CN108409752A - A kind of extraction separation method of picrinine - Google Patents
A kind of extraction separation method of picrinine Download PDFInfo
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- CN108409752A CN108409752A CN201810562176.4A CN201810562176A CN108409752A CN 108409752 A CN108409752 A CN 108409752A CN 201810562176 A CN201810562176 A CN 201810562176A CN 108409752 A CN108409752 A CN 108409752A
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- picrinine
- chloroform
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- C07—ORGANIC CHEMISTRY
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- C07D498/00—Heterocyclic compounds containing in the condensed system at least one hetero ring having nitrogen and oxygen atoms as the only ring hetero atoms
- C07D498/22—Heterocyclic compounds containing in the condensed system at least one hetero ring having nitrogen and oxygen atoms as the only ring hetero atoms in which the condensed system contains four or more hetero rings
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Abstract
The invention discloses a kind of methods of picrinine extraction separation, this method is using alstonia-leaf as raw material, using technical process such as sour water extraction, chloroform extraction, the separation of resin column chromatography for separation, silica gel column chromatography, recrystallizations, the product of 98% or more content is made, the method of the present invention can efficiently separate picrinine, remove impurity, and method is simple, it is easy to operate, it is suitable for industrialized production and marketing application.
Description
Technical field
The method that the present invention relates to a kind of to extract separation picrinine from alstonia-leaf, belongs to compound separation field.
Background technology
Alstonia-leaf, scientific name Folium Alstoniae Scholaris, the ground such as production Guangdong, Yunnan, this product is Guangdong and Guangxi Provinces and cloud
The medication of Nan Dengdi ethnic groups.Once it recorded in ground prescription will such as《Luchuan book on Chinese herbal medicine》、《Yunnan Chinese herbal medicine choosing》In, and be《Yunnan Province
The drug standards》（1974）With《Chinese Pharmacopoeia》（Version one in 1977）It is recorded；After develop alstonia-leaf particle, lamp stand blade etc.
Several formulations, for cough-relieving, eliminating the phlegm and chronic bronchitis cough.
Alkaloid and flavones are the main components of alstonia-leaf, and cauline leaf contains a variety of indoles alkaloids, such as picrinine
（picrinine）, enlightening platform alkali（ditaine）, lamp stand make a mistake because of alkali（echitemine）, porphyrin alkali（porphyrine ）, etc..It is raw
Alkaloids are the important active materials of alstonia-leaf, are the marks of desk lamp leaf wherein with the content highest of picrinine (picrinine)
The property known ingredient, is the item controlled of preparation.
Picrinine is colourless acicular crystal, is soluble in methanol, chloroform, acetone, dissolves in ethyl acetate, ethyl alcohol,
Not soluble in water and petroleum ether；It is soluble in dilute hydrochloric acid and dilute sulfuric acid, adds after solution becomes cloudy after alkali neutralization and precipitation is precipitated again.Chemical name
For 2 α, 5 α-Epoxy-1,2-dihydroakuammilan-17-oicacidmethylester, chemical structural formula such as Formulas I institute
Show；
, Formulas I；
Alstonia-leaf is seldom to the research data of alstonia-leaf due to being ethnic group's medication, and picrinine is the mark of alstonia-leaf
The property known ingredient, is the item controlled of preparation, therefore finds a kind of method of separation picrinine, is carried out more to picrinine
It is necessary that multiple medicine, which is managed and carries out research with activity,.
