CN102863381A - Novel method for extracting huperzine A from huperzia serrata - Google Patents
Novel method for extracting huperzine A from huperzia serrata Download PDFInfo
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Abstract
The invention relates to a novel method for extracting huperzine A from Huperziaserrataf.longipetiolata (Spring) Ching, and relates to the technical field of medicines. The novel method comprises the technical scheme as follows: (1) preparing extracting liquid; (2) purifying the extracting liquid; (3) preparing the total alkaloid of huperzia serrata; (4) preparing a rough product of huperzine A; and (5) preparing high-purity huperzine A, thus obtaining the white solid huperzine A with the purity of 98% to 99%. The novel method of extracting the huperzine A provided by the invention has the advantages that: (1) the new resource huperzia serrata is served as the raw material; and the single source of the medicine and technology method for extracting huperzine A from huperziaserrataf.longipetiolata (Spring) Ching are expanded; (2) 20% to 60% of ethanol water is adopted for extracting, therefore, little damage is brought to instruments and equipment, and low toxic and side effects are generated; and (3) the huperzine A is enriched through a reverse phase (Middle Pressure Liquid Chromatography) is adopted, thus, the cost is low, the purity is high, the yield is high, and the mass industrial production can be easily carried out.
Description
Technical field
The present invention relates to medical technical field, the long handle stone China fir that specifically produce in six areas take Guizhou Province is separated to the preparation method of alkaloid selagine first as raw material.Selagine easily sees through hemato encephalic barrier, and (AchE) has potent restraining effect to acetylcholinesterase in the brain, obviously improves levels of acetylcholine in the brain, promotes study, Memory Process or obviously improves amnemonic effect.
Background technology
Long handle stone China fir
Huperzia serrata f.longipetiolata (Spring) mutation of Ching through-stone Taxodiaceae stone araucaria pteridophyte Herba Lycopodii serrati.Be distributed under hillside, river valley, small stream limit, sylvan life, border or the shrubbery of the ground height above sea level 300-1900 rice such as Guizhou, Southwestern China area, Sichuan, Chongqing, Yunnan.Tool dissipating blood stasis for subsidence of swelling, hemostasia and promoting granulation, heat-clearing toxin-expelling functions, among the people for delousing, bed bug eradication and treatment snakebite etc.[" Guizhou Ferns Medicinal ". [M]. Kweiyang, Guizhou: Guizhou science and technology press, 2012,32.].
Selagine (Huperzine A) claims again Fuding alkali, for China scientist separates the lycopodium alkaloid that obtains from traditional herbal medicine " Herba Lycopodii serrati " [Herba Lycopodii serrati, Huperzia serrata(Thunb.ex Murray) Trev].
This compound is a kind of potent, highly selective and has reversible acetylcholinesterase depressant that the symptoms such as presenile dementia, pure dysmnesia and myasthenia gravis are had significant curative effect, now has been widely used in clinical.At present, although selagine can obtain by the method for chemosynthesis, its efficient is low, toxicity is large, cost is high.Therefore, selagine still mainly obtains from natural resources.
Selagine (Huperzine A): amino-11 ethylidene-5,8,9 of chemistry (5R, 9R, 11E)-5-by name, 10-tetrahydrochysene-7-methyl-5,9 methylene radical cycloocta [
b] pyridine-2 (1H)-ketone, molecular formula is C
15H
18N
2O, its chemical structural formula is:
Long handle stone China fir is at the southwest aboundresources, and it is wide to distribute, and with Herba Lycopodii serrati be congener, through preliminary study, find that the content of its selagine is close.Denudated in the situation of also havoc ecological resources by coyoting at existing medicine source Herba Lycopodii serrati, exploring the preparation method who extracts separating huperzine A from long handle stone China fir has far-reaching Social benefit and economic benefit undoubtedly.
In the prior art, the extraction of selagine is mainly by acid extraction, further by macroporous resin or normal phase silicagel column enrichment selagine.Serious to the plant and instrument infringement in its production process, the production cycle is long, and production cost is high, and product purity is low, and yield is low, is confined to laboratory applications more, is difficult to carry out large-scale production.Medium pressure liquid chromatography (reverse phase silica gel RP-C
18) method [MPLC (RP-18) method] be a kind of pump system pressure that utilizes up to monobasic or polynary combination degree of grade or the gradient elution of 50 bar/725 psi, thereby reach the separation purification method of sharp separation purpose.The method has overcome the shortcoming of prior art, and industrialization degree is high, and is simple, convenient, easily row.
