CN102627576B - Preparation method for colchicine - Google Patents
Preparation method for colchicine Download PDFInfo
- Publication number
- CN102627576B CN102627576B CN201210087258.0A CN201210087258A CN102627576B CN 102627576 B CN102627576 B CN 102627576B CN 201210087258 A CN201210087258 A CN 201210087258A CN 102627576 B CN102627576 B CN 102627576B
- Authority
- CN
- China
- Prior art keywords
- colchicine
- preparation
- raw material
- extraction
- phase extraction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- IAKHMKGGTNLKSZ-INIZCTEOSA-N (S)-colchicine Chemical compound C1([C@@H](NC(C)=O)CC2)=CC(=O)C(OC)=CC=C1C1=C2C=C(OC)C(OC)=C1OC IAKHMKGGTNLKSZ-INIZCTEOSA-N 0.000 title claims abstract description 150
- 229960001338 colchicine Drugs 0.000 title claims abstract description 75
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 238000000605 extraction Methods 0.000 claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000011347 resin Substances 0.000 claims abstract description 13
- 229920005989 resin Polymers 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 30
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 27
- 239000007788 liquid Substances 0.000 claims description 19
- 238000002425 crystallisation Methods 0.000 claims description 11
- 230000008025 crystallization Effects 0.000 claims description 11
- 239000013078 crystal Substances 0.000 claims description 9
- 239000000706 filtrate Substances 0.000 claims description 9
- 239000003480 eluent Substances 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 7
- 230000000274 adsorptive effect Effects 0.000 claims description 7
- 238000011033 desalting Methods 0.000 claims description 7
- 238000005194 fractionation Methods 0.000 claims description 7
- 238000004128 high performance liquid chromatography Methods 0.000 claims description 7
- 239000000047 product Substances 0.000 claims description 7
- 238000001953 recrystallisation Methods 0.000 claims description 7
- 238000002791 soaking Methods 0.000 claims description 7
- 238000001179 sorption measurement Methods 0.000 claims description 7
- 235000011149 sulphuric acid Nutrition 0.000 claims description 7
- 239000001117 sulphuric acid Substances 0.000 claims description 7
- 238000009834 vaporization Methods 0.000 claims description 7
- 230000008016 vaporization Effects 0.000 claims description 7
- 238000010792 warming Methods 0.000 claims description 7
- 241000234435 Lilium Species 0.000 claims description 6
- 241001250596 Pleione Species 0.000 claims description 5
- 239000003463 adsorbent Substances 0.000 claims description 5
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 4
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 4
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 4
- 235000011152 sodium sulphate Nutrition 0.000 claims description 4
- HLBBKKJFGFRGMU-UHFFFAOYSA-M sodium formate Chemical compound [Na+].[O-]C=O HLBBKKJFGFRGMU-UHFFFAOYSA-M 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 238000010298 pulverizing process Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 2
- 238000005406 washing Methods 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 abstract 1
- 238000000227 grinding Methods 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 239000010414 supernatant solution Substances 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 8
- 238000000926 separation method Methods 0.000 description 7
- 239000012153 distilled water Substances 0.000 description 5
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 231100000614 poison Toxicity 0.000 description 2
- 230000007096 poisonous effect Effects 0.000 description 2
- 208000027496 Behcet disease Diseases 0.000 description 1
- 208000009137 Behcet syndrome Diseases 0.000 description 1
- 241000255579 Ceratitis capitata Species 0.000 description 1
- 240000008853 Datura stramonium Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 201000005569 Gout Diseases 0.000 description 1
- 206010019668 Hepatic fibrosis Diseases 0.000 description 1
- 244000056623 Iphigenia indica Species 0.000 description 1
- 206010037549 Purpura Diseases 0.000 description 1
- 241001672981 Purpura Species 0.000 description 1
- 206010037660 Pyrexia Diseases 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 235000000208 Solanum incanum Nutrition 0.000 description 1
- 230000005856 abnormality Effects 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 150000003797 alkaloid derivatives Chemical class 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 206010002022 amyloidosis Diseases 0.000 description 1
- 229940121363 anti-inflammatory agent Drugs 0.000 description 1
- 239000002260 anti-inflammatory agent Substances 0.000 description 1
- 150000003943 catecholamines Chemical class 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 210000000349 chromosome Anatomy 0.000 description 1
- 230000001684 chronic effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002068 genetic effect Effects 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000031864 metaphase Effects 0.000 description 1
- 230000000394 mitotic effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000003976 plant breeding Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000000069 prophylactic effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
Landscapes
- Medicines Containing Plant Substances (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a preparation method for colchicine. The preparation method for the colchicine is a method for preparing the colchicine by ultrasonic-assistant dual-water phase extraction, and particularly comprises the steps as follows: grinding a raw material containing the colchicine; carrying out dual-water phase extraction under the action of ultrasonic waves to obtain a supernatant solution containing rich colchicine; concentrating to obtain extractum; adding chloroform, dissolving and filtering; separating filter liquor through a macroporous absorption resin column; eluting, concentrating and crystallizing; and drying to obtain the colchicine. The preparation method is simple to operate, high in extraction rate and short in extraction time, and is suitable for industrial production.
