CN104193754A - New method for extracting tetrandrine from radix stephaniae tetrandrae - Google Patents
New method for extracting tetrandrine from radix stephaniae tetrandrae Download PDFInfo
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- CN104193754A CN104193754A CN201410445767.5A CN201410445767A CN104193754A CN 104193754 A CN104193754 A CN 104193754A CN 201410445767 A CN201410445767 A CN 201410445767A CN 104193754 A CN104193754 A CN 104193754A
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- radix stephaniae
- stephaniae tetrandrae
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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
- C07D491/18—Bridged systems
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Abstract
The invention relates to a new method for extracting tetrandrine from radix stephaniae tetrandrae. The new method comprises the following processing steps: a, crushing the medicinal material radix stephaniae tetrandrae and sieving by use of a 100-mesh sieve; b, performing ultrasonic-microwave assisted extraction in an acidic solution; c, separating by use of a macroporous adsorption resin; and d, precipitating by use of lime milk, and repeatedly crystalizing twice to obtain the tetrandrine. The new method for extracting the tetrandrine from the radix stephaniae tetrandrae is used for extracting the tetrandrine by use of a modern extraction technology namely an ultrasonic-microwave combined extraction technology, and has the advantages of simple process, short extraction time, high selectivity and no harm to the environment.
Description
Technical field
The present invention relates to a kind of from Radix stephaniae tetrandrae the novel method of extract powder sinomenine, relate in particular to a kind of method of utilizing biological enzyme synergistic supersonic wave extract powder sinomenine.
Background technology
Radix stephaniae tetrandrae also claims Radix Stephaniae Tetrandrae, is the dry root of menispermaceous plants Radix stephaniae tetrandrae, has the effect of inducing diuresis to remove edema, wind-expelling pain-stopping, and modern pharmacology is tested and shown, Radix stephaniae tetrandrae total alkaloids has analgesia, step-down, myorelaxant effects.In Radix stephaniae tetrandrae, alkaloid is higher, generally can reach 1.5 ~ 2.0%, is mainly wherein Tetrrine, is secondly Fangchinoline.Both molecular structures have the nitrogen-atoms of two tertiary amine states, and alkalescence is stronger, all have the general solvability of Fat-soluble alkaloids.But substituting group there are differences in their molecular structure, Tetrrine is methoxyl group, and Fangchinoline is phenolic hydroxyl group, so the polarity of Tetrrine is less, can be dissolved in cold benzene, and Fangchinoline polarity is larger, is insoluble in cold benzene.
Patent and the document of the current extraction about Tetrrine are more, mainly use alcohol extraction and acid precipitation method, supercritical fluid extraction, or sour water percolation process etc., all there is many deficiencies.As an outstanding person has reported the alcohol reflux Radix stephaniae tetrandrae total alkaloids with 85%,, alkalization heavy through acid and chloroform extraction again, with acetone refining, obtain Tetrrine afterwards, the shortcoming of the method is to use toxicity chloroform large, that volatility is large to make solvent, all larger on the impact of operator's health and environment; Huang Liping has reported use supercritical fluid extraction Tetrrine, and its weak point is that equipment cost is high, is unwell to suitability for industrialized production; The industrial sour water percolation processs that adopt at present extract more, milk of lime precipitation, then soak and extract through cold benzene, acetone refining obtains Tetrrine, and its weak point is complex operation, extraction yield is low, waste liquid amount is large.
Summary of the invention
The object of the invention is for the deficiencies in the prior art, provide that a kind of technique is simple, easy to operate, the novel method of extract powder sinomenine fast and efficiently.
