CN1903856A - Preparation method of Tetrandrine and Fangchino-kine - Google Patents
Preparation method of Tetrandrine and Fangchino-kine Download PDFInfo
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Abstract
The present invention belongs to the field of plant effective component extraction technology. In particular, it relates to a preparation method of hanfangchin A and hanfangchin B. Said method includes the following steps: (1), preparing material: pulverizing or slicing raw material; (2), extraction: adding quicklime into raw material, added amount is 6-10% of raw material weight, then using polar organic solvent to make thermal reflux extraction of extract, recovering solvent, making concentrate undergo the processes of standing still, crystallization and filtration so as to obtain precipitate; (3), crystallization: using acetone to dissolve precipitate with thermal reflux, concentrating the dissolved solution to proper extent, standing still and crystallizing; (4), crude product preparation: using cold benzene to dissolve crystal to obtain insoluble substance and benzene dissolved solution, said insoluble substance is hanfangchin B crude product, the concentrated paste to benzene dissolved solution is hanfangchin A crude product.
Description
Affiliated technical field:
The present invention relates to plant efficient part extractive technique field, be specifically related to the preparation method of a kind of hanfangchin A and hanfangchin B.
Background technology:
The Chinese medicine powder root of fangji is used the history of existing more than one thousand years in China, oneself (claiming Radix Stephaniae Tetrandrae again) is the dry root section of Menispermaceae stephania plant (Stephania tetrandra S.Moore) for the powder workshop, the main effective constituent of its root kind is sinomenine (hanfangchin A, tetrandrine) and Radix Stephaniae Tetrandrae promise woods alkali (hanfangchin B, fangehinoline), hanfangchin C, contain flavonoid glycoside, phenols, organic acid, volatilization wet goods in addition.Studies show that sinomenine, Radix Stephaniae Tetrandrae promise woods alkali have effects such as analgesia, anti-inflammatory, step-down, antitumor, lax voluntary muscle, Recent study finds that sinomenine also has antiarrhythmic effect.Technology below the method for extraction hanfangchin A and hanfangchin B (fangehinoline) adopts more from the Radix stephaniae tetrandrae root at present: transfer PH10 with alkali after the ethanol-extracted, again with chloroform extraction, concentrated, condensed cream is through column chromatography for separation, ethanol, acetone crystallization, the problem that existing technology exists is: 1, complex process: processing step is many, operation easier is big, and adopts same operational path can not obtain two kinds of compositions simultaneously; 2, production cost height: solvent species is many, long through column chromatography, production cycle in the technology, so production cost is higher.
Summary of the invention:
The present invention will overcome complex process and the high problem of production cost that prior art exists.
For overcoming the problem that prior art exists, technical scheme of the present invention is: the preparation method of a kind of hanfangchin A and hanfangchin B comprises the steps successively
(1) gets the raw materials ready: acceptable material is pulverized or section;
(2) extract: add 6～10% heavy unslaked lime of raw material in the raw material, extract with the polar organic solvent thermal backflow then, reclaim solvent, concentrated solution is placed crystallization, must precipitate after the filtration;
(3) crystallization: precipitation is dissolved with the acetone thermal backflow, and acetone solution liquid is concentrated to an amount of placement crystallization;
(4) crude product preparation: crystallization is dissolved with cold benzene, gets insolubles and benzene lysate, and insolubles is the hanfangchin B crude product, and the condensed cream of benzene lysate is the hanfangchin A crude product.
Above-mentioned steps also comprises (5) purifying:
1. insolubles gets hanfangchin B with the acetone crystallization;
2. the condensed cream of benzene lysate gets hanfangchin A with the acetone crystallization.
The preferred version of such scheme is:
In the above-mentioned steps (1): pulverizing material can sieve by 16mm, unsuitable meticulous; Thickness is less than 1cm during section.