Summary of the invention
The objective of the invention is for serious to the plant and instrument infringement in the background technology, the production cycle is long, a kind of novel method of extracting selagine from new resources long handle stone China fir (mutation of Herba Lycopodii serrati) of the problems such as production cost height development.
A kind of novel method of extracting selagine from long handle stone China fir of the present invention follows these steps to preparation successively:
(1) preparation of extracting solution:
After the long handle stone China fir sample pulverizing with seasoning, with ethanol water heating and refluxing extraction, repeat to extract for several times, collect extracting solution;
(2) purification of extracting solution:
With extracting solution concentrating under reduced pressure Recycled ethanol, concentrated solution is transferred pH to 2-3 with the HCl aqueous solution, extracts for several times with ethyl acetate, removes impurity; The organic phase ethyl acetate discards or reclaims, and sour water is the purification extracting solution mutually;
(3) preparation of long handle stone China fir total alkaloids:
To purify extracting solution and transfer pH to 9-10 with ammoniacal liquor, with chloroform extraction for several times, the combined chloroform extraction liquid, underpressure distillation is removed chloroform and is got long handle stone China fir total alkaloids;
(4) preparation of selagine crude product:
With long handle stone China fir total alkaloids MPLC (RP-18) method, carry out wash-out take methanol-water as solvent systems, wash with water first, remove water soluble component, use again the methanol-water wash-out of 5-30%v/v, contain the component of selagine by the HPLC combining data detection, concentrated, vacuum-drying gets faint yellow solid, is the selagine crude product;
(5) preparation of high-purity huperzine A:
Add proper amount of acetone or ethanol in above-mentioned selagine crude product, heating makes its dissolving and filtered while hot, and filtrate is crystallization under room temperature, so repeatedly recrystallization for several times, making selagine purity is 98-99%.
Each process condition of the present invention is:
(1) preparation of extracting solution:
The long handle stone China fir sample of seasoning is crushed to the 20-80 order, adds doubly heavy 20-60% v/v ethanol water of 10-20,75 ℃ heating and refluxing extraction 3-5 hour, repeat to extract 3-4 time, the collection extracting solution is for subsequent use;
(2) purification of extracting solution:
Extracting solution is evaporated to the 8-15% of original volume, and concentrated solution is transferred pH to 2-3 with the HCl aqueous solution of 5 ‰ v/v, with equal-volume ethyl acetate extraction 3-4 time, removes impurity; The organic phase ethyl acetate discards or reclaims, and sour water is the purification extracting solution mutually;
(3) preparation of long handle stone China fir total alkaloids:
To purify extracting solution and transfer pH to 9-10 with the ammoniacal liquor of 1:1 (v/v), with isopyknic chloroform extraction 4-5 time, combined chloroform extraction liquid, underpressure distillation is removed chloroform and is got long handle stone China fir total alkaloids;
(4) preparation of selagine crude product:
With long handle stone China fir total alkaloids MPLC (RP-18) method, carry out wash-out take methanol-water as solvent systems, wash with water first, remove water soluble component, use again the methanol-water wash-out of 5-30% v/v, contain the component of selagine by the HPLC combining data detection, the methanol-water elutriant is concentrated, vacuum-drying gets faint yellow solid, is the selagine crude product;
(5) preparation of high-purity huperzine A:
Add proper amount of acetone or ethanol in above-mentioned selagine crude product, heating makes its dissolving and filtered while hot, and filtrate is crystallization under room temperature, and recrystallization is 2-3 time so repeatedly, and making selagine purity is 98-99%.
