CN104193756A - Method for extracting securinine from securinega - Google Patents
Method for extracting securinine from securinega Download PDFInfo
- Publication number
- CN104193756A CN104193756A CN201410446369.5A CN201410446369A CN104193756A CN 104193756 A CN104193756 A CN 104193756A CN 201410446369 A CN201410446369 A CN 201410446369A CN 104193756 A CN104193756 A CN 104193756A
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- alkali
- leaf reed
- leaf
- extracting
- reed
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D491/00—Heterocyclic compounds containing in the condensed ring system both one or more rings having oxygen atoms as the only ring hetero atoms and one or more rings having nitrogen atoms as the only ring hetero atoms, not provided for by groups C07D451/00 - C07D459/00, C07D463/00, C07D477/00 or C07D489/00
- C07D491/12—Heterocyclic compounds containing in the condensed ring system both one or more rings having oxygen atoms as the only ring hetero atoms and one or more rings having nitrogen atoms as the only ring hetero atoms, not provided for by groups C07D451/00 - C07D459/00, C07D463/00, C07D477/00 or C07D489/00 in which the condensed system contains three hetero rings
- C07D491/20—Spiro-condensed systems
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Medicines Containing Plant Substances (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention relates to a method for extracting securinine from securinega. The method comprises the following processing steps: a. drying securinega branches and leaves in an 80DEG C drying oven, grinding and sieving with a 60-mesh sieve; b. in an acidic solution, performing continuous reverse-flow ultrasonic extraction; c. performing alkali neutralization, separating through macroporous adsorptive resin, and eluting with ammonia water-ethanol solution; and d. performing reduced-pressure concentration until the volume is one fifth of original volume, cooling and crystalizing, filtering, and recrystallizing twice with 80% ethanol to obtain yellow securinine needle crystals. The securinine is extracted by performing continuous reverse-flow ultrasonic extraction through adopting modern extraction technology, the method has the advantages of being simple in technology, small in energy consumption, short in extraction time and low in cost, and is suitable for industrial mass production.
Description
Technical field
The invention belongs to natural product chemistry field, relate to a kind of method of extracting leaf reed alkali from a leaf reed, relate in particular to a kind of method of utilizing continuous countercurrent ultrasonic extraction one leaf reed alkali.
Background technology
Medicinal leaf reed is browse and the root of euphorbia plant one leaf reed, different name Suffrutescent Securinega Twig.One leaf reed taste is pungent, bitter, warm in nature, poisonous.Have activate blood and relax tendons, effect of tonifying speen and tonifying kidney, can be used for lumbago due to pathogenic wind-dampness, numbness of the limbs, hemiplegia, impotence, facioplegia, poliomyelitis sequela.One leaf reed contains multiple alkaloid, wherein taking leaf reed alkali as main component.Find that via Chinese scholars research leaf reed alkali is in the memory that medically can significantly improve senile dementia patient, in addition, also there is many biologic activity such as the reverse transcription that suppresses tumor proliferative, supports bacterial-infection resisting, anti-malarial, effectively suppresses viruses molecule copies, there is vast potential for future development.
Patent and the document of the current extraction about leaf reed alkali are less, mainly adopt traditional organic solvent to soak extraction method.This technique organic solvent amount of expending is large, the production cycle is long, environmental pollution is serious.So, explore a production technique simple to operate, that production efficiency is high most important.
The principle of ultrasonic wave leaching is that ultrasonic wave is applied on thing to be leached, and by hyperacoustic high-frequency mechanical vibration, accelerates breaking and the transfer of material of cell walls, improves leaching efficiency.In the time utilizing ultrasonic wave to leach, ultrasonic wave can be sent ten thousand hertz or even up to the ultrasonic frequency of several megahertzes, there will be acoustic cavitation, acoustic streaming, acoustic radiation force in communication process.Ultrasonic energy also can be converted into heat energy simultaneously, is that internal temperature raises in moment, accelerates the dissolving of effective constituent.There is not yet so far the effective constituent of closing continuous countercurrent supersound extraction one leaf reed, particularly extract the research report of leaf reed alkali.
Summary of the invention
The object of this invention is to provide the method for extraction one leaf reed alkali that a kind of technique is simple, easy to operate, extraction time is short, production efficiency is high.