Description
Technical field
The present invention relates to a kind of preparation method of colchicine, particularly adopt ultrasonic assistant aqueous two-phase extraction to prepare the method for colchicine by iphigenia indica, Bulbus Tulipae, lily.
Background technology
Colchicine has another name called colchicine, is a kind of alkaloid, and molecular formula is C
22h
25o
6n, pure colchicine is yellow needles, fusing point 157 DEG C.Soluble in water, ethanol and chloroform.Bitter is poisonous.Colchicine can suppress mitotic division, destroys spindle body, makes karyomit(e) be stuck in metaphase.From nineteen thirty-seven American scholar Blakeslee (A.F.Blakeslee) etc., after the chromosome number doubling the plants such as thorn apple by colchicine succeeds, colchicine is just widely used in cytology, genetic research and plant breeding.For the effective unique anti-inflammatory agent of urarthritis, gout acute attack being had to the result for the treatment of shown especially, is also effective prophylactic agent.In addition, colchicine also has certain effect being used for the treatment of in hepatic fibrosis, amyloidosis, family's Mediterranean fruit fly, catecholamine abnormality periodic fever, chronic immunity thrombopenic purpura, Behcet syndrome etc.
Colchicine is present in lily, and wherein the content of colchicine is between 0.1-0.4%.
In the prior art, colchicine mainly adopts synthetic method to produce, and step is long, and productive rate is low.Patent CN101602686 CO
2overcritically to extract from colchicine bulb powder, and adopt macroporous adsorbent resin to be separated, the extraction yield of colchicine is 0.002%, and purity is greater than 90%.This method preparation cost is high, and extraction yield is low.Patent CN101817760 mono-kind prepares the method for colchicine from new fresh Bulbus Lilii, extract 2-3 time with methanol eddy, with alumina column absorption after soda acid purifying, then use sherwood oil, eluent ethyl acetate, the 1/4 placement crystallization that elutriant is concentrated into its volume obtains coarse crystallization thing.The saturated dissolving of coarse crystallization thing ethyl acetate backflow, adjusts the temperature to less than 0 DEG C crystallization 16 hours, leaches, and obtain colchicine after recrystallize at least twice drying, its extraction yield is more than 0.16%, and content is greater than 97%, and this method technique is too complicated.
Summary of the invention
The present invention is directed to above-mentioned technical problem, there is provided that a kind of cost is lower, technique is simpler, can carry out the method for preparation of industrialization colchicine, the method for raw material, adopts Ultrasound-assisted aqueous two-phase extraction to prepare colchicine with lily, Lijiang, yunnan Pseudobulbus Cremastrae Seu Pleiones, Bulbus Lloydiae tibeticae.