Each step preferred processing condition of the present invention is:
(1) preparation of extracting solution:
The long handle stone China fir sample of seasoning is crushed to 40 orders, adds 20 times heavy 20% v/v ethanol water, extract 3 times in 75 ℃ of heating in water bath refluxing extraction, the 1st time 5 hours, the 2nd time 4 hours, the 3rd time 4 hours, merge No. 3 times extracting solution;
(2) purification of extracting solution:
Said extracted liquid is evaporated to 10% of original volume under 50 ℃, concentrated solution is transferred pH to 2-3 with the HCl aqueous solution of 5 ‰ v/v, uses equal-volume ethyl acetate extraction 3 times, removes impurity; The organic phase ethyl acetate discards or reclaims, and sour water is the purification extracting solution mutually;
(3) preparation of long handle stone China fir total alkaloids:
To purify extracting solution and transfer pH to 9-10 with the ammoniacal liquor of 1:1 (v/v), with isopyknic chloroform extraction 4 times, combined chloroform extraction liquid, underpressure distillation is removed chloroform and is got long handle stone China fir total alkaloids;
(4) preparation of selagine crude product:
With long handle stone China fir total alkaloids MPLC (RP-18) method, carry out wash-out take methanol-water as solvent systems, wash with water first, remove water soluble component, use again the methanol-water wash-out of 5-30% v/v, contain the component of selagine by the HPLC combining data detection, the methanol-water elutriant is concentrated, vacuum-drying gets faint yellow solid, is the selagine crude product;
(5) preparation of high-purity huperzine A:
Add proper amount of acetone or ethanol in above-mentioned selagine crude product, heating makes its dissolving and filtered while hot, and filtrate is crystallization under room temperature, and recrystallization is 3 times so repeatedly, and making selagine purity is 98-99%.
Step of the present invention (3)-(5) agents useful for same is analytical pure AR, and water is distilled water.
MPLC(RP-18 of the present invention) the used middle compression leg of method is that the sharp fringe of Law Firm Suzhou Jiangsu scientific ﹠ technical corporation produces numbering: S-1101-3000; The post specification: internal diameter * highly * and volume=156 * 410 * 7800, the mm of unit.
The used solvent of step of the present invention (5) recrystallization is preferably acetone.
Adopt above-mentioned technology to extract the advantage of selagine: (1) adopts the 20%-60% ethanol-water extraction, and little to the plant and instrument infringement, toxic side effect is low; (2) by anti-phase MPLC method enrichment selagine, cost is low, efficient is high, yield is high, is easy to large-scale industrial production.
Description of drawings
Fig. 1 is preparation technology's schematic flow sheet of selagine, description of drawings the preparation process of selagine be: the preparation of (1) extracting solution; (2) purification of extracting solution; (3) preparation of long handle stone China fir total alkaloids; (4) preparation of selagine crude product; (5) preparation of high-purity huperzine A.
Fig. 2 is the selagine nucleus magnetic resonance
1The H-NMR spectrogram illustrates hydrogen (CH in the selagine
3,-CH
2The ownership of ,-CH).
Fig. 3 is the selagine nucleus magnetic resonance
13C-NMR and DEPT spectrogram illustrate type (primary, secondary, uncle and quaternary carbon) and the ownership of carbon in the selagine.
Fig. 4 is the selagine mass spectrum, and molecular weight and the fragmentation pattern of selagine is described.
Fig. 5 is selagine standard substance HPLC collection of illustrative plates.
Fig. 6 is selagine sample HPLC collection of illustrative plates.Illustrate that the selagine sample is consistent with standard substance HPLC collection of illustrative plates.
Embodiment
The present invention is further elaborated below in conjunction with embodiment.The following embodiment of mandatory declaration is for explanation the present invention rather than limitation of the present invention.Essence according to the present invention all belongs to the scope of protection of present invention to the simple modifications that the present invention carries out.
Proton nmr spectra
1H-NMR, carbon-13 nmr spectra
13C-NMR measures (tetramethylsilane ether TMS is interior mark) by INOVA 400MHZ NMR spectrometer with superconducting magnet (VARIAN Oncology Systems); Agilent 1100 high performance liquid chromatography (U.S. Agilent Science and Technology Ltd.); Hydraulic fluid phase (MPLC) chromatogram (Switzerland Buchi company limited) among the Buchi; Middle compression leg (numbering: be that Jiangsu sharp fringe (Suzhou) scientific ﹠ technical corporation produces S-1101-3000); Step (3)-(5) reagent is analytical pure AR, and water is distilled water.