In the above-mentioned steps (2): the add-on of polar organic solvent is 3～5 times of amounts of raw material, and refluxing extraction 1.5～2h/ time is extracted for several times; United extraction liquid, underpressure distillation are concentrated into 4～6% of extracting liquid volume, solvent recuperation recycling, concentrated solution is at room temperature placed 12～15 hours after-filtration and must be precipitated, filtered liquid discards, precipitation dry crude product.
In the above-mentioned steps (3): with drying of gained crude product weigh 3～4 times of amounts with crude product acetone heated and stirred dissolving for several times, 1～1.5 hour/time, filter lysate, merge lysate, air distillation is concentrated into 15～18% of lysate, be placed into crystallizing at room temperature 12～15 hours, filter crystallization, crystallization dry crystal crude product; Filtered liquid concentrates and reclaims acetone.
In the above-mentioned steps (5):
1. with the oven dry of hanfangchin B crude product,, place crystallization 12～15 hours under the lysate room temperature, filter, obtain hanfangchin B with acetone thermal backflow dissolving, filtration;
2. with the oven dry of hanfangchin A crude product,, place crystallization 12～15 hours under the lysate room temperature, filter, obtain hanfangchin A with acetone thermal backflow dissolving, filtration.
In the above-mentioned steps (2), extract the miscible organic solvent of water and be meant: the arbitrary combination of 65～85% methyl alcohol, ethanol and these two kinds of solvents.
Cold benzene in the above-mentioned steps (4) is meant the benzene of temperature in the time of 10～15 ℃.
Compared with prior art, advantage of the present invention is:
1, step of the present invention is simple: the public process flow of the present invention is simple, does not need column chromatography, and Production Flow Chart is short, and is simple to operate, can obtain two kinds of products simultaneously under same operational path;
2, product purity height: the extraction yield of hanfangchin A can reach 97%; The extraction yield of hanfangchin B can reach 98%.
3, production cost is low: gained crystallization filtrated stock cover is used crystallization for the first time, can improve the rate of recovery, reduces acetone consumption, effectively reduces cost; The used recovery solvent of each step can be recycled, thereby reduces production costs, and the present invention is fit to suitability for industrialized production.
4, product nontoxicity: from then on do not contain the horse pocket spirit acid that causes renal toxicity in the raw material in the product of gained.
Embodiment:
Following examples further describe in detail the present invention, are to help to understand content of the present invention.
Embodiment 1:
The extraction and separation method of a kind of hanfangchin A and hanfangchin B comprises the steps: successively
(1) pulverizes: get the 600kg raw material pulverizing and sieve, must pulverize material 595kg by 16mm.Material content is: Tetrandrine 0.95%, Radix stephaniae tetrandrae second element 0.495%.
(2) extract: get and pulverize material 500kg, drop in the extractor, and the 40kg lime powder added with raw material gradually, adding 2000kg concentration then and be 70% methyl alcohol, thermal backflow is extracted 3 times, 1.5h/ it is inferior, united extraction liquid 5520kg, the extracting solution underpressure distillation is concentrated into 260kg, places room temperature, after-filtration must precipitate 40kg in 12 hours, the precipitation dry crude product 18kg.
Detect through high-pressure liquid phase (HPLC): contain Tetrandrine 5.24kg in the extracting solution, the plain 2.73kg of Radix stephaniae tetrandrae second, calculating extraction yield is 92%; Contain Tetrandrine 4.88kg in the oven dry crude product, the plain 2.38kg of Radix stephaniae tetrandrae second calculates the precipitation effective constituent rate of recovery and is respectively 93% and 87%.
(3) crystallization: the precipitation dry crude product 18kg, add 54kg acetone, the thermal backflow stirring and dissolving is dissolved 3 times altogether, 1 hour/time, filter press is crossed filter residue with the 30kg washing with acetone at every turn, merges dissolution filter liquid and washings, be total to 220kg acetone solution liquid, air distillation is concentrated into 36kg, leaves standstill to cool to room temperature, place centrifuging after 15 hours, dry crystallization 6.5kg.