The present invention is achieved through the following technical solutions:
1, aqueous two-phase extraction: will containing colchicine raw material pulverizing, add raw material weight 3-5 80%-95% ethanol doubly and the water of raw material weight 4-6 times respectively, mixing adds 0.5-2 salt doubly after soaking 20-30min, aqueous two-phase extraction 30-60min is carried out under the hyperacoustic effect of certain frequency, temperature is 40-70 DEG C, filter after extraction, filtrate is left standstill 10-15min, filtrate layering, Liquid liquid Separation must be rich in the upper solution of colchicine, get upper liquid concentrating under reduced pressure, temperature 50-55 DEG C, reclaim ethanol, after can not being concentrated into phlegma, continue to be warming up to 70-80 DEG C, transpiring moisture is 1.10-1.15g/cm to extraction concentrated solution proportion
3, obtained containing colchicine medicinal extract,
2, desalting and purifying: add medicinal extract weight 6-10 chloroform doubly in medicinal extract, the colchicine in medicinal extract is dissolved, and the impurity components such as inorganic salt do not dissolve, and filters, must containing the chloroformic solution of colchicine;
3, fractionation by adsorption, crystallization: the chloroformic solution containing colchicine is separated by macroporous adsorptive resins, eluent is made with the sulphuric acid soln of 0.5-0.8%, collect the water that elutriant reduction vaporization are no less than 3/4, recrystallization is carried out twice by adding ethyl acetate in concentrated solution, Tc 0-10 DEG C, time 8-10h, after crystal drying, obtain colchicine product, by the purity of HPLC analysed preparation.
It is a kind of in Lijiang, yunnan Pseudobulbus Cremastrae Seu Pleiones, Lijiang, yunnan Bulbus Tulipae, lily for containing colchicine raw material described in the present invention.
Salt described in the present invention is the one in ammonium sulfate, sodium sulfate, sodium formiate.
Hyperacoustic frequency described in the present invention is 30-200kHz.
Macroporous adsorbent resin described in the present invention is the one in D101, D3520, D201 macroporous adsorbent resin.
The drying of crystal described in the present invention is in vacuum, under 30-60 DEG C of condition, process 15-20h.
compared with prior art, tool of the present invention has the following advantages:
1, the present invention adopts ultrasound-assisted extraction, improves the percentage extraction of colchicine, can shorten extraction time 30min more than compared with extracting with Conventional solvents method simultaneously.
2, the present invention adopts aqueous two-phase extraction, serves again the effect of separation and purification while extraction.
3, the present invention avoids using poisonous organic solvent extraction, and low price, simple to operate, percentage extraction is high, is suitable for suitability for industrialized production.
Embodiment
embodiment 1:the preparation method of this colchicine, concrete operations are as follows:
1, aqueous two-phase extraction: get Lijiang, yunnan Pseudobulbus Cremastrae Seu Pleiones 3kg, add 10kg 95% ethanol and 15kg water respectively, 3kg ammonium sulfate is added after soaking 30min, aqueous two-phase extraction 40min is carried out under hyperacoustic effect, temperature is at 45 DEG C, ultrasonic frequency controls at 100kHz, filter, filtrate is left standstill 15min, and Liquid liquid Separation must be rich in the upper solution of colchicine, get upper liquid concentrating under reduced pressure, temperature is 55 DEG C, reclaims ethanol 3.56kg, after not going out phlegma, continue to be warming up to 80 DEG C, transpiring moisture is 1.12g/cm to extraction concentrated solution proportion
3, obtain the heavy 314.15g of medicinal extract.
2, desalting and purifying: will add the chloroform of 2.6kg in medicinal extract, dissolves colchicine, filters containing the chloroformic solution of colchicine.
3, fractionation by adsorption, crystallization: the chloroformic solution containing colchicine is separated by D101 macroporous adsorptive resins, eluent is made with the sulphuric acid soln of mass percent concentration 0.5%, collect the water that elutriant reduction vaporization fall 3/4, recrystallization is carried out twice by adding ethyl acetate in concentrated solution, Tc 0 DEG C, time 8h, crystal distilled water wash, vacuum 50 DEG C of dry 16h, obtaining colchicine product 5.65g, is 96.04% by the purity of HPLC analysed preparation.
embodiment 2:the preparation method of this colchicine, concrete operations are as follows:
1, aqueous two-phase extraction: get Lijiang, yunnan Bulbus Tulipae 3kg, add 9kg 95% ethanol and 15kg water respectively, 2kg sodium sulfate is added after soaking 25min, aqueous two-phase extraction 50min is carried out under hyperacoustic effect, temperature is 50 DEG C, ultrasonic frequency is 40kHz, filter, filtrate is left standstill 15min, and Liquid liquid Separation must be rich in the upper solution of colchicine, get upper liquid concentrating under reduced pressure, temperature is 55 DEG C, reclaims ethanol 3.12kg, after not going out phlegma, continue to be warming up to 75 DEG C, transpiring moisture is 1.10g/cm to extraction concentrated solution proportion
3, obtain the heavy 286.32g of medicinal extract.