The present invention includes following steps:
A. leaf reed branch, leaf, through natural drying, in 80 DEG C of drying in oven, were pulverized 60 mesh sieves;
B. get leaf reed meal, add 0.5 ~ 2% the aqueous sulfuric acid of 5 ~ 7 times, be placed in continuous countercurrent ultrasonic extraction device, under 60 ~ 70 DEG C, 50 ~ 70KHz, extract 2 ~ 3h;
C. by centrifugal above-mentioned extracting solution, get supernatant liquor, in alkali and rear directly pass through pretreated macroporous adsorbent resin, first use the distilled water flushing of equivalent, use again 5 ~ 8% ammoniacal liquor ethanolic soln wash-out to adsorb saturated resin column, till flowing out elutriant lifeless matter alkali reaction, collect elutriant;
D. elutriant is evaporated to 1/5 o'clock of original volume, lets cool crystallization, filters, and 80% ethyl alcohol recrystallization 2 times, obtains yellow leaf reed alkali needle.
Pretreatment process described in step c is that resin first spends the night by 80% alcohol immersion, is washed till without alcohol taste with distilled water, uses 5% HCl instead and soaks 1h, and distilled water is washed till neutrality, and then uses 5% sodium hydroxide solution instead and soak 1h, and distilled water is washed till neutrality, for subsequent use.
Macroporous adsorbent resin type described in step c is D-101, D-72, AB-8 etc.
Alkali described in step c is the mineral alkalis such as sodium hydroxide, potassium hydroxide, sodium carbonate.
The present invention utilizes ultrasonic wave to make medicinal material in solvent, pass through the generation of vibration cavatition of certain frequency, destroy the cell of vegetable drug, make solvent be easy to infiltrate in cell, shorten widely the time that solvent enters cell interior, release, diffusion and the dissolving of intracellular organic matter are strengthened, can realize continuous operation, improve production efficiency, be applicable to suitability for industrialized production simultaneously.
Further illustrate the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment.
embodiment:
Embodiment 1:
One leaf reed branch, leaf is through natural drying, in 80 DEG C of drying in oven, pulverized 60 mesh sieves, get leaf reed meal 100g, add 2% the aqueous sulfuric acid of 5 times, be placed in continuous countercurrent ultrasonic extraction device, in 60 DEG C, under 70KHz, extract 2h, centrifugal, get supernatant liquor, in sodium hydroxide and rear directly pass through pretreated AB-8 macroporous adsorbent resin, first use the distilled water flushing of equivalent, adsorb saturated resin column with 8% ammoniacal liquor ethanolic soln wash-out again, till flowing out elutriant lifeless matter alkali reaction, collect elutriant, elutriant is evaporated to 1/5 o'clock of original volume, let cool crystallization, filter, 80% ethyl alcohol recrystallization 2 times, obtain yellow leaf reed alkali needle 0.49g, be 93.2% through its purity of determination of acid-basetitration.
Embodiment 2:
One leaf reed branch, leaf is through natural drying, in 80 DEG C of drying in oven, pulverized 60 mesh sieves, get leaf reed meal 100g, add 1% the aqueous sulfuric acid of 7 times, be placed in continuous countercurrent ultrasonic extraction device, in 55 DEG C, under 60KHz, extract 2.5h, centrifugal, get supernatant liquor, in sodium carbonate and rear directly pass through pretreated D-72 macroporous adsorbent resin, first use the distilled water flushing of equivalent, adsorb saturated resin column with 6% ammoniacal liquor ethanolic soln wash-out again, till flowing out elutriant lifeless matter alkali reaction, collect elutriant, elutriant is evaporated to 1/5 o'clock of original volume, let cool crystallization, filter, 80% ethyl alcohol recrystallization 2 times, obtain yellow leaf reed alkali needle 0.58g, be 94.4% through its purity of determination of acid-basetitration.
Embodiment 3:
One leaf reed branch, leaf is through natural drying, in 80 DEG C of drying in oven, pulverized 60 mesh sieves, get leaf reed meal 100g, add 0.5% the aqueous sulfuric acid of 6 times, be placed in continuous countercurrent ultrasonic extraction device, in 50 DEG C, under 50KHz, extract 3h, centrifugal, get supernatant liquor, in potassium hydroxide and rear directly pass through pretreated D-101 macroporous adsorbent resin, first use the distilled water flushing of equivalent, adsorb saturated resin column with 5% ammoniacal liquor ethanolic soln wash-out again, till flowing out elutriant lifeless matter alkali reaction, collect elutriant, elutriant is evaporated to 1/5 o'clock of original volume, let cool crystallization, filter, 80% ethyl alcohol recrystallization 2 times, obtain yellow leaf reed alkali needle 0.54g, be 93.9% through its purity of determination of acid-basetitration.