Embodiment 1
(1). get the long handle stone China fir medicinal material 10Kg that crushes and put into extractor, 20% the ethanol water that adds 20 times of amounts 5 hours for the first time, 4 hours for the second time, 4 hours for the third time, merges 3 times extracting solution in 75 ℃ of lower refluxing extraction 3 times;
(2). said extracted liquid is evaporated to 10% of original volume under 50 ℃, concentrated solution is transferred pH to 2-3 with 5 ‰ HCl, uses and the isopyknic ethyl acetate extraction of concentrated solution 3 times, and ethyl acetate discards, and the sour water layer is for subsequent use;
(3). the sour water layer is transferred pH to 9-10 with the ammoniacal liquor of 1:1 (v/v), uses and the isopyknic chloroform extraction of concentrated solution 4 times, and combined chloroform extraction liquid and concentrating under reduced pressure get total alkaloids;
(4). total alkaloids MPLC (RP-18) method, carry out wash-out take methanol-water as solvent systems, wash with water first and remove water soluble component, use again the methanol-water wash-out of 5-30%, contain the component of selagine by the HPLC combining data detection, concentrated vacuum-drying gets faint yellow solid;
(5). add proper amount of acetone in above-mentioned faint yellow solid, heating makes its dissolving and filtered while hot, and filtrate is crystallization under room temperature, obtains off-white color solid purity 90%, according to identical method repeatedly recrystallization 2 times white solid, purity〉98%, 1.9g altogether.
Embodiment 2
(1). get the long handle stone China fir medicinal material 30Kg that crushes and put into extractor, 40% the ethanol water that adds 15 times of amounts 5 hours for the first time, 4 hours for the second time, 4 hours for the third time, the 4th time 3 hours, merges 4 times extracting solution in 75 ℃ of lower refluxing extraction 4 times;
(2). said extracted liquid is evaporated to 10% of original volume under 50 ℃, concentrated solution is transferred pH to 2-3 with 5 ‰ HCl, uses and the isopyknic ethyl acetate extraction of concentrated solution 4 times, and ethyl acetate discards, and the sour water layer is for subsequent use;
(3). the sour water layer is transferred pH to 9-10 with ammoniacal liquor, uses and the isopyknic chloroform extraction of concentrated solution 4 times, and combined chloroform extraction liquid and concentrating under reduced pressure get total alkaloids;
(4). total alkaloids MPLC (RP-18) method, carry out wash-out take methanol-water as solvent systems, wash with water first and remove water soluble component, use again the methanol-water wash-out of 5-30%, contain the component of selagine by the HPLC combining data detection, concentrated vacuum-drying gets faint yellow solid;
(5). add an amount of ethanol in above-mentioned faint yellow solid, heating makes its dissolving and filtered while hot, and filtrate is crystallization under room temperature, obtains off-white color solid purity 90%, according to identical method repeatedly recrystallization 2 times white solid, purity〉98%, 5.4g altogether.
Embodiment 3
(1). get the long handle stone China fir medicinal material 50Kg that crushes and put into extractor, 60% the ethanol water that adds 10 times of amounts 5 hours for the first time, 4 hours for the second time, 4 hours for the third time, merges 3 times extracting solution in 75 ℃ of lower refluxing extraction 3 times;
(2). said extracted liquid is evaporated to 10% of original volume under 50 ℃, concentrated solution is transferred pH to 2-3 with 5 ‰ HCl, uses and the isopyknic ethyl acetate extraction of concentrated solution 4 times, and ethyl acetate discards, and the sour water layer is for subsequent use;
(3) the sour water layer is transferred pH to 9-10 with ammoniacal liquor, uses and the isopyknic chloroform extraction of concentrated solution 5 times, and combined chloroform extraction liquid and concentrating under reduced pressure get total alkaloids;
(4). total alkaloids MPLC (RP-18) method, carry out wash-out take methanol-water as solvent systems, wash with water first and remove water soluble component, use again the methanol-water wash-out of 5-30%, contain the component of selagine by the HPLC combining data detection, concentrated vacuum-drying gets faint yellow solid;
(5). add an amount of ethanol in above-mentioned faint yellow solid, heating makes its dissolving and filtered while hot, and filtrate is crystallization under room temperature, obtains off-white color solid purity 90%, according to identical method repeatedly recrystallization 3 times white solid, purity〉98%, 8.4g altogether.