The present invention includes following steps:
A. Radix stephaniae tetrandrae pulverizing medicinal materials, crosses 100 mesh sieves;
B. get Radix stephaniae tetrandrae meal, the acidic aqueous solution that the pH value that adds 5 ~ 7 times is 3.5 ~ 4.5, is placed in ultrasonic-microwave extraction device, and ultrasonic wave 500W(often opens), microwave power is 400 ~ 500W, extraction time is 60 ~ 90min;
C. above-mentioned extracting solution is centrifugal, get supernatant liquor, directly by pretreated large hole cation exchanger resin D72, adsorb, first use the distilled water flushing of equivalent, use again the ammoniacal liquor ethanolic soln wash-out of 0.4 ~ 0.5mol to adsorb saturated resin column, flow velocity is 10mL/min, till flowing out elutriant lifeless matter alkali reaction;
D. concentrate eluant, uses acetone solution, and recrystallization is 2 times repeatedly, obtains highly purified white Tetrrine.
The acid of adjusting PH described in step b is sulfuric acid or hydrochloric acid etc.
Pretreatment process described in step c is with 95% alcohol immersion 24h, then is washed till without alcohol taste with distilled water, uses 5% HCl immersion 2h instead, and distilled water is washed till neutrality, standby.
The present invention utilizes hyperacoustic cavatition, the cell that destroys vegetable drug, makes solvent be easy to infiltrate in cell, and hyperacoustic judder simultaneously can be transmitted huge energy to medicinal material and the solvent of lixiviate, make them do high-speed motion, strengthened release, diffusion and the dissolving of intracellular organic matter; In conjunction with the high energy effect of microwave, the effect that the each point in sample media is subject to is consistent again, accelerates target compound and from solid phase, enters the process of solvent.Compare with traditional extracting method, the method has high efficiency and strong selectivity, simple to operate, and productive rate is high, and product is easy to the advantages such as purifying.
Below in conjunction with embodiment, further illustrate the present invention, but the scope of protection of present invention is not limited to following embodiment.
embodiment:
Embodiment 1:
Radix stephaniae tetrandrae pulverizing medicinal materials, cross 100 mesh sieves, get meal 500g, the aqueous hydrochloric acid that the pH value that adds 5 times is 3.5, be placed in ultrasonic-microwave extraction device, ultrasonic wave 500W(often opens), microwave power is 400W, extraction time is 90min, extracting solution is centrifugal, get supernatant liquor, directly by pretreated large hole cation exchanger resin D72, adsorb, first use the distilled water flushing of equivalent, with the ammoniacal liquor ethanolic soln wash-out of 0.4mol/L, adsorb saturated resin column again, flow velocity is 10mL/min, till flowing out elutriant lifeless matter alkali reaction, concentrate eluant, with acetone solution, recrystallization is 2 times repeatedly, obtain highly purified white Tetrrine 3.89g, through HPLC, recording purity is 95.4%.
Embodiment 2:
Radix stephaniae tetrandrae pulverizing medicinal materials, cross 100 mesh sieves, get meal 500g, the aqueous sulfuric acid that the pH value that adds 7 times is 4.0, be placed in ultrasonic-microwave extraction device, ultrasonic wave 500W(often opens), microwave power is 500W, extraction time is 70min, extracting solution is centrifugal, get supernatant liquor, directly by pretreated large hole cation exchanger resin D72, adsorb, first use the distilled water flushing of equivalent, with the ammoniacal liquor ethanolic soln wash-out of 0.6mol/L, adsorb saturated resin column again, flow velocity is 10mL/min, till flowing out elutriant lifeless matter alkali reaction, concentrate eluant, with acetone solution, recrystallization is 2 times repeatedly, obtain highly purified white Tetrrine 4.15g, through HPLC, recording purity is 98.1%.
Embodiment 3:
Radix stephaniae tetrandrae pulverizing medicinal materials, cross 100 mesh sieves, get meal 500g, the aqueous sulfuric acid that the pH value that adds 6 times is 4.5, be placed in ultrasonic-microwave extraction device, ultrasonic wave 500W(often opens), microwave power is 450W, extraction time is 60min, extracting solution is centrifugal, get supernatant liquor, directly by pretreated large hole cation exchanger resin D72, adsorb, first use the distilled water flushing of equivalent, with the ammoniacal liquor ethanolic soln wash-out of 0.5mol/L, adsorb saturated resin column again, flow velocity is 10mL/min, till flowing out elutriant lifeless matter alkali reaction, concentrate eluant, with acetone solution, recrystallization is 2 times repeatedly, obtain highly purified white Tetrrine 3.98g, through HPLC, recording purity is 96.3%.
