvent contains 0.8kg of castor oil betaine, the heating reflux extraction is carried out twice (the dosage of the mixed solvent for the first extraction is 1000L, the reflux time is 3 hours, the dosage of the mixed solvent for the first extraction is 900L, the reflux time is 1.5 hours), the filtration is carried out, and the two extracting solutions are combined to obtain the mixed solvent extracting solution.
(2) Silica gel column adsorption: the mixed solvent extract was passed through a silica gel column chromatography (column chromatography silica gel amount: 30L, height to diameter ratio of silica gel column: 6:1) at a flow rate of 0.5 BV/hr. Collecting eluate of silica gel chromatography column, and concentrating until no solvent is present to obtain brown yellow oily substance, i.e. Voacanga Artocarpa volatile oil.
(3) Silica gel column elution: the silica gel column was eluted with 4BV of eluent at a flow rate of 0.8 BV/h. The eluent is a mixed solvent of petroleum ether and ethyl acetate, wherein the ratio of petroleum ether: ethyl acetate 10: 1, (V/V), 0.2% acetic acid is also contained in the eluent. Collecting eluate, concentrating under reduced pressure until the concentration of solid in the concentrated solution is 22%, cooling to 5 deg.C, stirring at 60r/min for crystallization for 16 hr, vacuum filtering, and drying to obtain 2.29kg of tabersonine product.
The content of tabersonine obtained in this example was 99.13% and the yield of tabersonine was 96.60% as determined by High Performance Liquid Chromatography (HPLC) external standard method.
Example 2
(1) Reflux extraction: taking 100kg of African voaca seed raw material, crushing the raw material until the particle size is 1-2 mm, putting the crushed raw material into an extraction tank, adding a mixed solvent containing No. 6 solvent oil and ethyl acetate, 6 solvent oil: ethyl acetate ═ 20: 1(V/V), wherein the mixed solvent contains 0.6kg of castor oil betaine, the heating reflux extraction is carried out twice (the dosage of the mixed solvent for the first extraction is 1000L, the reflux time is 2.5 hours; the dosage of the mixed solvent for the first extraction is 800L, the reflux time is 2 hours), the filtration is carried out, and the two extracting solutions are combined to obtain the mixed solvent extracting solution.
(2) Silica gel column adsorption: the mixed solvent extract was passed through a silica gel column chromatography (column chromatography silica gel amount 25L, height/diameter ratio of silica gel column 8:1) at a flow rate of 0.8 BV/hr. Collecting eluate of silica gel chromatography column, and concentrating until no solvent is present to obtain brown yellow oily substance, i.e. Voacanga Artocarpa volatile oil.
(3) Silica gel column elution: the silica gel column was eluted with 3BV of eluent at a flow rate of 1.0 BV/h. The eluent is a mixed solvent of 6# solvent oil and ethyl acetate, wherein the ratio of 6# solvent oil: ethyl acetate ═ 8:1, (V/V), 0.5% acetic acid is also contained in the eluent. Collecting eluate, concentrating under reduced pressure until the concentration of solid in the concentrated solution is 23%, cooling to 6 deg.C, stirring at 30r/min for crystallization for 18 hr, filtering, and drying to obtain 2.22kg of tabersonine product.
The content of tabersonine obtained in this example was 98.85% and the yield of tabersonine was 94.22% as determined by High Performance Liquid Chromatography (HPLC) external standard method.
Example 3
(1) Reflux extraction: taking 100kg of African voaca seed raw material, crushing the raw material until the particle size is 1-2 mm, putting the crushed raw material into an extraction tank, adding a mixed solvent of cyclohexane and ethyl acetate, wherein the mixed solvent comprises the following components: ethyl acetate 15: 1, (V/V), wherein the mixed solvent contains 1kg of castor oil betaine, the heating reflux extraction is carried out twice (the dosage of the mixed solvent for the first extraction is 900L, the reflux time is 3 hours, the dosage of the mixed solvent for the first extraction is 800L, the reflux time is 2 hours), the filtration is carried out, and the two extracting solutions are combined to obtain the mixed solvent extracting solution.