2, desalting and purifying: will add the chloroform of 1.8kg in concentrated extract, dissolves colchicine, filters containing the chloroformic solution of colchicine.
3, fractionation by adsorption, crystallization: the chloroformic solution containing colchicine is separated by D3520 macroporous adsorptive resins, eluent is made with the sulphuric acid soln of mass percent concentration 0.6%, collect the water that elutriant reduction vaporization fall 4/5, recrystallization is carried out twice by adding ethyl acetate in concentrated solution, Tc 5 DEG C, time 10h, crystal distilled water wash, vacuum 60 DEG C of dry 15h, obtaining colchicine product 4.68g, is 97.26% by the purity of HPLC analysed preparation.
embodiment 3:the preparation method of this colchicine, concrete operations are as follows:
1, aqueous two-phase extraction: get lily bulb 3kg, adds 12kg 85% ethanol and 16kg water respectively, and add 1.5kg sodium formiate after soaking 30min, under hyperacoustic effect, carry out aqueous two-phase extraction 30min, temperature is 60 DEG C, and ultrasonic frequency is 80kHz.Filter, filtrate is left standstill 10min, and Liquid liquid Separation must be rich in the upper solution of colchicine, get upper liquid concentrating under reduced pressure, temperature is 55 DEG C, reclaims ethanol 4.64kg, after not going out phlegma, continue to be warming up to 80 DEG C, transpiring moisture is 1.13g/cm to extraction concentrated solution proportion
3, obtain the heavy 269.55g of medicinal extract.
2, desalting and purifying: will add the chloroform of medicinal extract weight 2kg in concentrated extract, dissolves colchicine, filters containing the chloroformic solution of colchicine.
3, fractionation by adsorption, crystallization: the chloroformic solution containing colchicine is separated by D201 macroporous adsorptive resins, eluent is made with the sulphuric acid soln of 0.8%, collect the water that elutriant reduction vaporization fall 4/5, recrystallization is carried out twice by adding ethyl acetate in concentrated solution, Tc 10 DEG C, time 10h, crystal distilled water wash, vacuum 30 DEG C of dry 20h, obtaining colchicine product 3.46g, is 95.01% by the purity of HPLC analysed preparation.
embodiment 4:the preparation method of this colchicine, concrete operations are as follows:
1, aqueous two-phase extraction: get Lijiang, yunnan Pseudobulbus Cremastrae Seu Pleiones 3kg, add 14kg 80% ethanol and 12kg water respectively, 4kg ammonium sulfate is added after soaking 30min, aqueous two-phase extraction 45min is carried out under hyperacoustic effect, temperature is at 70 DEG C, ultrasonic frequency controls at 140kHz, filter, filtrate is left standstill 12min, and Liquid liquid Separation must be rich in the upper solution of colchicine, get upper liquid concentrating under reduced pressure, temperature is 50 DEG C, reclaims ethanol 4.95kg, after not going out phlegma, continue to be warming up to 80 DEG C, transpiring moisture is 1.15g/cm to extraction concentrated solution proportion
3, obtain the heavy 365.48g of medicinal extract.
2, desalting and purifying: will add the chloroform of 3kg in concentrated extract, dissolves colchicine, filters containing the chloroformic solution of colchicine.