Claims (4)
1. a method of extracting leaf reed alkali from a leaf reed, is characterized in that, comprises the following steps:
A. leaf reed branch, leaf, through natural drying, in 80 DEG C of drying in oven, were pulverized 60 mesh sieves;
B. get leaf reed meal, add 0.5 ~ 2% the aqueous sulfuric acid of 5 ~ 7 times, be placed in continuous countercurrent ultrasonic extraction device, under 60 ~ 70 DEG C, 50 ~ 70KHz, extract 2 ~ 3h;
C. by centrifugal above-mentioned extracting solution, get supernatant liquor, in alkali and rear directly pass through pretreated macroporous adsorbent resin, first use the distilled water flushing of equivalent, use again 5 ~ 8% ammoniacal liquor ethanolic soln wash-out to adsorb saturated resin column, till flowing out elutriant lifeless matter alkali reaction, collect elutriant;
D. elutriant is evaporated to 1/5 o'clock of original volume, lets cool crystallization, filters, and 80% ethyl alcohol recrystallization 2 times, obtains yellow leaf reed alkali needle.
2. a kind of method of extracting leaf reed alkali from a leaf reed according to claim 1, it is characterized in that, pretreatment process described in step c is that resin first spends the night by 80% alcohol immersion, be washed till without alcohol taste with distilled water, use 5% HCl immersion 1h instead, distilled water is washed till neutrality, and then uses 5% sodium hydroxide solution immersion 1h instead, distilled water is washed till neutrality, for subsequent use.
3. a kind of method of extracting leaf reed alkali from a leaf reed according to claim 1, is characterized in that, the macroporous adsorbent resin type described in step c is D-101, D-72, AB-8 etc.
4. a kind of method of extracting leaf reed alkali from a leaf reed according to claim 1, is characterized in that, the alkali described in step c is the mineral alkalis such as sodium hydroxide, potassium hydroxide, sodium carbonate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410446369.5A CN104193756A (en) | 2014-09-04 | 2014-09-04 | Method for extracting securinine from securinega |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410446369.5A CN104193756A (en) | 2014-09-04 | 2014-09-04 | Method for extracting securinine from securinega |
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| Publication Number | Publication Date |
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| CN104193756A true CN104193756A (en) | 2014-12-10 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410446369.5A Pending CN104193756A (en) | 2014-09-04 | 2014-09-04 | Method for extracting securinine from securinega |
Country Status (1)
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| CN (1) | CN104193756A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105832742A (en) * | 2016-04-28 | 2016-08-10 | 南京赋海澳赛医药科技有限公司 | Application of composition of Virosaine A pyrrolidine derivative and morpholinyl derivative to medicine for increasing leucocyte |
| CN105853435A (en) * | 2016-04-28 | 2016-08-17 | 南京赋海澳赛医药科技有限公司 | Application of composition of pyrrolidine derivative and morpholinyl derivative of Virosaine A to anti-inflammatory medicine |
| CN105920014A (en) * | 2016-04-28 | 2016-09-07 | 南京赋海澳赛医药科技有限公司 | Application of composition of tetrahydropyrrolyl and morpholinyl derivatives of Virosaine A in antibacterial medicines |
-
2014
- 2014-09-04 CN CN201410446369.5A patent/CN104193756A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105832742A (en) * | 2016-04-28 | 2016-08-10 | 南京赋海澳赛医药科技有限公司 | Application of composition of Virosaine A pyrrolidine derivative and morpholinyl derivative to medicine for increasing leucocyte |
| CN105853435A (en) * | 2016-04-28 | 2016-08-17 | 南京赋海澳赛医药科技有限公司 | Application of composition of pyrrolidine derivative and morpholinyl derivative of Virosaine A to anti-inflammatory medicine |
| CN105920014A (en) * | 2016-04-28 | 2016-09-07 | 南京赋海澳赛医药科技有限公司 | Application of composition of tetrahydropyrrolyl and morpholinyl derivatives of Virosaine A in antibacterial medicines |
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| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20141210 |