Claims (3)
1. a novel method for extract powder sinomenine from Radix stephaniae tetrandrae, is characterized in that, comprises the following steps:
A. Radix stephaniae tetrandrae pulverizing medicinal materials, crosses 100 mesh sieves;
B. get Radix stephaniae tetrandrae meal, the acidic aqueous solution that the pH value that adds 5 ~ 7 times is 3.5 ~ 4.5, is placed in ultrasonic-microwave extraction device, and ultrasonic wave 500W(often opens), microwave power is 400 ~ 500W, extraction time is 60 ~ 90min;
C. above-mentioned extracting solution is centrifugal, get supernatant liquor, directly by pretreated large hole cation exchanger resin D72, adsorb, first use the distilled water flushing of equivalent, use again the ammoniacal liquor ethanolic soln wash-out of 0.4 ~ 0.5mol/L to adsorb saturated resin column, flow velocity is 10mL/min, till flowing out elutriant lifeless matter alkali reaction;
D. concentrate eluant, uses acetone solution, and recrystallization is 2 times repeatedly, obtains highly purified white Tetrrine.
According to claim 1 a kind of from Radix stephaniae tetrandrae the novel method of extract powder sinomenine, it is characterized in that, the acid of the adjusting PH described in step b is sulfuric acid or hydrochloric acid etc.
According to claim 1 a kind of from Radix stephaniae tetrandrae the novel method of extract powder sinomenine, it is characterized in that, the pretreatment process described in step c is for 95% alcohol immersion 24h, with distilled water, be washed till without alcohol taste again, use 5% HCl immersion 2h instead, distilled water is washed till neutrality, standby.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201410445767.5A CN104193754A (en) | 2014-09-04 | 2014-09-04 | New method for extracting tetrandrine from radix stephaniae tetrandrae |
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| CN201410445767.5A CN104193754A (en) | 2014-09-04 | 2014-09-04 | New method for extracting tetrandrine from radix stephaniae tetrandrae |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105541857A (en) * | 2016-01-18 | 2016-05-04 | 北京七巧时代科技有限公司 | Tetrandrine extract as well as preparation method and application thereof |
| CN105640831A (en) * | 2016-01-18 | 2016-06-08 | 北京七巧时代科技有限公司 | Multi-effect plant cleanser |
| CN110179799A (en) * | 2019-06-20 | 2019-08-30 | 中国人民解放军军事科学院军事医学研究院 | The application of tetrandrine and the extracting method of tetrandrine |
| CN113367242A (en) * | 2021-06-10 | 2021-09-10 | 中国农业科学院草原研究所 | Method for extracting alkaloid from nettle and application of alkaloid as growth promoting additive |
| CN114558050A (en) * | 2022-03-21 | 2022-05-31 | 上海浙星新型材料科技有限公司 | Preparation method of traditional Chinese medicine stephania tetrandra extract |
-
2014
- 2014-09-04 CN CN201410445767.5A patent/CN104193754A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105541857A (en) * | 2016-01-18 | 2016-05-04 | 北京七巧时代科技有限公司 | Tetrandrine extract as well as preparation method and application thereof |
| CN105640831A (en) * | 2016-01-18 | 2016-06-08 | 北京七巧时代科技有限公司 | Multi-effect plant cleanser |
| CN110179799A (en) * | 2019-06-20 | 2019-08-30 | 中国人民解放军军事科学院军事医学研究院 | The application of tetrandrine and the extracting method of tetrandrine |
| CN113367242A (en) * | 2021-06-10 | 2021-09-10 | 中国农业科学院草原研究所 | Method for extracting alkaloid from nettle and application of alkaloid as growth promoting additive |
| CN114558050A (en) * | 2022-03-21 | 2022-05-31 | 上海浙星新型材料科技有限公司 | Preparation method of traditional Chinese medicine stephania tetrandra extract |
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Application publication date: 20141210 |