Invention content
Present invention aims at a kind of method of the extraction separation picrinine from alstonia-leaf is provided, this method is with lamp stand
Leaf is raw material；It is achieved through the following technical solutions the object of the invention：
（1）The sour water that 5~7 times of its quality is added in dry alstonia-leaf decocts 2~3 times, 2~3 hours every time, filters；It closes
And filtrate, it is 1.05~1.10 that filtrate, which is concentrated into relative density, three times with chloroform extraction, removes chloroform layer, remaining raffinate is used
Adjusting PH with base is collected to 9~10, then three times with chloroform extraction and merges chloroform extract liquor, alkaloid is obtained after concentrate drying；
（2）The ethanol solution or methanol solution of alkaloid volumetric concentration 80~90% dissolve, and quality is added in filtering in filtrate
The triethylamine aqueous solution of concentration 0.01~0.02%, it is 25~30% to make ethyl alcohol or methanol concentration in filtrate, then passes through resin column
Alkaloid is adsorbed, first impurity is eluted with the eluent I of 3~4 times of column volumes, then eluted with eluent II, collects picrinine
Section eluent, concentration are drying to obtain picrinine crude product, wherein eluent I be by triethylamine be added to mass concentration 40~
The triethylamine methanol aqueous solution or three second of mass concentration 0.01~0.02% are made in 45% ethanol water or methanol aqueous solution
Amine ethanol water；Eluent II is the ethanol water or methanol aqueous solution that triethylamine is added to mass concentration 50~55%
In the triethylamine methanol aqueous solution or triethylamine ethanol water of mass concentration 0.01~0.02% is made；
（3）After the chloroform dissolving of 4~5 times of its quality of picrinine crude product, above enter in silicagel column, first with 2~3 times of column volumes
Chloroform elutes, then uses chlorofonn-ethylacetate gradient elution, collects picrinine section eluent, the dry dita leaves to obtain the final product of concentration
Alkali；
（4）By step（3）After picrinine acetone solution, petroleum ether to crystal is added dropwise and occurs, stands still for crystals, filters, instead
It operates 2~3 times again, last crystal vacuum drying is to get picrinine.
The step（1）In sour water be mass concentration 0.1~0.2% aqueous sulfuric acid or aqueous hydrochloric acid solution.
The step（1）In alkali be mass concentration 40~50% sodium hydrate aqueous solution.
The step（2）Resin in resin column is polyamide.
The step（2）The ethanol solution of 3~4 times of its quality of alkaloid dissolve.
The step（3）When middle gradient elution first with the volume ratio of 3~4 times of column volumes be 75~80:20~25 chloroform-
Ethyl elute impurity, then with volume ratio be 65~70:30~35 chloroform-ethyl elutes alkaloid.
The advantages of the method for the present invention and technique effect：Dita leaves alkali content in alstonia-leaf is very low, only one thousandth
Left and right, separation and purification are more difficult；The property of sour water is soluble in when the present invention extracts according to picrinine using 0.1~0.2%
Sour water extracts, and ensure that the recovery rate of picrinine, avoids using expensive organic solvent；According to dita leaves alkali salt
It is soluble in sour water, the chloroform extracting impurities of the characteristic insoluble in organic solvent；It is again easy in alkaline environment according to picrinine
Be dissolved in organic solvent characteristic chloroform is extracted after raffinate be tuned into after alkalinity and extract alkaloid with chloroform；The life being obtained by extraction
Alkaloids first use polyamide column chromatography, then take off column chromatography using silicon, finally obtain 98% or more content using means re-crystallization
Picrinine, the method for the present invention is simple to operation, be suitable for industrialized production and marketing application.
Specific implementation mode
With reference to embodiment, invention is further described in detail, but protection scope of the present invention be not limited to it is described
Content in the method for the present invention is unless otherwise specified all made of conventional method, unless otherwise specified using reagent, is all made of routine
The reagent or commercially available conventional reagent that method is prepared.