(2) Silica gel column adsorption: and (3) enabling the mixed solvent extracting solution to pass through a silica gel chromatographic column at the flow rate of 0.6 BV/h, wherein the using amount of column chromatography silica gel is 28L, and the height-diameter ratio of the silica gel chromatographic column is 7: 1. Collecting eluate of silica gel chromatography column, and concentrating until no solvent is present to obtain brown yellow oily substance, i.e. Voacanga Artocarpa volatile oil.
(3) Silica gel column elution: the silica gel column was eluted with 2.5BV of eluent at a flow rate of 0.6 BV/h. The eluent is a mixed solvent of cyclohexane and methyl acetate, wherein the ratio of cyclohexane: methyl acetate 12: 1, (V/V), 0.3% acetic acid is also contained in the eluent. Collecting eluate, concentrating under reduced pressure until the concentration of solid in the concentrated solution is 20%, cooling to 8 deg.C, stirring at 90r/min for crystallization for 20 hr, vacuum filtering, and drying to obtain 2.24kg of tabersonine product.
The content of tabersonine obtained in this example was 98.52% and the yield of tabersonine was 93.91% as determined by High Performance Liquid Chromatography (HPLC) external standard method.
Example 4
The other conditions and procedure were the same as in example 1 except that in the reflux extraction of step (1), the ratio of petroleum ether: ethyl acetate ═ 12: 1, (V/V). The content of tabersonine obtained in this example was 99.24% and the yield of tabersonine was 93.32% as determined by High Performance Liquid Chromatography (HPLC) external standard method.
Example 5
The other conditions and procedure were the same as in example 1 except that in the reflux extraction of step (1), the ratio of petroleum ether: ethyl acetate 24: 1, (V/V). The content of tabersonine obtained in this example was 98.84% and the yield of tabersonine was 91.27% as determined by High Performance Liquid Chromatography (HPLC) external standard method.
Example 6
The other conditions and procedure were the same as in example 1 except that in the step (3) of silica gel column elution, petroleum ether: ethyl acetate ═ 6:1, (V/V). The content of tabersonine obtained in this example was 92.34% and the yield of tabersonine was 95.27% as determined by High Performance Liquid Chromatography (HPLC) external standard method.
Example 7
The other conditions and procedure were the same as in example 1 except that in the step (3) of silica gel column elution, petroleum ether: ethyl acetate 15: 1, (V/V). The content of tabersonine obtained in this example was 99.23% and the yield of tabersonine was 86.98% as determined by High Performance Liquid Chromatography (HPLC) external standard method.
Example 8
The other conditions and procedure were the same as in example 1 except that in the reflux extraction of step (1), the castor oil betaine in the mixed solvent was replaced with tetradecyl betaine of equal mass. The content of tabersonine obtained in this example was 99.07% and the yield of tabersonine was 94.85% as determined by High Performance Liquid Chromatography (HPLC) external standard method.
Example 9
The other conditions and procedure were the same as in example 1 except that in the reflux extraction of step (1), the amount of castor oil betaine in the mixed solvent was 0.4 kg. The content of tabersonine obtained in this example was 98.72% and the yield of tabersonine was 92.41% as determined by High Performance Liquid Chromatography (HPLC) external standard method.
Example 10
The other conditions and procedure were the same as in example 1 except that in the reflux extraction of step (1), the amount of castor oil betaine in the mixed solvent was 1.2 kg. The content of tabersonine obtained in this example was 99.18% and the yield of tabersonine was 94.54% as determined by High Performance Liquid Chromatography (HPLC) external standard method.
Example 11
The other conditions and procedure were the same as in example 1 except that acetic acid was not contained in the eluent in the silica gel column elution of step (3). The content of tabersonine obtained in this example was 98.93% and the yield of tabersonine was 93.74%, as determined by High Performance Liquid Chromatography (HPLC) external standard method.