Detect through high-pressure liquid phase (HPLC): Tetrandrine 63.7%, Radix stephaniae tetrandrae second element 29.2%.Calculate the precipitation effective constituent rate of recovery and be respectively 84.8% and 82.8%.
(4) crude product preparation: dry to such an extent that crystallization 6.5kg adds 20kg benzene, stirring and dissolving under 10～15 ℃ of conditions is dissolved 2 times altogether, 1 hour/time, filter press was used 5kg benzene washing and filtering slag at every turn, merge dissolution filter liquid and washings, altogether 45kg benzene lysate and 4kg benzene insoluble.The air distillation of benzene lysate concentrate condensed cream 5kg, be the Tetrandrine crude product, benzene insoluble is the plain crude product of Radix stephaniae tetrandrae second.
The plain crude product of Radix stephaniae tetrandrae second dry 2.1kg, detect through high-pressure liquid phase (HPLC): Tetrandrine 2.1%, Radix stephaniae tetrandrae second element 92%: the Tetrandrine crude product dry 4.4kg, detect through high-pressure liquid phase (HPLC): Tetrandrine 93%, Tetrandrine 1.7%.
(5) purifying:
1. the hanfangchin B crude product is dried 2.1kg, with 6.4kg acetone thermal backflow dissolving 1.5 hours, filter respectively after having dissolved, the washing of insolubles small amount of acetone, merge washings respectively, lysate is placed room temperature, and crystallization is 24 hours then, filtering for crystallizing dry the 1.75kg crystalline product, be hanfangchin B.The plain yield of Radix stephaniae tetrandrae second is 0.29%, and content is 98%.
2. the hanfangchin A crude product is dried 4.4kg, with 13.2kg acetone thermal backflow dissolving 1.5 hours, filter respectively after having dissolved, the washing of insolubles small amount of acetone, merge washings respectively, lysate is placed room temperature, and crystallization is 24 hours then, filtering for crystallizing dry the 3.7g crystalline product, be hanfangchin A.The Tetrandrine yield is 0.62%, and content is 97%.
Embodiment 2:
(1) pulverizes: get the 600kg raw material pulverizing and sieve, must pulverize material 590kg by 16mm.Material content is: Tetrandrine 0.95%, Radix stephaniae tetrandrae second element 0.495%.
(2) extract: get and pulverize material 500kg, drop in the extractor, and the 40kg lime powder added with raw material gradually, adding 2000kg concentration then and be 70% ethanol, thermal backflow is extracted 3 times, 1.5h/ it is inferior, united extraction liquid 5650kg, the extracting solution underpressure distillation is concentrated into 265kg, places room temperature, after-filtration must precipitate 44kg in 12 hours, the precipitation dry crude product 20kg.
Detect through high-pressure liquid phase (HPLC): contain Tetrandrine 5.42kg in the extracting solution, the plain 2.97kg of Radix stephaniae tetrandrae second, calculating extraction yield is 95%; Contain Tetrandrine 4.93kg in the oven dry crude product, the plain 2.60kg of Radix stephaniae tetrandrae second calculates the precipitation effective constituent rate of recovery and is respectively 91% and 87.5%.
(3) crystallization: the precipitation dry crude product 20kg, add 60kg acetone, the thermal backflow stirring and dissolving is dissolved 3 times altogether, 1 hour/time, filter press is crossed filter residue with the 30kg washing with acetone at every turn, merges dissolution filter liquid and washings, be total to 240kg acetone solution liquid, air distillation is concentrated into 40kg, leaves standstill to cool to room temperature, place centrifuging after 12 hours, dry crystallization 6.7kg.
Detect through high-pressure liquid phase (HPLC): Tetrandrine 64.1%, Radix stephaniae tetrandrae second element 31.1%.Calculate the precipitation effective constituent rate of recovery and be respectively 87.1% and 80%.