Embodiment 1：Alstonia-leaf 10kg is taken, the aqueous sulfuric acid 70kg of mass concentration 0.1% is added, boils 3 hours, is filtered,
Filter residue is added 0.1% aqueous sulfuric acid 50kg of mass concentration and boils again to be carried 3 hours, is filtered, and filtrate obtained by secondary filter, filter are merged
It is 1.05 that liquid, which is concentrated under reduced pressure into relative density, obtains clear cream 20kg；10kg chloroforms are added while stirring in clear cream, continue after adding
Stirring 5 minutes stands 2 hours, separates chloroform layer, and water layer repeats extraction 2 times with equal amounts of chloroform, merges chloroform extract liquor, recycling
Chloroform, concentrate make offal treatment；Water layer is adjusted to pH=9 with the sodium hydroxide of mass concentration 40%, with chloroform extract 3 times, often
Secondary dosage is 10kg, merges 3 chloroform extract liquors, and alkaloid is obtained after concentrate drying；The volumetric concentration of 3 times of its quality of alkaloid
The triethylamine aqueous solution of mass concentration 0.01% is added in filtrate, keeps ethyl alcohol in filtrate dense for 90% ethanol solution dissolving, filtering
Degree is 25%, then by polyamide resin column, with 4 column volume eluents I（Triethylamine is added to the second of mass concentration 40%
The triethylamine ethanol water of mass concentration 0.01% is made in alcohol solution）Impurity is eluted, then with eluent II（By triethylamine
It is added to the triethylamine ethanol water that mass concentration 0.01% is made in the ethanol water of mass concentration 50%）Elution biology
Alkali is collected and contains picrinine section eluent, is concentrated and dried to obtain picrinine crude product；Its quality of picrinine crude product
After 5 times of chloroform dissolving, above enter in silicagel column, first use the elutions of 2 times of column volume chloroforms, then with the volume ratio 80 of 3 times of column volumes：20
Chlorofonn-ethylacetate elution impurity, then use volume ratio 70：30 chlorofonn-ethylacetate elution biology
Alkali collects picrinine section eluent, is concentrated and dried, and finally with petroleum ether after acetone solution, is added dropwise to crystal appearance, stands
Crystallization, filtering operate 2 times repeatedly, and last crystal vacuum drying is to get picrinine crystal 4.2g, content 98.2%.
Embodiment 2：Alstonia-leaf 10kg is taken, the aqueous hydrochloric acid solution 60kg of mass concentration 0.1% is added, boils 2 hours, is filtered,
Filter residue is added 0.1% aqueous hydrochloric acid solution 60kg of mass concentration and boils again to be carried 2 hours, is filtered, and is repeated to boil and is carried primary, is merged three times
Filtering gained filtrate, it is 1.08 that filtrate decompression, which is concentrated into relative density, obtains clear cream 22kg；10kg is added while stirring in clear cream
Chloroform continues stirring 5 minutes after adding, stand 2 hours, separates chloroform layer, and water layer repeats extraction 2 times with equal amounts of chloroform, merges
Chloroform extract liquor, recycles chloroform, and concentrate makees offal treatment；Water layer is adjusted to pH=10 with 50% sodium hydroxide of mass concentration, uses
Chloroform extracts 3 times, and each dosage is 10 kg, merges 3 chloroform extraction fluids, and alkaloid is obtained after concentrate drying；Its quality of alkaloid
The methanol solution of 4 times of volumetric concentration 80% dissolves, and the triethylamine aqueous solution of mass concentration 0.02% is added in filtering in filtrate,
It is 30% to make methanol concentration in filtrate, then by polyamide resin column, with 3 column volume eluents I（Triethylamine is added to
The triethylamine methanol aqueous solution of mass concentration 0.02% is made in the methanol aqueous solution of mass concentration 45%）Impurity is eluted, then with washing
De- liquid II（Triethylamine is added to the triethylamine methanol-water that mass concentration 0.02% is made in the methanol aqueous solution of mass concentration 55%
Solution）Alkaloid is eluted, collects and contains picrinine section eluent, be concentrated and dried to obtain picrinine crude product；Dita leaves
The chloroform of 4 times of its quality of alkali crude product dissolves, and above enters in silicagel column, first uses 3 times of column volume chloroforms elutions, then with 4 times of column volumes
Volume ratio 75：Then 25 chlorofonn-ethylacetate elution impurity uses volume ratio 65：35 chlorofonn-ethylacetate is washed
De- liquid elutes alkaloid, collects picrinine section eluent, is concentrated and dried, and finally with after acetone solution, petroleum ether is added dropwise extremely
Crystal occurs, and stands still for crystals, and filters, and operates 3 times repeatedly, and last crystal vacuum drying is to get picrinine quartz crystal
3.8g, content 98.7%.
