CN101396373A - Cinobufacini extract and preparation method thereof - Google Patents
Cinobufacini extract and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a Chinese toad bufotoxin extract and a preparation method thereof. The extract contains the main effective components of cinobufagin with the content more than 0.15 percent and resibufogenin with the content more than 0.10 percent. The extract is made from dry toad skin and is prepared by the technologies of poaching, column chromatographic separation, eluting, condensing, drying, etc. The invention effectively removes useless substances (impurity) in the extract, is enriched in effective component and achieves the goals of improving the curative effect and reducing the toxic and side effects.
Description
Technical field
The present invention relates to a kind of extract and preparation method thereof, particularly a kind of Cinobufacini extract and preparation method thereof.
Background technology
Cinobufacini extract is the pale brown color extractum that the dry skin of Bufonidae (Bufonidae) animal Bufo siccus Bufo bufogargarizans Cantor makes through the extraction purification; The detoxifcation of cinobufacin tool, detumescence, pain relieving effect, be used for, disease such as late tumor, chronic hepatitis B, its biological active substances mainly is bufotoxin class (bufotoxins) and hydrolyzate bufotalin class (bufageins) thereof, bufotenine class (bufoteinines), also contains other chemical compounds such as cholesterol.
At present cinobufacin injection, oral liquid, tablet have been applied to clinically, but find cause product that certain toxic and side effects is arranged, and curative effect to reduce because inert matter (impurity) content height in the extract, active constituent content are low in clinical practice.
Summary of the invention
One object of the present invention is to disclose a kind of extract; Another object of the present invention is to disclose a kind of Cinobufacini extract; A further object of the invention is to disclose the preparation technology of this extract.
The present invention seeks to be achieved through the following technical solutions:
Cinobufagin content is more than 0.15% in the Cinobufacini extract of the present invention, and bufogenin content is more than 0.10%.
The preparation method of Cinobufacini extract of the present invention is:
Get dry maxima skin 1 weight portion, decoct 1-3 time, the decocting that at every turn adds the 4-12 parts by volume boiled 20 minutes-2 hours, merge decoction liquor, filter, filtrate is cooled to below 40 ℃, last macroporous adsorptive resins absorption, with 3-9 times of column volume water elution, add the 50%-95% ethanol elution of 2-8 times of column volume more earlier, collect ethanol elution, after reclaiming the ethanol in the eluent, concentrate, drying promptly gets Cinobufacini extract.
The preparation method of Cinobufacini extract of the present invention is preferably:
Get dry maxima skin 1 weight portion, decoct 2-3 time, the decocting that at every turn adds the 5-10 parts by volume boiled 0.5-1.5 hour, merge decoction liquor, filter, filtrate is cooled to below 40 ℃, last macroporous adsorptive resins absorption, with 5-7 times of column volume water elution, add the 60%-85% ethanol elution of 3-6 times of column volume more earlier, collect ethanol elution, after reclaiming the ethanol in the eluent, concentrate, drying promptly gets Cinobufacini extract.
The preparation method of Cinobufacini extract of the present invention is preferably:
Get dry maxima skin 1 weight portion, add the water of 10 parts by volume, decocted 45 minutes, promptly one fry in shallow oil; One fries in shallow oil the water that the back medicinal residues add 5 parts by volume, decocts 30 minutes, promptly two fries in shallow oil; Merge decoction liquor twice, filter, filtrate is cooled to below 40 ℃, last macroporous adsorptive resins absorption, with 6 times of column volume water elutions, add 70% ethanol elution of 5 times of column volumes more earlier, collect ethanol elution, behind the ethanol in the recovery eluent, concentrate, drying promptly gets Cinobufacini extract.
The preparation method of Cinobufacini extract of the present invention is preferably:
Get dry maxima skin 1 weight portion, add the water of 7 parts by volume, decocted 45 minutes, promptly one fry in shallow oil; One fries in shallow oil the water that the back medicinal residues add 5 parts by volume, decocts 45 minutes, promptly two fries in shallow oil; Merge decoction liquor twice, filter, filtrate is cooled to below 40 ℃, last macroporous adsorptive resins absorption, with 7 times of column volume water elutions, add 60% ethanol elution of 6 times of column volumes more earlier, collect ethanol elution, behind the ethanol in the recovery eluent, concentrate, drying promptly gets Cinobufacini extract.