(4) crude product preparation: dry to such an extent that crystallization 6.7kg adds 20kg benzene, stirring and dissolving under 10～15 ℃ of conditions, dissolve altogether 2 times, 1 hour/time, filter press, each with 5kg benzene washing and filtering slag, merge dissolution filter liquid and washings, be total to 45kg benzene lysate and 4.7kg benzene insoluble, the air distillation of benzene lysate concentrates and obtains the 5kg condensed cream, be the Tetrandrine crude product, benzene insoluble is the plain crude product of Radix stephaniae tetrandrae second.
Vacuum drying insolubles and condensed cream are dried thing respectively.Detect through high-pressure liquid phase (HPLC): Tetrandrine 2.2% in the insolubles, Radix stephaniae tetrandrae second element 93%: Tetrandrine 94% in the condensed cream oven dry thing, Radix stephaniae tetrandrae second element 1.6%.
(5) purifying:
1. the hanfangchin B crude product is dried 2.2kg, with 6.6kg acetone thermal backflow dissolving 1.5 hours, filter respectively after having dissolved, the washing of insolubles small amount of acetone, merge washings respectively, lysate is placed room temperature, and crystallization is 24 hours then, filtering for crystallizing dry the 1.81kg crystalline product, be hanfangchin B.The plain yield of Radix stephaniae tetrandrae second is 0.31%, and content is 98.1%.
2. the hanfangchin A crude product is dried 4.5kg, with 13.5kg acetone thermal backflow dissolving 1.5 hours, filter respectively after having dissolved, the washing of insolubles small amount of acetone, merge washings respectively, lysate is placed room temperature, and crystallization is 24 hours then, filtering for crystallizing dry the 3.75g crystalline product, be hanfangchin A.The Tetrandrine yield is 0.625%, and content is 97.1%.
Embodiment 3:
(1) pulverizes: get the 600kg raw material pulverizing and sieve, must pulverize material 590kg by 16mm.Material content is: Tetrandrine 0.95%, Radix stephaniae tetrandrae second element 0.495%.
(2) extract: get and pulverize material 500kg, drop in the extractor, and the 50kg lime powder added with raw material gradually, adding 1500kg concentration then and be 80% methyl alcohol, thermal backflow is extracted 3 times, 2h/ time, united extraction liquid 4000kg extracting solution, the extracting solution underpressure distillation is concentrated into 270kg, places room temperature, after-filtration must precipitate 41kg in 12 hours, the precipitation dry crude product 18.5kg.
Detect through high-pressure liquid phase (HPLC): contain Tetrandrine 5.30kg in the extracting solution, the plain 2.70kg of Radix stephaniae tetrandrae second, calculating extraction yield is 92.1%; Contain Tetrandrine 4.89kg in the oven dry crude product, the plain 2.40kg of Radix stephaniae tetrandrae second calculates the precipitation effective constituent rate of recovery and is respectively 93.2% and 87.4%.
(3) crystallization: the precipitation dry crude product 16kg, add 55kg acetone, the thermal backflow stirring and dissolving is dissolved 3 times altogether, 1.5 hour/time, filter press is crossed filter residue with the 30kg washing with acetone at every turn, merges dissolution filter liquid and washings, be total to 200kg acetone solution liquid, air distillation is concentrated into 36kg, leaves standstill to cool to room temperature, place centrifuging after 12 hours, dry crystallization 6.48kg.
Detect through high-pressure liquid phase (HPLC): Tetrandrine 63.8%, Radix stephaniae tetrandrae second element 29.5%.Calculate the precipitation effective constituent rate of recovery and be respectively 85% and 83%.
(4) crude product preparation: dry to such an extent that crystallization 6.5kg adds 20kg toluene, stirring and dissolving under 10～15 ℃ of conditions, dissolve altogether 2 times, 1.5 hours/time, filter press, each with 5kg benzene washing and filtering slag, merge dissolution filter liquid and washings, be total to 47kg toluene lysate and 4.6kg benzene insoluble, the air distillation of benzene lysate concentrates and obtains the 5.5kg condensed cream, be the Tetrandrine crude product, benzene insoluble is the plain crude product of Radix stephaniae tetrandrae second.
Detect through high-pressure liquid phase (HPLC): Tetrandrine 2.6% in the insolubles, Radix stephaniae tetrandrae second element 92.3%: Tetrandrine 92.9% in the condensed cream oven dry thing, Radix stephaniae tetrandrae second element 1.9%.
(5) purifying:
1. the hanfangchin B crude product is dried 2.13kg, with 6.5kg acetone thermal backflow dissolving 1.5 hours, filter respectively after having dissolved, the washing of insolubles small amount of acetone, merge washings respectively, lysate is placed room temperature, and crystallization is 28 hours then, filtering for crystallizing dry the 1.74kg crystalline product, be hanfangchin B.The plain yield of Radix stephaniae tetrandrae second is 0.29%, and content is 98.1%.
2. the hanfangchin A crude product is dried 4.45kg, with 13.5kg acetone thermal backflow dissolving 1.5 hours, filter respectively after having dissolved, the washing of insolubles small amount of acetone, merge washings respectively, lysate is placed room temperature, and crystallization is 28 hours then, filtering for crystallizing dry the 3.73g crystalline product, be hanfangchin A.The Tetrandrine yield is 0.62%, and content is 97.6%.
Embodiment 4:
(1) pulverize: get the section of 510kg raw material, thickness must be pulverized material 500kg less than 1cm during section.Material content is: Tetrandrine 0.9%, Radix stephaniae tetrandrae second element 0.5%.
(2) extract: get and pulverize material 500kg, drop in the extractor, and the 30kg lime powder added with raw material gradually, adding raw material 1900kg concentration then and be 80% methyl alcohol and 600kg80% ethanol, thermal backflow is extracted 3 times, 1.5h/ it is inferior, merge the 7000kg extracting solution, the extracting solution underpressure distillation is concentrated into 320kg, places room temperature, after-filtration must precipitate 34kg in 15 hours, the precipitation dry crude product 16.2kg.
Detect through high-pressure liquid phase (HPLC): contain Tetrandrine 4.59kg in the extracting solution, the plain 2.42kg of Radix stephaniae tetrandrae second, calculating extraction yield is 94%; Contain Tetrandrine 4.23kg in the oven dry crude product, the plain 2.1kg of Radix stephaniae tetrandrae second calculates the precipitation effective constituent rate of recovery and is respectively 95% and 90%.
(3) crystallization for the first time: precipitation dry crude product 16.2kg, add 55kg acetone, the thermal backflow stirring and dissolving is dissolved 3 times altogether, 1 hour/time, filter press is crossed filter residue with the 30kg washing with acetone at every turn, merges dissolution filter liquid and washings, be total to 220kg acetone solution liquid, air distillation is concentrated into 33kg, leaves standstill to cool to room temperature, place centrifuging after 15 hours, dry crystallization 5.61kg.
Detect through high-pressure liquid phase (HPLC): Tetrandrine 63.8%, Radix stephaniae tetrandrae second element 29.5%.Calculate the precipitation effective constituent rate of recovery and be respectively 86.6% and 84.6%.
(4) crude product preparation: dry to such an extent that crystallization 5.61kg adds 20kg toluene, stirring and dissolving under 10～15 ℃ of conditions, dissolve altogether 2 times, 1.3 hours/time, filter press, each with 5kg benzene washing and filtering slag, merge dissolution filter liquid and washings, be total to 48kg toluene lysate and 4.0kg toluene insolubles, the air distillation of benzene lysate concentrates and obtains the 4.5kg condensed cream, be the Tetrandrine crude product, benzene insoluble is the plain crude product of Radix stephaniae tetrandrae second.
Detect through high-pressure liquid phase (HPLC): Tetrandrine 2.62% in the insolubles, Radix stephaniae tetrandrae second element 92.1%: Tetrandrine 92.7% in the condensed cream oven dry thing, Radix stephaniae tetrandrae second element 1.92%.
(5) purifying:
1. the hanfangchin B crude product is dried 1.84kg, with 6.25kg acetone thermal backflow dissolving 2 hours, filter respectively after having dissolved, the washing of insolubles small amount of acetone, merge washings respectively, lysate is placed room temperature, and crystallization is 24 hours then, filtering for crystallizing dry the 1.51kg crystalline product, be hanfangchin B.The plain yield of Radix stephaniae tetrandrae second is 0.30%, and content is 98%.
2. the hanfangchin A crude product is dried 3.74kg, with 13kg acetone thermal backflow dissolving 2 hours, filter respectively after having dissolved, the washing of insolubles small amount of acetone, merge washings respectively, lysate is placed room temperature, and crystallization is 24 hours then, filtering for crystallizing dry the 3.23g crystalline product, be hanfangchin A.The Tetrandrine yield is 0.63%, and content is 97.8%.
Claims (8)
1, the preparation method of a kind of hanfangchin A and hanfangchin B comprises the steps successively,
(1) gets the raw materials ready: acceptable material is pulverized or section;
(2) extract: add 6～10% heavy unslaked lime of raw material in the raw material, extract with the polar organic solvent thermal backflow then, reclaim solvent, concentrated solution is placed crystallization, must precipitate after the filtration;
(3) crystallization: precipitation is dissolved with the acetone thermal backflow, and acetone solution liquid is concentrated to an amount of placement crystallization;
(4) crude product preparation: crystallization is dissolved with cold benzene, gets insolubles and benzene lysate, and insolubles is the hanfangchin B crude product, and the condensed cream of benzene lysate is the hanfangchin A crude product.
2, the preparation method of a kind of hanfangchin A as claimed in claim 1 and hanfangchin B is characterized in that: described step also comprises (5) purifying,
1. insolubles gets hanfangchin B with the acetone crystallization;
2. the condensed cream of benzene lysate gets hanfangchin A with the acetone crystallization.
3, the preparation method of a kind of hanfangchin A as claimed in claim 1 or 2 and hanfangchin B is characterized in that: in the described step (1), pulverizes material and can sieve by 16mm, and unsuitable meticulous; Thickness is less than 1cm during section.
4, the preparation method of a kind of hanfangchin A as claimed in claim 3 and hanfangchin B is characterized in that: in the described step (2), the add-on of polar organic solvent is 3～5 times of amounts of raw material, and refluxing extraction 1.5～2h/ time is extracted for several times; United extraction liquid, underpressure distillation are concentrated into 4～6% of extracting liquid volume, solvent recuperation recycling, concentrated solution is at room temperature placed 12～15 hours after-filtration and must be precipitated, filtered liquid discards, precipitation dry crude product.
5, the preparation method of a kind of hanfangchin A as claimed in claim 4 and hanfangchin B, it is characterized in that: in the described step (3), with drying of gained crude product weigh 3～4 times of amounts with crude product acetone heated and stirred dissolving for several times, 1～1.5 hour/time, filter lysate, merge lysate, air distillation is concentrated into 15～18% of lysate, be placed into crystallizing at room temperature 12～15 hours, filter crystallization, crystallization dry crystal crude product; Filtered liquid concentrates and reclaims acetone.
6, the preparation method of a kind of hanfangchin A as claimed in claim 5 and hanfangchin B is characterized in that: in the described step (5),
1. with the oven dry of hanfangchin B crude product,, place crystallization 12～15 hours under the lysate room temperature, filter, obtain hanfangchin B with acetone thermal backflow dissolving, filtration;
2. with the oven dry of hanfangchin A crude product,, place crystallization 12～15 hours under the lysate room temperature, filter, obtain hanfangchin A with acetone thermal backflow dissolving, filtration.
7, the preparation method of a kind of hanfangchin A as claimed in claim 6 and hanfangchin B is characterized in that: in the described step (2), extract the miscible organic solvent of water and be meant: the arbitrary combination of 65～85% methyl alcohol, ethanol and these two kinds of solvents.
8, the preparation method of a kind of hanfangchin A as claimed in claim 7 and hanfangchin B is characterized in that: the cold benzene in the described step (4) is meant the benzene of temperature in the time of 10～15 ℃.
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| CN102382119A (en) * | 2011-10-19 | 2012-03-21 | 陕西省西安植物园 | Extraction method of tetrandrine and demethyltetrandrine |
| CN102649793A (en) * | 2011-02-25 | 2012-08-29 | 苏州宝泽堂医药科技有限公司 | Preparation method of alkaloid in stephania tetrandra |
| CN102649794A (en) * | 2011-02-25 | 2012-08-29 | 苏州宝泽堂医药科技有限公司 | Purification method of fangchinoline |
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| WO2002051812A1 (en) * | 2000-12-27 | 2002-07-04 | Cba International, Inc. | Method for extracting bisbenzylisoquinolines |
| AU2002318715A1 (en) * | 2002-07-18 | 2004-02-09 | Institute Of Chinese Materia Medica, China Academy Of Traditional Chinese Medicine | Preparation extracted from stephania tetrandra s. moor and the use thereof |
| CN1203853C (en) * | 2002-11-12 | 2005-06-01 | 陈介甫 | Special ingredient extract of tetrandra root and its use |
| CN1328280C (en) * | 2002-11-28 | 2007-07-25 | 中国科学院上海药物研究所 | Tetrandrine and tetrandrine compound, synthesis and uses thereof |
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| CN102649794A (en) * | 2011-02-25 | 2012-08-29 | 苏州宝泽堂医药科技有限公司 | Purification method of fangchinoline |
| CN102382119A (en) * | 2011-10-19 | 2012-03-21 | 陕西省西安植物园 | Extraction method of tetrandrine and demethyltetrandrine |
| CN102382119B (en) * | 2011-10-19 | 2014-06-25 | 陕西省西安植物园 | Extraction method of tetrandrine and demethyltetrandrine |
| WO2014048377A1 (en) | 2012-09-28 | 2014-04-03 | 杭州本生药业有限公司 | Drug composition for treating tumors and application thereof |
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| CN111153909A (en) * | 2020-01-17 | 2020-05-15 | 石药集团江西金芙蓉药业股份有限公司 | A double-template molecular imprinting purification method for alpha-and beta-carotene in Stephania tetrandra |
| CN111153909B (en) * | 2020-01-17 | 2022-05-17 | 石药集团江西金芙蓉药业股份有限公司 | A double-template molecular imprinting purification method for alpha-and beta-carotene in Stephania tetrandra |
| CN111217822A (en) * | 2020-03-12 | 2020-06-02 | 上海浙星新型材料科技有限公司 | Preparation method of tetrandrine as Chinese medicinal anti-allergy agent |
| CN112608328A (en) * | 2020-12-24 | 2021-04-06 | 重庆医药高等专科学校 | Crystal form of 5-bromotetrandrine ethyl formate and preparation method thereof |
| CN112608328B (en) * | 2020-12-24 | 2021-09-28 | 重庆医药高等专科学校 | Crystal form of 5-bromotetrandrine ethyl formate and preparation method thereof |
| CN113185527A (en) * | 2021-05-10 | 2021-07-30 | 浙江耐司康药业有限公司 | Method for separating tetrandrine and tetrandrine |
| CN113185527B (en) * | 2021-05-10 | 2022-07-29 | 浙江耐司康药业有限公司 | Method for separating tetrandrine and tetrandrine |
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