Claims (6)
1. novel method of extracting selagine from long handle stone China fir is characterized in that following these steps to successively preparation:
(1) preparation of extracting solution:
After the long handle stone China fir sample pulverizing with seasoning, with ethanol water heating and refluxing extraction, repeat to extract for several times, collect extracting solution;
(2) purification of extracting solution:
With extracting solution concentrating under reduced pressure Recycled ethanol, concentrated solution is transferred pH to 2-3 with the HCl aqueous solution, extracts for several times with ethyl acetate, removes impurity; The organic phase ethyl acetate discards or reclaims, and sour water is the purification extracting solution mutually;
(3) preparation of long handle stone China fir total alkaloids:
To purify extracting solution and transfer pH to 9-10 with ammoniacal liquor, with chloroform extraction for several times, the combined chloroform extraction liquid, underpressure distillation is removed chloroform and is got long handle stone China fir total alkaloids;
(4) preparation of selagine crude product:
With long handle stone China fir total alkaloids MPLC (RP-18) method, carry out wash-out take methanol-water as solvent systems, wash with water first, remove water soluble component, use again the methanol-water wash-out of 5-30%v/v, contain the component of selagine by the HPLC combining data detection, concentrated, vacuum-drying gets faint yellow solid, is the selagine crude product;
(5) preparation of high-purity huperzine A:
Add proper amount of acetone or ethanol in above-mentioned selagine crude product, heating makes its dissolving and filtered while hot, and filtrate is crystallization under room temperature, so repeatedly recrystallization for several times, making selagine purity is 98-99%.
2. a kind of novel method of extracting selagine from long handle stone China fir according to claim 1 is characterized in that each process condition is:
(1) preparation of extracting solution:
The long handle stone China fir sample of seasoning is crushed to the 20-80 order, adds doubly heavy 20-60% v/v ethanol water of 10-20,75 ℃ heating and refluxing extraction 3-5 hour, repeat to extract 3-4 time, the collection extracting solution is for subsequent use;
(2) purification of extracting solution:
Extracting solution is evaporated to the 8-15% of original volume, and concentrated solution is transferred pH to 2-3 with the HCl aqueous solution of 5 ‰ v/v, with equal-volume ethyl acetate extraction 3-4 time, removes impurity; The organic phase ethyl acetate discards or reclaims, and sour water is the purification extracting solution mutually;
(3) preparation of long handle stone China fir total alkaloids:
To purify extracting solution and transfer pH to 9-10 with the ammoniacal liquor of 1:1 (v/v), with isopyknic chloroform extraction 4-5 time, combined chloroform extraction liquid, underpressure distillation is removed chloroform and is got long handle stone China fir total alkaloids;
(4) preparation of selagine crude product:
With long handle stone China fir total alkaloids MPLC (RP-18) method, carry out wash-out take methanol-water as solvent systems, wash with water first, remove water soluble component, use again the methanol-water wash-out of 5-30% v/v, contain the component of selagine by the HPLC combining data detection, the methanol-water elutriant is concentrated, vacuum-drying gets faint yellow solid, is the selagine crude product;
(5) preparation of high-purity huperzine A:
Add proper amount of acetone or ethanol in above-mentioned selagine crude product, heating makes its dissolving and filtered while hot, and filtrate is crystallization under room temperature, and recrystallization is 2-3 time so repeatedly, and making selagine purity is 98-99%.