Embodiment 3：Alstonia-leaf 10kg is taken, 0.2% aqueous sulfuric acid 60kg of mass concentration is added, boils 2.5 hours, is filtered,
Filter residue is added 0.1% aqueous sulfuric acid 50kg of mass concentration and boils again to be carried 2 hours, is filtered, and filtrate obtained by secondary filter, filter are merged
It is 1.1 that liquid, which is concentrated under reduced pressure into relative density, obtains clear cream 17kg；10kg chloroforms are added while stirring in clear cream, continue after adding
Stirring 5 minutes stands 2 hours, separates chloroform layer, and water layer repeats extraction 2 times with equal amounts of chloroform, merges chloroform extract liquor, recycling
Chloroform, concentrate make offal treatment；Water layer is adjusted to pH=9.5 with 45% sodium hydroxide of mass concentration, with chloroform extract 3 times, often
Secondary dosage is 10 kg, merges 3 chloroform extraction fluids, obtains alkaloid；Alkaloid is molten with the ethyl alcohol of its 3.5 times of volumetric concentration 85% of quality
Liquid dissolves, and the triethylamine aqueous solution of mass concentration 0.015% is added in filtering in filtrate, and it is 28% to make concentration of alcohol in filtrate, so
Afterwards by polyamide resin column, with 3.5 column volume eluents I（Triethylamine is added to the ethanol water of mass concentration 42%
In the triethylamine ethanol water of mass concentration 0.015% is made）Impurity is eluted, then with eluent II（Triethylamine is added to matter
Measure the triethylamine ethanol water that mass concentration 0.014% is made in the ethanol water of concentration 53%）Alkaloid is eluted, collection contains
There is picrinine section eluent, is concentrated and dried to obtain picrinine crude product；The chlorine of 4.5 times of its quality of picrinine crude product
Imitative dissolving, above enters in silicagel column, first uses 2.5 times of column volume chloroforms elutions, then with the volume ratio 78 of 3.5 times of column volumes：22 chlorine
Then imitative-ethyl acetate elution impurity uses volume ratio 67：33 chlorofonn-ethylacetate elution alkaloid is received
Collect picrinine section eluent, be concentrated and dried, finally with petroleum ether after acetone solution, is added dropwise to crystal appearance, stands still for crystals,
Filtering operates 2 times repeatedly, and last crystal vacuum drying is to get picrinine crystal 4.5g, content 98.5%.
Embodiment 4：Alstonia-leaf 50kg is taken, the aqueous sulfuric acid 250kg of mass concentration 0.15% is added, boils 3 hours, mistake
Filter, the aqueous sulfuric acid 250kg that mass concentration 0.2% is added in filter residue again are boiled and are carried 3 hours, are filtered, and are repeated to boil and are carried primary, are closed
And 3 filtering gained filtrates, it is 1.08 that filtrate decompression, which is concentrated into relative density, obtains clear cream 110kg；Add while stirring in clear cream
Enter 50kg chloroforms, continue stirring 5 minutes after adding, stand 2 hours, separate chloroform layer, water layer repeats extraction 2 with equal amounts of chloroform
It is secondary, merge chloroform extract liquor, recycle chloroform, concentrate makees offal treatment；Water layer is adjusted to pH with 42% sodium hydroxide of mass concentration
=9, it is extracted 3 times with chloroform, each dosage is 50 kg, merges 3 chloroform extraction fluids, obtains alkaloid；Alkaloid 3 times of bodies of its quality
The triethylamine aqueous solution of mass concentration 0.02% is added in filtrate, makes in filtrate for the methanol solution dissolving of product concentration 88%, filtering
Methanol concentration is 26%, then by polyamide resin column, with 4 column volume eluents I（Triethylamine is added to mass concentration
The triethylamine methanol aqueous solution of mass concentration 0.02% is made in 40% methanol aqueous solution）Impurity is eluted, then with eluent II（It will
Triethylamine is added to the triethylamine methanol aqueous solution that mass concentration 0.02% is made in the methanol aqueous solution of mass concentration 50%）Elution
Alkaloid is collected and contains picrinine section eluent, is concentrated and dried to obtain picrinine crude product；Picrinine crude product uses it
The dissolving of the chloroform that 5 times of quality, above enters in silicagel column, first uses 3 times of column volume chloroforms elutions, then with the volume ratio 76 of 3 times of column volumes:
Then 24 chlorofonn-ethylacetate elution impurity use volume ratio 68:22 chlorofonn-ethylacetate elution biology
Alkali collects picrinine section eluent, is concentrated and dried, and finally with petroleum ether after acetone solution, is added dropwise to crystal appearance, stands
Crystallization, filtering operate 2 times repeatedly, and last crystal vacuum drying is to get picrinine crystal 23.2g, content 98.7%.
Embodiment 5：Alstonia-leaf 50kg is taken, 0.2% aqueous hydrochloric acid solution 300kg of mass concentration is added, boils 3 hours, is filtered,
Filter residue is added 0.2 % aqueous hydrochloric acid solutions 250kg of mass concentration and boils again to be carried 2 hours, is filtered, and 2 filtering gained filtrates, filter are merged
It is 1.1 that liquid, which is concentrated under reduced pressure into relative density, obtains clear cream 98kg；50kg chloroforms are added while stirring in clear cream, continue after adding
Stirring 5 minutes stands 2 hours, separates chloroform layer, and water layer repeats extraction 2 times with equal amounts of chloroform, merges chloroform extract liquor, recycling
Chloroform, concentrate make offal treatment；Water layer is adjusted to pH=10 with 45% sodium hydroxide of mass concentration, with chloroform extract 3 times, every time
Dosage is 50 kg, merges 3 chloroform extraction fluids, obtains alkaloid；Alkaloid is molten with the ethanol solution of its 3 times of volumetric concentration 85% of quality
The triethylamine aqueous solution of mass concentration 0.01% is added in solution, filtering in filtrate, and it is 27% to make concentration of alcohol in filtrate, is then led to
Polyamide resin column is crossed, with 3 column volume eluents I（Triethylamine is added in the ethanol water of mass concentration 45% and is made
The triethylamine ethanol water of mass concentration 0.01%）Impurity is eluted, then with eluent II（Triethylamine is added to mass concentration
The triethylamine ethanol water of mass concentration 0.02% is made in 54% ethanol water）Alkaloid is eluted, collects and contains duck foot
Leaf alkali section eluent, is concentrated and dried to obtain picrinine crude product；The chloroform of 4 times of its quality of picrinine crude product dissolves,
On enter in silicagel column, first eluted with 3 times of column volume chloroforms, then with the volume ratio 80 of 4 times of column volumes:20 chlorofonn-ethylacetate
Then elution impurity uses volume ratio 66:34 chlorofonn-ethylacetate elution alkaloid collects dita leaves
Alkali section eluent is concentrated and dried, and finally with petroleum ether after acetone solution, is added dropwise to crystal appearance, is stood still for crystals, is filtered, grasp repeatedly
Make 3 times, last crystal vacuum drying is to get picrinine quartz crystal 25.8g, content 98.2%.
Claims (6)
1. a kind of extraction separation method of picrinine, which is characterized in that include the following steps：
（1）The sour water that 5~7 times of its quality is added in dry alstonia-leaf decocts 2~3 times, 2~3 hours every time, filters；It closes
And filtrate, it is 1.05~1.10 that filtrate, which is concentrated into relative density, three times with chloroform extraction, removes chloroform layer, remaining raffinate is used
Adjusting PH with base is collected to 9~10, then three times with chloroform extraction and merges chloroform extract liquor, alkaloid is obtained after concentrate drying；
（2）The ethanol solution or methanol solution of alkaloid volumetric concentration 80~90% dissolve, and quality is added in filtering in filtrate
The triethylamine aqueous solution of concentration 0.01~0.02%, it is 25~30% to make ethyl alcohol or methanol concentration in filtrate, then passes through resin column
Alkaloid is adsorbed, first impurity is eluted with the eluent I of 3~4 times of column volumes, then eluted with eluent II, collects picrinine
Section eluent, concentration are drying to obtain picrinine crude product, wherein eluent I be by triethylamine be added to mass concentration 40~
The triethylamine methanol aqueous solution or three second of mass concentration 0.01~0.02% are made in 45% ethanol water or methanol aqueous solution
Amine ethanol water；Eluent II is the ethanol water or methanol aqueous solution that triethylamine is added to mass concentration 50~55%
In the triethylamine methanol aqueous solution or triethylamine ethanol water of mass concentration 0.01~0.02% is made；
（3）After the chloroform dissolving of 4~5 times of its quality of picrinine crude product, above enter in silicagel column, first with 2~3 times of column volumes
Chloroform elute, then use chlorofonn-ethylacetate gradient elution, collect picrinine section eluent, be concentrated and dried to obtain the final product dita
Leaf alkali；
（4）By step（3）After picrinine acetone solution, petroleum ether to crystal is added dropwise and occurs, stands still for crystals, filters, instead
It operates 2~3 times again, last crystal vacuum drying is to get picrinine.
2. the extraction separation method of picrinine according to claim 1, it is characterised in that：Step（1）In sour water
For the aqueous sulfuric acid or aqueous hydrochloric acid solution of mass concentration 0.1~0.2%.
3. the extraction separation method of picrinine according to claim 1, it is characterised in that：Step（1）In alkali be
The sodium hydrate aqueous solution of mass concentration 40~50%.
4. the extraction separation method of picrinine according to claim 1, it is characterised in that：Step（2）In resin column
Resin be polyamide.
5. the extraction separation method of picrinine according to claim 1, it is characterised in that：Step（2）Alkaloid
With 3~4 times of the ethanol solution dissolving of its quality.
6. the extraction separation method of picrinine according to claim 1, it is characterised in that：Step（3）Middle gradient is washed
When de- first with the volume ratio of 3~4 times of column volumes be 75~80:20~25 chloroform-ethyl elutes impurity, then uses volume ratio
It is 65~70:30~35 chloroform-ethyl elutes alkaloid.
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| CN201810562176.4A CN108409752B (en) | 2018-06-04 | 2018-06-04 | Method for extracting and separating picrinine |
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| CN201810562176.4A CN108409752B (en) | 2018-06-04 | 2018-06-04 | Method for extracting and separating picrinine |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101084894A (en) * | 2006-06-07 | 2007-12-12 | 中国科学院昆明植物研究所 | Medicine for treating diseases concerned with respiratory and use thereof |
| CN101658540A (en) * | 2009-09-24 | 2010-03-03 | 刘富来 | Method for preparing medicine for treating respiratory tract diseases caused by pig blue ear diseases and the like |
| CN102040613A (en) * | 2010-12-03 | 2011-05-04 | 昆明振华制药厂有限公司 | Picrinine reference substance in common alstonia leaf and preparation method thereof |
-
2018
- 2018-06-04 CN CN201810562176.4A patent/CN108409752B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101084894A (en) * | 2006-06-07 | 2007-12-12 | 中国科学院昆明植物研究所 | Medicine for treating diseases concerned with respiratory and use thereof |
| CN101658540A (en) * | 2009-09-24 | 2010-03-03 | 刘富来 | Method for preparing medicine for treating respiratory tract diseases caused by pig blue ear diseases and the like |
| CN102040613A (en) * | 2010-12-03 | 2011-05-04 | 昆明振华制药厂有限公司 | Picrinine reference substance in common alstonia leaf and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 赵春杰: "《中药学专业知识（二）》", 30 April 2014, 人民军医出版社 * |
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