Comparative example 1
The other conditions and procedures were the same as in example 1 except that in the reflux extraction of step (1), the mixed solvent contained no castor oil betaine. The content of tabersonine obtained in this example was 96.73% and the yield of tabersonine was 86.44% as determined by High Performance Liquid Chromatography (HPLC) external standard method.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. A clean production method for extracting tabersonine from African voacanga comprises the following steps:
(1) reflux extraction: crushing African voaca fruit raw materials, putting into an extraction tank, adding a mixed solvent of a lipophilic organic solvent containing a hydrophobic betaine derivative and a medium-polarity organic solvent, heating and refluxing, and filtering to obtain a mixed solvent extracting solution;
(2) silica gel column adsorption: passing the mixed solvent extractive solution through silica gel chromatographic column, collecting silica gel chromatographic column effluent, and concentrating until no solvent is present to obtain brown yellow oily substance, i.e. Voacanga seed volatile oil;
(3) silica gel column elution: eluting the silica gel chromatographic column with an eluant, collecting the eluant, concentrating the eluant under reduced pressure, cooling the concentrated solution, stirring for crystallization, performing suction filtration, and drying to obtain a tabersonine finished product.
2. The method of claim 1, wherein in step (1), the hydrophobic betaine derivative is at least one selected from the group consisting of dodecyl dimethyl betaine, tetradecyl dimethyl betaine, hexadecyl dimethyl betaine, castor oil betaine, tall oil betaine, and dialkyl phosphate betaine.
3. The method according to claim 1 or 2, wherein the hydrophobic betaine derivative is present in an amount of 6 to 10% by weight of the African muguet raw material.
4. The method according to claim 1 or 2, wherein in the step (1), the lipophilic organic solvent is at least one of diethyl ether, petroleum ether, n-hexane, cyclohexane, mineral spirit # 6, mineral spirit # 120; the medium polarity organic solvent is at least one selected from ethyl acetate, methyl acetate, propyl acetate, butyl acetate, dichloromethane and chloroform.
5. The method according to claim 4, wherein the ratio (V/V) of the lipophilic organic solvent to the ethyl acetate is 15 to 20: 1; the total dosage of the mixed solvent of the lipophilic organic solvent and the ethyl acetate is 15-20 times (L/kg) of the weight of the African voacanga seed raw material.
6. The method according to claim 5, wherein in the step (1), the heating reflux of the mixed solvent of the lipophilic organic solvent and the medium-polarity organic solvent is performed in two or more times, the amount of the mixed solvent added in each time is decreased by 10 to 30%, and the extraction time is decreased by 20 to 50%.
7. The method according to claim 1, wherein in the step (2), the volume consumption of the column chromatography silica gel is 0.2-0.5 times (L/kg) of the weight of the African fringed fruit raw material, the height-diameter ratio of the silica gel chromatography column is 5-8: 1, and the flow rate of the silica gel chromatography column is 0.5-1.0 BV/h.
8. The method as claimed in claim 1, wherein in the step (3), the eluent is a mixed solvent of a lipophilic organic solvent and a medium-polarity organic solvent, wherein the lipophilic organic solvent is at least one selected from diethyl ether, petroleum ether, n-hexane, cyclohexane, 6# solvent oil and 120# solvent oil; the medium-polarity organic solvent is selected from at least one of ethyl acetate, methyl acetate, propyl acetate, butyl acetate, dichloromethane and chloroform; the ratio (V/V) of the lipophilic organic solvent to the medium polar solvent is 8-12: 1.
9. the method as claimed in claim 8, wherein the eluent contains 0.1-1% acetic acid (V/V); preferably, the eluent contains 0.2-0.5% of acetic acid (V/V).
10. The method according to claim 1, wherein in the step (3), the amount of the eluent is 2-4 BV, and the elution flow rate is 0.5-1.0 BV/hr. Eluting the silica gel chromatographic column with an eluent to desorb the tabersonine adsorbed in the silica gel resin column; and/or
The concentration of solid matters in the concentrated solution is 20-25%, the temperature for cooling is 5-10 ℃, the stirring speed is 30-90 r/min, and the crystallization time is 12-24 hours.
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| CN102477035B (en) * | 2010-11-23 | 2014-12-10 | 成都合盛生物技术有限公司 | Cleaning process for extracting and purifying tabersonine from voacango Africana stapf seeds |
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