The preparation method of Cinobufacini extract of the present invention is preferably:
Get dry maxima skin 1 weight portion, add the water of 10 parts by volume, decocted 30 minutes, promptly one fry in shallow oil; One fries in shallow oil the water that the back medicinal residues add 8 parts by volume, decocts 30 minutes, promptly two fries in shallow oil; Merge decoction liquor twice, filter, filtrate is cooled to below 40 ℃, last macroporous adsorptive resins absorption, with 5 times of column volume water elutions, add 80% ethanol elution of 4 times of column volumes more earlier, collect ethanol elution, behind the ethanol in the recovery eluent, concentrate, drying promptly gets Cinobufacini extract.
The macroporous adsorbent resin model is preferably neutral or low Polar Adsorbent Resin such as D101, AB-8 or NKA-9 in the above-mentioned preparation method.
The relation of weight portion/parts by volume of the present invention is: grams per milliliter
Get Cinobufacini extract of the present invention, add adjuvant, according to preparation process, make the dosage form of clinical acceptance, include but not limited to pharmaceutical dosage forms such as injection, capsule, drop pill, soft capsule, tablet, dispersible tablet, oral liquid, buccal tablet, ointment, nasal drop, granule.
Technical scheme of the present invention prepares extraction object height that cinobufagin in the Cinobufacini extract of gained, the existing described method of purification by macroporous resin technology (application number 200410083994.4) of bufogenin content make more than 5 times, and it is complete illustrate that bufotoxin effective constituents of the present invention keeps; And by with the pharmacodynamics contrast test of extract [get] by patent (application number 200510005277.4) " cinobufacin (Cutis Bufonis) extract production process " preparation, prove that extract obtained drug effect raising of the present invention and toxicity reduce.The present invention effectively removed the inert matter in the extract (impurity), enrichment effective ingredient, reached and improved the purpose that curative effect reduces toxic and side effects.
Following experimental example and embodiment are used to further specify but are not limited to the present invention.
Experimental example 1 extract yield and indoles total alkaloid content
1.1 instrument and reagent: UV-2401 ultraviolet-uisible spectrophotometer (day island proper Tianjin); Extract I (embodiment 1 described extract of the present invention); Extract II [getting] by patent (application number 200510005277.4) " cinobufacin (Cutis Bufonis) extract production process " preparation; 5-hydroxy tryptamine reference substance (Nat'l Pharmaceutical ﹠ Biological Products Control Institute).
1.2 experimental technique: the indoles Determination of Total Alkaloid is carried out with reference to method under HUACHANSU ZHUSHEYE (WS3-Bb-0027-95) " assay " item, the results are shown in Table 1.
Table 1 extract yield and indoles total alkaloid content
The result proves that extract yield of the present invention reduces but the indoles total alkaloid content obviously improves, and effective ingredient indoles total alkaloids obtains enrichment, and abandons a large amount of inert matters (impurity).
Cinobufagin, bufogenin content analysis in experimental example 2 extracts
2.1 instrument and reagent: HP-1100 high performance liquid chromatograph and detector (U.S. Hewlett-Packard), embodiment 1 described extract of the present invention; Cinobufagin reference substance and bufogenin reference substance (Nat'l Pharmaceutical ﹠ Biological Products Control Institute);
2.2 experimental technique: with reference to " content assaying method carries out under one one 265 pages (version was one one 316 pages in 2000) Venenum Bufonis items of Chinese pharmacopoeia version in 2005, the results are shown in Table 2.
Each extract cinobufagin of table 2, bufogenin content
* cinobufagin, the bufogenin content of extract in patent extract data referencing patent (application number 200410083994.4) " a kind of magnificent toadpoison freeze-dried powder and preparation method thereof " description " three, cinobufacin ethanol extract content analysis ".
The result proves that cinobufagin and bufogenin content improve greatly in the extract of the present invention, and the bufotoxin effective constituents obtains enrichment largely.
Experimental example 3 extract pharmacodynamics comparative study test
3.1 test material and reagent
3.1.1 extract I: embodiment 1 described extract of the present invention; Every g extractum is equivalent to the 60.61g crude drug in whole.Face the solution for standby that is made into desired concn with distilled water with preceding.This test dose is pressed crude drug in whole g/kg and is calculated.
Extract II: get by patent (application number 200510005277.4) " cinobufacin (Cutis Bufonis) extract production process " preparation; Every g extractum is equivalent to the 27.78g crude drug in whole.Face the solution for standby that is made into desired concn with distilled water with preceding.This test dose is pressed crude drug in whole g/kg and is calculated.
Cyclophosphamide: injection, Hengrui Medicine Co., Ltd., Jiangsu Prov., specification 0.2g/ bottle, lot number: 06071721, face with preceding with the fresh preparation of distilled water.
3.1.2 tumor strain
S180 tumor strain: available from the Huaxi Hospital Attached to Sichuan Univ institute of oncology.
H22 tumor strain: available from the Huaxi Hospital Attached to Sichuan Univ institute of oncology.
3.1.3 laboratory animal
Kunming mouse: the SPF level, female, body weight 24～26g, the Sichuan Provincial Academy of Traditional Chinese Medicine Experimental Animal Center provides.
3.2 experimental technique
3.2.1 oral each extract is to the influence of S180 mouse tumor growth
The strain of recovery mice S180 tumor adds an amount of sterile saline, abundant mixing, be mixed with tumor cell suspension (cell number〉1 * 10
7～2 * 10
7/ ml) be inoculated in 5 allogeneic mouse peritoneals (generation kind Mus).Extract ascites after 7 days, be inoculated in once more in 5 allogeneic mouse peritoneals (secondary kind of Mus).Choose the secondary kind Mus of growth after 7 days and extract ascites, mixing dilutes 10 times, counting cells concentration.Adjust cell concentration to 2 * 10
7/ ml, it is subcutaneous to be inoculated in 70 mice forelimb axils, every injected in mice 0.2ml, after inoculation the 2nd day, animal is weighed and be divided into 6 groups at random, irritate stomach HC I20g/kg, 4.0g/kg respectively, HC II20g/kg, 4.0g/kg, cyclophosphamide 20mg/kg and equivalent solvent, the distilled water matched group then gives isopyknic distilled water.Once a day, continuous 10 days.Put to death animal in 24 hours after the last administration, weigh, strip tumor, claim weight in wet base.The results are shown in Table 3.
Each extract of table 3 is to the inhibitory action of S180 mice
Compare with the solvent matched group: * P＜0.05, * * P＜0.01, * * * P＜0.001.
The result proves that each dosage group of extract I and extract II all can significantly suppress the growth of mice S180, and its tumour inhibiting rate is respectively 74.6%, 64.0%, 69.7% and 68.6%, with matched group significant difference is arranged relatively.Can find out also that from table 3 growth to the weight of animals when producing tumor-inhibiting action of each dosage group of extract I there is no obvious influence, and when suppressing tumor growth, also the slow down speed of growth of animal of extract II, the prompting extract II has certain toxic action when producing therapeutical effect.
3.2.2 oral each extract is to the influence of life cycle of H22 liver cancer mouse
The strain of recovery mice H22 tumor adds an amount of sterile saline, abundant mixing, be mixed with tumor cell suspension (cell number〉1 * 10
7～2 * 10
7/ ml) be inoculated in 5 allogeneic mouse peritoneals (generation kind Mus).Extract ascites after 7 days, be inoculated in once more in 5 allogeneic mouse peritoneals (secondary kind of Mus).Choose the secondary kind Mus of growth after 7 days and extract ascites, mixing dilutes 10 times, counting cells concentration.Adjust cell concentration to 2 * 10
7/ ml, be inoculated in 67 mouse peritoneals, every injected in mice 0.2ml, after inoculation the 2nd day, animal is weighed and be divided into 6 groups at random, irritate stomach extract I 20g/kg, 4.0g/kg respectively, extract II 20g/kg, 4.0g/kg, cyclophosphamide 20mg/kg, the distilled water matched group then gives isopyknic distilled water.Once a day, continuous 10 days.Continue after the last administration to observe and the record death time of animal behind inoculated tumour, the result carries out the t check, the results are shown in Table 4.
Oral each extract of table 4 is to the influence of life cycle of H22 liver cancer mouse
Compare with the solvent matched group: * P＜0.05, * * P＜0.01.
As seen from Table 4, but extract I 20g/kg, 4.0g/kg and extract II 20g/kg, 4.0g/kg equal life cycle of significant prolongation H22 mice compared significant difference with solvent.Its rate elongation is respectively 43.8%, 28.5%, 21.5% and 11.1%.As seen the extract I effect that prolongs tumor-bearing mice life cycle obviously is better than extract II.
3.3 brief summary
Above result proves that two kinds of extracts all have antitumor action, but better with the effect of extract I (preparation method of the present invention is extract obtained), toxicity is lower.
Following embodiment all can realize the effect of above-mentioned experimental example.