3, fractionation by adsorption, crystallization: the chloroformic solution containing colchicine is separated by D201 macroporous adsorptive resins, eluent is made with the sulphuric acid soln of 0.6%, collect the water that elutriant reduction vaporization fall 3/4, recrystallization is carried out twice by adding ethyl acetate in concentrated solution, Tc 2 DEG C, time 9h, crystal distilled water wash, vacuum 40 DEG C of dry 20h, obtaining colchicine product 5.03g, is 97.67% by the purity of HPLC analysed preparation.
embodiment 5:the preparation method of this colchicine, concrete operations are as follows:
1, aqueous two-phase extraction: get Lijiang, yunnan Bulbus Tulipae 3kg, adds 15kg 90% ethanol and 18kg water respectively, adds 6kg sodium sulfate after soaking 20min.Aqueous two-phase extraction 60min is carried out under hyperacoustic effect, temperature is at 40 DEG C, and ultrasonic frequency controls at 200kHz, filters, filtrate is left standstill 14min, Liquid liquid Separation must be rich in the upper solution of colchicine, gets upper liquid concentrating under reduced pressure, and temperature is 54 DEG C, reclaim ethanol 5.21kg, after not going out phlegma, continue to be warming up to 80 DEG C, transpiring moisture is 1.10g/cm to extraction concentrated solution proportion
3, obtain the heavy 341.26g of medicinal extract.
2, desalting and purifying: will add the chloroform of medicinal extract weight 3.4kg in concentrated extract, dissolves colchicine, filters containing the chloroformic solution of colchicine.
3, fractionation by adsorption, crystallization: the chloroformic solution containing colchicine is separated by D101 macroporous adsorptive resins, eluent is made with the sulphuric acid soln of 0.8%, collect the water that elutriant reduction vaporization fall 3/4, recrystallization is carried out twice by adding ethyl acetate in concentrated solution, Tc 8 DEG C, time 10h, crystal distilled water wash, vacuum 35 DEG C of dry 18h, obtaining colchicine product 4.04g, is 96.44% by the purity of HPLC analysed preparation.
Claims (4)
1. a preparation method for colchicine, is characterized in that carrying out as follows:
(1) aqueous two-phase extraction: will containing colchicine raw material pulverizing, add raw material weight 3-5 80-95% ethanol doubly and the water of raw material weight 4-6 times, mixing adds raw material weight 0.5-2 salt doubly after soaking 20-30min, mix 40-70 DEG C, carry out aqueous two-phase extraction 30-60min under ul-trasonic irradiation, filter, filtrate is left standstill 10-15min, filtrate layering, get upper liquid concentrating under reduced pressure, ethanol is reclaimed at 50-55 DEG C, after can not being concentrated into phlegma, continue to be warming up to 70-80 DEG C, transpiring moisture is 1.10-1.15g/cm to extraction concentrated solution proportion
3, obtained containing colchicine medicinal extract;
(2) desalting and purifying: add medicinal extract weight 6-10 chloroform doubly in medicinal extract, filter, must containing the chloroformic solution of colchicine;
(3) fractionation by adsorption, crystallization: the chloroformic solution containing colchicine is separated by macroporous adsorptive resins, eluent is made with the sulphuric acid soln of mass percent concentration 0.5-0.8%, collect the water that elutriant reduction vaporization are no less than 3/4, in concentrated solution, add ethyl acetate carry out recrystallization twice, Tc 0-10 DEG C, time 8-10h, obtained colchicine product after crystal washing is dry, by the purity of HPLC analysed preparation;
Described salt is the one in ammonium sulfate, sodium sulfate, sodium formiate;
Described hyperacoustic frequency is 30-200kHz.
2. the preparation method of colchicine according to claim 1, is characterized in that: be one or more mixture in Lijiang, yunnan Pseudobulbus Cremastrae Seu Pleiones, Lijiang, yunnan Bulbus Tulipae, lily containing colchicine raw material.
3. the preparation method of colchicine according to claim 1, is characterized in that: macroporous adsorbent resin is the one in D101, D3520, D201 macroporous adsorbent resin.