3. a kind of novel method of extracting selagine from long handle stone China fir according to claim 2 is characterized in that each process condition is:
(1) preparation of extracting solution:
The long handle stone China fir sample of seasoning is crushed to 40 orders, adds 20 times heavy 20% v/v ethanol water, extract 3 times in 75 ℃ of heating in water bath refluxing extraction, the 1st time 5 hours, the 2nd time 4 hours, the 3rd time 4 hours, merge No. 3 times extracting solution;
(2) purification of extracting solution:
Said extracted liquid is evaporated to 10% of original volume under 50 ℃, concentrated solution is transferred pH to 2-3 with the HCl aqueous solution of 5 ‰ v/v, uses equal-volume ethyl acetate extraction 3 times, removes impurity; The organic phase ethyl acetate discards or reclaims, and sour water is the purification extracting solution mutually;
(3) preparation of long handle stone China fir total alkaloids:
To purify extracting solution and transfer pH to 9-10 with the ammoniacal liquor of 1:1 (v/v), with isopyknic chloroform extraction 4 times, combined chloroform extraction liquid, underpressure distillation is removed chloroform and is got long handle stone China fir total alkaloids;
(4) preparation of selagine crude product:
With long handle stone China fir total alkaloids MPLC (RP-18) method, carry out wash-out take methanol-water as solvent systems, wash with water first, remove water soluble component, use again the methanol-water wash-out of 5-30% v/v, contain the component of selagine by the HPLC combining data detection, the methanol-water elutriant is concentrated, vacuum-drying gets faint yellow solid, is the selagine crude product;
(5) preparation of high-purity huperzine A:
Add proper amount of acetone or ethanol in above-mentioned selagine crude product, heating makes its dissolving and filtered while hot, and filtrate is crystallization under room temperature, and recrystallization is 3 times so repeatedly, and making selagine purity is 98-99%.
4. one of according to claim 1-3 described a kind of novel method of extracting selagine from long handle stone China fir is characterized in that step (3)-(5) agents useful for same is analytical pure AR, and water is distilled water.
5. one of according to claim 1-3 described a kind of novel method of extracting selagine from long handle stone China fir is characterized in that MPLC(RP-18) the used middle compression leg of method is that Jiangsu sharp fringe (Suzhou) scientific ﹠ technical corporation produces numbering: S-1101-3000; Post specification: internal diameter 156mm, height 410mm, volume 7800(mm)
3
6. one of according to claim 1-3 described a kind of novel method of extracting selagine from long handle stone China fir is characterized in that the used solvent of step (5) recrystallization is acetone.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103705548A (en) * | 2014-01-10 | 2014-04-09 | 吉首大学 | Method for extracting huperzia serrata total alkaloid from living bodies |
| CN103951618A (en) * | 2014-05-09 | 2014-07-30 | 自贡天健生物科技有限公司 | Huperzine A crystal, and preparation method and application thereof |
| CN106349162A (en) * | 2016-08-26 | 2017-01-25 | 安徽省虹升生物股份有限公司 | Method for extracting huperzine A from leaves of huperzia serrata |
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| CN101134743A (en) * | 2007-08-21 | 2008-03-05 | 陕西嘉禾植物化工有限责任公司 | Method for extracting and separating Huperzine from huperzine serrate |
| CN102432535A (en) * | 2011-12-29 | 2012-05-02 | 重庆市秀山红星中药材开发有限公司 | Method for extracting and separating huperzine A and huperzine B from huperzia serrata |
| CN102617469A (en) * | 2012-04-09 | 2012-08-01 | 重庆市秀山红星中药材开发有限公司 | Method for extracting huperzine a from huperzia serrata |
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| CN101134743A (en) * | 2007-08-21 | 2008-03-05 | 陕西嘉禾植物化工有限责任公司 | Method for extracting and separating Huperzine from huperzine serrate |
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| CN102617469A (en) * | 2012-04-09 | 2012-08-01 | 重庆市秀山红星中药材开发有限公司 | Method for extracting huperzine a from huperzia serrata |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103705548A (en) * | 2014-01-10 | 2014-04-09 | 吉首大学 | Method for extracting huperzia serrata total alkaloid from living bodies |
| CN103705548B (en) * | 2014-01-10 | 2015-11-04 | 吉首大学 | A kind of live body extracts the method for Huperzia serrata biological total alkali |
| CN103951618A (en) * | 2014-05-09 | 2014-07-30 | 自贡天健生物科技有限公司 | Huperzine A crystal, and preparation method and application thereof |
| CN106349162A (en) * | 2016-08-26 | 2017-01-25 | 安徽省虹升生物股份有限公司 | Method for extracting huperzine A from leaves of huperzia serrata |
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Application publication date: 20130109 |