The specific embodiment
Embodiment 1:
Get dry maxima skin 1kg, add the 10L decocting and boiled 45 minutes, promptly one fry in shallow oil; One fries in shallow oil back medicinal residues adding 5L decocting boiled 30 minutes, promptly two fried in shallow oil; Merge decoction liquor twice, filter, filtrate is cooled to 30 ℃, last D101 macroporous adsorptive resins absorption, earlier use the 6L water elution, add the 5L70% ethanol elution again, collect ethanol elution, after reclaiming the ethanol in the eluent, concentrate, drying gets Cinobufacini extract 16.5g, the cinobufagin total amount is 31.2mg in the extract after measured, and the bufogenin total amount is 20.8mg.
Embodiment 2:
Get dry maxima skin 1kg, add the 7L decocting and boiled 45 minutes, promptly one fry in shallow oil; One fries in shallow oil back medicinal residues adding 5L water decocted 45 minutes again, promptly two fried in shallow oil; Merge decoction liquor twice, filter, filtrate is cooled to 25 ℃, last AB-8 macroporous adsorptive resins absorption, earlier use the 7L water elution, add 6L 60% ethanol elution again, collect ethanol elution, after reclaiming the ethanol in the eluent, concentrate, drying gets Cinobufacini extract 15.3g, the cinobufagin total amount is 22.9mg in the extract after measured, and the bufogenin total amount is 15.6mg.
Embodiment 3:
Get dry maxima skin 1kg, add 10L water, decocted 30 minutes, promptly one fry in shallow oil; One fries in shallow oil back medicinal residues adding 8L decocting boiled 30 minutes, promptly two fried in shallow oil; Merge decoction liquor twice, filter, filtrate is cooled to 35 ℃, last NKA-9 macroporous adsorptive resins absorption, earlier use the 5L water elution, add the 4L80% ethanol elution again, collect ethanol elution, after reclaiming the ethanol in the eluent, concentrate, drying gets Cinobufacini extract 18.4g, the cinobufagin total amount is 36.5mg in the extract after measured, and the bufogenin total amount is 24.2mg.
Embodiment 4:
Get dry maxima skin 1kg, add 5L water, decocted 1 hour, promptly one fry in shallow oil; One fries in shallow oil back medicinal residues adding 4L water fries in shallow oil half an hour again, and decoction liquor filters, and filtrate is cooled to 32 ℃, last D101 macroporous adsorptive resins absorption, earlier use the 8L water elution, add 7L 55% ethanol elution again, collect ethanol elution, after reclaiming the ethanol in the eluent, concentrate, drying gets Cinobufacini extract 13.8g, the cinobufagin total amount is 20.8mg in the extract after measured, and the bufogenin total amount is 13.9mg.
Embodiment 5:
Get dry maxima skin 1kg, add 22L water, decocted 45 fens, decoction liquor filters, and filtrate is cooled to 38 ℃, last AB-8 macroporous adsorptive resins absorption, earlier use the 4L water elution, add 3L 90% ethanol elution again, collect ethanol elution, after reclaiming the ethanol in the eluent, concentrate, drying gets Cinobufacini extract 17.1g, the cinobufagin total amount is 30.6mg in the extract after measured, and the bufogenin total amount is 24.3mg.
Embodiment 6:
Get dry maxima skin 1kg, add the 4L decocting at every turn and boiled 25 minutes, decoct 3 times; Merge three times decoction liquor, filter, filtrate is cooled to 28 ℃, last NKA-9 macroporous adsorptive resins absorption, earlier use the 8L water elution, add 2L 95% ethanol elution again, collect ethanol elution, after reclaiming the ethanol in the eluent, concentrate, drying gets Cinobufacini extract 15.8g, the cinobufagin total amount is 24.0mg in the extract after measured, and the bufogenin total amount is 16.5mg.
Claims (13)
1, a kind of Cinobufacini extract is characterized in that cinobufagin content is more than 0.15% in this extract, and bufogenin content is more than 0.10%.
2, Cinobufacini extract as claimed in claim 1, it is characterized in that this extract is prepared by following method: get dry maxima skin 1 weight portion, decoct 1-3 time, the decocting that at every turn adds the 4-12 parts by volume boiled 20 minutes-2 hours, merge decoction liquor, filter, filtrate is cooled to below 40 ℃, and last macroporous adsorptive resins absorption is earlier with 3-9 times of column volume water elution, the 50%-95% ethanol elution that adds 2-8 times of column volume again, collect ethanol elution, behind the ethanol in the recovery eluent, concentrate, drying promptly gets Cinobufacini extract.
3, Cinobufacini extract as claimed in claim 2, it is characterized in that this extract is prepared by following method: get dry maxima skin 1 weight portion, decoct 2-3 time, the decocting that at every turn adds the 5-10 parts by volume boiled 0.5-1.5 hour, merge decoction liquor, filter, filtrate is cooled to below 40 ℃, and last macroporous adsorptive resins absorption is earlier with 5-7 times of column volume water elution, the 60%-85% ethanol elution that adds 3-6 times of column volume again, collect ethanol elution, behind the ethanol in the recovery eluent, concentrate, drying promptly gets Cinobufacini extract.
4, Cinobufacini extract as claimed in claim 2 is characterized in that this extract is prepared by following method: get dry maxima skin 1 weight portion, add the water of 10 parts by volume, decocted 45 minutes, promptly one fry in shallow oil; One fries in shallow oil the water that the back medicinal residues add 5 parts by volume, decocts 30 minutes, promptly two fries in shallow oil; Merge decoction liquor twice, filter, filtrate is cooled to below 40 ℃, last macroporous adsorptive resins absorption, with 6 times of column volume water elutions, add 70% ethanol elution of 5 times of column volumes more earlier, collect ethanol elution, behind the ethanol in the recovery eluent, concentrate, drying promptly gets Cinobufacini extract.
5, Cinobufacini extract as claimed in claim 2 is characterized in that this extract is prepared by following method: get dry maxima skin 1 weight portion, add the water of 7 parts by volume, decocted 45 minutes, promptly one fry in shallow oil; One fries in shallow oil the water that the back medicinal residues add 5 parts by volume, decocts 45 minutes, promptly two fries in shallow oil; Merge decoction liquor twice, filter, filtrate is cooled to below 40 ℃, last macroporous adsorptive resins absorption, with 7 times of column volume water elutions, add 60% ethanol elution of 6 times of column volumes more earlier, collect ethanol elution, behind the ethanol in the recovery eluent, concentrate, drying promptly gets Cinobufacini extract.
6, Cinobufacini extract as claimed in claim 2 is characterized in that this extract is prepared by following method: get dry maxima skin 1 weight portion, add the water of 10 parts by volume, decocted 30 minutes, promptly one fry in shallow oil; One fries in shallow oil the water that the back medicinal residues add 8 parts by volume, decocts 30 minutes, promptly two fries in shallow oil; Merge decoction liquor twice, filter, filtrate is cooled to below 40 ℃, last macroporous adsorptive resins absorption, with 5 times of column volume water elutions, add 80% ethanol elution of 4 times of column volumes more earlier, collect ethanol elution, behind the ethanol in the recovery eluent, concentrate, drying promptly gets Cinobufacini extract.
7,, it is characterized in that the macroporous adsorbent resin model is the neutral or low Polar Adsorbent Resin of D101, AB-8 or NKA-9 in this preparation method of extract as the arbitrary described Cinobufacini extract of claim 2-6.
8, the preparation method of Cinobufacini extract as claimed in claim 1, it is characterized in that this method is: get dry maxima skin 1 weight portion, decoct 1-3 time, the decocting that at every turn adds the 4-12 parts by volume boiled 20 minutes-2 hours, merge decoction liquor, filter, filtrate is cooled to below 40 ℃, and last macroporous adsorptive resins absorption is earlier with 3-9 times of column volume water elution, the 50%-95% ethanol elution that adds 2-8 times of column volume again, collect ethanol elution, behind the ethanol in the recovery eluent, concentrate, drying promptly gets Cinobufacini extract.
9, the preparation method of Cinobufacini extract as claimed in claim 8, it is characterized in that this method is: get dry maxima skin 1 weight portion, decoct 2-3 time, the decocting that at every turn adds the 5-10 parts by volume boiled 0.5-1.5 hour, merge decoction liquor, filter, filtrate is cooled to below 40 ℃, and last macroporous adsorptive resins absorption is earlier with 5-7 times of column volume water elution, the 60%-85% ethanol elution that adds 3-6 times of column volume again, collect ethanol elution, behind the ethanol in the recovery eluent, concentrate, drying promptly gets Cinobufacini extract.
10, the preparation method of Cinobufacini extract as claimed in claim 8 is characterized in that this method is: get dry maxima skin 1 weight portion, add the water of 10 parts by volume, decocted 45 minutes, promptly one fry in shallow oil; One fries in shallow oil the water that the back medicinal residues add 5 parts by volume, decocts 30 minutes, promptly two fries in shallow oil; Merge decoction liquor twice, filter, filtrate is cooled to below 40 ℃, last macroporous adsorptive resins absorption, with 6 times of column volume water elutions, add 70% ethanol elution of 5 times of column volumes more earlier, collect ethanol elution, behind the ethanol in the recovery eluent, concentrate, drying promptly gets Cinobufacini extract.
11, the preparation method of Cinobufacini extract as claimed in claim 8 is characterized in that this method is: get dry maxima skin 1 weight portion, add the water of 7 parts by volume, decocted 45 minutes, promptly one fry in shallow oil; One fries in shallow oil the water that the back medicinal residues add 5 parts by volume, decocts 45 minutes, promptly two fries in shallow oil; Merge decoction liquor twice, filter, filtrate is cooled to below 40 ℃, last macroporous adsorptive resins absorption, with 7 times of column volume water elutions, add 60% ethanol elution of 6 times of column volumes more earlier, collect ethanol elution, behind the ethanol in the recovery eluent, concentrate, drying promptly gets Cinobufacini extract.
12, the preparation method of Cinobufacini extract as claimed in claim 8 is characterized in that this method is: get dry maxima skin 1 weight portion, add the water of 10 parts by volume, decocted 30 minutes, promptly one fry in shallow oil; One fries in shallow oil the water that the back medicinal residues add 8 parts by volume, decocts 30 minutes, promptly two fries in shallow oil; Merge decoction liquor twice, filter, filtrate is cooled to below 40 ℃, last macroporous adsorptive resins absorption, with 5 times of column volume water elutions, add 80% ethanol elution of 4 times of column volumes more earlier, collect ethanol elution, behind the ethanol in the recovery eluent, concentrate, drying promptly gets Cinobufacini extract.
13,, it is characterized in that the macroporous adsorbent resin model is the neutral or low Polar Adsorbent Resin of D101, AB-8 or NKA-9 in this method as the preparation method of the arbitrary described Cinobufacini extract of claim 8-12.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102973605A (en) * | 2011-06-02 | 2013-03-20 | 江苏省中医药研究院 | Toad skin extract dry powder inhalant and preparation method and applications thereof |
| CN105884855A (en) * | 2016-05-25 | 2016-08-24 | 安徽华润金蟾药业股份有限公司 | Cinobufagin refrigerating purification system and control method thereof |
| CN106496299A (en) * | 2016-08-31 | 2017-03-15 | 安徽华润金蟾药业股份有限公司 | The preparation method of high concentration Cinobufacini extract |
| CN114920795A (en) * | 2022-05-12 | 2022-08-19 | 赣江中药创新中心 | Preparation method of dried toad skin bufogenin lactone component |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1270769C (en) * | 2004-10-15 | 2006-08-23 | 张平 | Cinobufotalin lyophilized powder for injection and its preparation method |
| CN1813802A (en) * | 2005-02-04 | 2006-08-09 | 安徽金蟾生化股份有限公司 | Bufonid skin extract production process |
| CN1810827A (en) * | 2006-02-23 | 2006-08-02 | 崔彬 | Anticancer prepn containing three anticancer compounds of toad or toad cake and its prepn process |
| CN101019891B (en) * | 2007-02-14 | 2011-10-26 | 周亚球 | Toad skin total alkaloid and its prepn, analysis and prepn process |
-
2007
- 2007-09-29 CN CN2007101754398A patent/CN101396373B/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102973605A (en) * | 2011-06-02 | 2013-03-20 | 江苏省中医药研究院 | Toad skin extract dry powder inhalant and preparation method and applications thereof |
| CN102973605B (en) * | 2011-06-02 | 2015-05-27 | 江苏省中医药研究院 | Toad skin extract dry powder inhalant and preparation method and applications thereof |
| CN105884855A (en) * | 2016-05-25 | 2016-08-24 | 安徽华润金蟾药业股份有限公司 | Cinobufagin refrigerating purification system and control method thereof |
| CN105884855B (en) * | 2016-05-25 | 2017-09-15 | 安徽华润金蟾药业股份有限公司 | A kind of cinobufagin freezing purification system and its control method |
| CN106496299A (en) * | 2016-08-31 | 2017-03-15 | 安徽华润金蟾药业股份有限公司 | The preparation method of high concentration Cinobufacini extract |
| CN114920795A (en) * | 2022-05-12 | 2022-08-19 | 赣江中药创新中心 | Preparation method of dried toad skin bufogenin lactone component |
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| Publication number | Publication date |
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| CN101396373B (en) | 2011-04-06 |
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