4. the preparation method of colchicine according to claim 1, is characterized in that: crystal drying is in vacuum, processes 15-20h under temperature 30-60 DEG C of condition.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210087258.0A CN102627576B (en) | 2012-03-29 | 2012-03-29 | Preparation method for colchicine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210087258.0A CN102627576B (en) | 2012-03-29 | 2012-03-29 | Preparation method for colchicine |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102627576A CN102627576A (en) | 2012-08-08 |
| CN102627576B true CN102627576B (en) | 2014-12-31 |
Family
ID=46586003
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210087258.0A Expired - Fee Related CN102627576B (en) | 2012-03-29 | 2012-03-29 | Preparation method for colchicine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102627576B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104610084B (en) * | 2015-02-04 | 2016-06-01 | 黄晨熙 | Extract the method for colchicine |
| CN106045871A (en) * | 2016-07-18 | 2016-10-26 | 唐翔 | Method for extracting iphigenia indica colchicine in auxiliary manner by adopting micro-cutting assisting interaction technology |
| CN106187807A (en) * | 2016-07-18 | 2016-12-07 | 陈志峰 | The extraction process of colchicine in a kind of Radix hemerocalis plicatae |
| CN110693993A (en) * | 2019-10-31 | 2020-01-17 | 安佰超 | Liver-protecting tablet for delaying drunkenness and preparation method thereof |
| CN115536542B (en) * | 2021-06-29 | 2024-01-05 | 昆药集团股份有限公司 | Preparation method of colchicine |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101602686A (en) * | 2009-05-26 | 2009-12-16 | 苏州派腾生物医药科技有限公司 | A kind of preparation method of colchicine |
-
2012
- 2012-03-29 CN CN201210087258.0A patent/CN102627576B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101602686A (en) * | 2009-05-26 | 2009-12-16 | 苏州派腾生物医药科技有限公司 | A kind of preparation method of colchicine |
Non-Patent Citations (2)
| Title |
|---|
| 刘陈力为等.超声波法提取黄花菜中秋水仙碱的研究.《湖南城市学院学报(自然科学版)》.2012,第21卷(第1期),第69-71页. * |
| 双水相萃取技术的研究现状与应用;辜鹏等;《化工技术与开发》;20071130;第36卷(第11期);第29-33页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102627576A (en) | 2012-08-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102627576B (en) | Preparation method for colchicine | |
| CN101798355B (en) | Method for integrated separation and extraction of tea polysaccharide, theanine, polyphenol and caffeine | |
| CN101781351B (en) | Method for extracting ginsenoside Rb1 from American ginseng and powder-injection thereof | |
| CN102617468A (en) | Method for ultrasound-assisted extraction of lappaconitine | |
| CN102491938A (en) | Purification method of deoxynojirimycin | |
| CN107739305A (en) | A kind of method for improving carnosic acid content in rosemary fat-soluble antioxidant | |
| CN102146083A (en) | Method for separating and extracting cepharanthine | |
| CN104262251A (en) | Method for extracting huperzine A from serrate clubmoss herb | |
| CN102060856B (en) | Method for extracting tabersonine from voacanga seeds | |
| CN104000840A (en) | Preparation method of extractive containing gastrodin and gastrodia elata polysaccharide | |
| CN103012544A (en) | Method for extracting saponin and polysaccharide from tea-seed pancake | |
| CN111777656B (en) | Method for extracting astragaloside from fresh astragalus | |
| CN106631807A (en) | Method for preparing chlorogenic acid from blueberry leaves | |
| CN102078342A (en) | Preparation method of water-soluble ginkgo biloba extract (GBE) | |
| CN110669096B (en) | Method for preparing astragaloside from astragalus | |
| CN102626430A (en) | Method for preparing total alkaloid from daphniphyllum calycinum | |
| CN106831930A (en) | A kind of extractant extracted for ursolic acid and extracting method | |
| CN101967505A (en) | Method for preparing dihydro quercetin | |
| CN105111144A (en) | Method of extracting nuciferine from lotus leaves | |
| CN106905339B (en) | Method for purifying phillygenin from forsythia suspense leaves | |
| CN112094184B (en) | Method for extracting shikimic acid from ginkgo leaf extract chromatographic wastewater | |
| CN103739648A (en) | Preparation method for mussaendoside U | |
| CN108912203B (en) | Preparation method of ginsenoside CK | |
| CN103387501A (en) | Method for preparing high-purity L-synephrine | |
| CN102675142B (en) | Method for purifying capsicine in hot pepper |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20141231 Termination date: 20160329 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |