CN102898409A - Method for extracting fischeriana B from Euphorbia ebracteolata Hayata - Google Patents
Method for extracting fischeriana B from Euphorbia ebracteolata Hayata Download PDFInfo
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- CN102898409A CN102898409A CN201210340206XA CN201210340206A CN102898409A CN 102898409 A CN102898409 A CN 102898409A CN 201210340206X A CN201210340206X A CN 201210340206XA CN 201210340206 A CN201210340206 A CN 201210340206A CN 102898409 A CN102898409 A CN 102898409A
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Abstract
The invention discloses a method for extracting fischeriana B from Euphorbia ebracteolata Hayata. The method comprises the following steps: crushing the root of Euphorbia ebracteolata Hayata; adding ethanol; subjecting an obtained alkaline solution of ethanol to refluxing; carrying out pumping filtration and separation; adding an alkali into a filtrate obtained after pumping filtration to adjust a pH value to 8 to 10; standing for 24 to 48 h to allow insoluble substances to be precipitated; carrying out filtration to remove the insoluble substances; adding an acid for acidifying so as to allow a pH value to be 2 to 3; carrying out standing, deposition and pumping filtration so as to obtain a filter cake; dissolving the filter cake with a solvent; then adding silica gel for mixing of a sample; carrying out spin drying to obtain powder; then carrying out gradient elution, column chromatographic separation, evaporation and condensation to obtain a solid; and dissolving the obtained solid in methanol and carrying out re-crystallization and filtration so as to obtain fischeriana B. The method is simple to operated, and an obtained product has high purity.
Description
Technical field
The present invention relates to the Separation of Natural Products field, exactly is a kind of method of extracting root of langdu second element from euphorbia ebiacteolata Hayata.
Background technology
Euphorbia ebiacteolata Hayata belongs to euphorbia plant, and its effective component is root, and has higher toxicity.Medicinal material originates in the ground such as Anhui, Henan, Jiangsu, Shandong, Hubei, for a long time because its higher toxicity.But nearest progress shows, the euphorbia ebiacteolata Hayata root has good pharmaceutical component, the dissipating bind of can relieving oedema or abdominal distension through diuresis or purgation, broken long-pending desinsection.Be used for oedema abdominal distension, the phlegm carnivorism is long-pending; Outer for tuberculous lymphadenitis, psoriasis, the maggot of going out.Therefore use in these areas the favor that enjoys academia.
Because the pollution of environment has been accelerated in for a long time use of chemical pesticide, residual the exceeding standard of various chemical pesticides becomes the principal element that affects people's lives, therefore, the natural agricultural chemicals of seeking suitable environmentally friendly sterilant and low toxicity becomes the main task of current Pesticide Science.
This area obtains environmentally friendly biogenic pesticide in the urgent need to a kind of reasonable Separation of Natural Products method.
Summary of the invention
The purpose of this invention is to provide a kind of simple to operate, the method for from euphorbia ebiacteolata Hayata, extracting root of langdu second element that product purity is higher.
Above-mentioned purpose realizes by following scheme:
A kind of method of extracting root of langdu second element from euphorbia ebiacteolata Hayata is characterized in that: may further comprise the steps:
(1) get the euphorbia ebiacteolata Hayata root, be crushed to the 40-60 order, drop in the reactor, add the ethanol of 60%-80%, and regulate pH value to 8-11, obtain the basic solution of ethanol, 70-80 ℃ of left and right sides oil bath backflow 2-4h, suction filtration separates, and gets filtrate;
(2) add alkali in the filtrate of suction filtration and regulate PH to 8-10, leave standstill 24-48h, insolubles is precipitated out, then remove by filter insolubles, be acidified with acid so that PH=2-3 staticly settles, suction filtration obtains filter cake;
(3) with adding silica gel mixed sample behind the dissolution with solvents filter cake, be spin-dried for powdered, adopt sherwood oil, ethyl acetate system, gradient elution, column chromatography for separation, the concentrated solid that obtains of evaporate to dryness;
(4) step (3) gained dissolution of solid is carried out recrystallization in methyl alcohol, namely get root of langdu second element after the filtration.
Described a kind of method of extracting root of langdu second element from euphorbia ebiacteolata Hayata, it is characterized in that: the basic solution solid-liquid ratio of the ethanol in the step (1) is 1:6-10.
Described a kind of method of extracting root of langdu second element from euphorbia ebiacteolata Hayata is characterized in that: the described alkali that adds among the alkali adjusting PH to 8-10 of step (2) refers to sodium hydroxide solution, and the acid in being acidified with acid refers to hydrochloric acid.
Described a kind of method of extracting root of langdu second element from euphorbia ebiacteolata Hayata, it is characterized in that: described silica gel particle particle diameter is the 200-300 order.
Described a kind of method of extracting root of langdu second element from euphorbia ebiacteolata Hayata, it is characterized in that: described recrystallization rearing crystal time is 4-6h.
Beneficial effect of the present invention is: the method is simple to operate, and product purity is high, it is generally acknowledged chromatogram inclusion-free peak, is sterling.The core of this new production technique is to utilize the method for alkali extraction and acid precipitation to extract active parasite killing composition root of langdu second element from euphorbia ebiacteolata Hayata root powder.
Embodiment
Embodiment 1,
(1), successively get 50g euphorbia ebiacteolata Hayata root powder, add the aqueous ethanolic solution of 400mL 60%, regulate PH=10 with sodium hydroxide;
(2) 70 ℃ of water-bath backflow 4h, suction filtration separates
(3) solution is added alkali and continue precipitation, filter.Evaporation concentration.Add hydrochloric acid and regulate PH=2, staticly settle, suction filtration obtains filter cake
(4) filter cake is distributed in the silica gel, mixes powder, column chromatography for separation obtains root of langdu second element.
Embodiment 2,
A kind of method of extracting root of langdu second element from euphorbia ebiacteolata Hayata may further comprise the steps:
(1) get the euphorbia ebiacteolata Hayata root, be crushed to 50 orders, drop in the reactor, add 80% ethanol, and regulate pH value to 8, obtain the basic solution that liquor ratio is 1:8 ethanol, 80 ℃ of left and right sides oil bath backflow 4h, suction filtration separates, and gets filtrate;
(2) the hydro-oxidation sodium solution is regulated PH to 10 in the filtrate of suction filtration, leaves standstill 24h, and insolubles is precipitated out, and then removes by filter insolubles, adds the hydrochloric acid acidifying so that PH=3 staticly settles, and suction filtration obtains filter cake;
(3) be 200-300 purpose silica gel mixed sample with adding grain diameter behind the dissolution with solvents filter cake, be spin-dried for powdered, adopt sherwood oil, ethyl acetate system, gradient elution, column chromatography for separation, the concentrated solid that obtains of evaporate to dryness;
(4) step (3) gained dissolution of solid is carried out recrystallization in methyl alcohol, rearing crystal time is 5h, namely gets root of langdu second element after the filtration.
Claims (5)
1. method of extracting root of langdu second element from euphorbia ebiacteolata Hayata is characterized in that: may further comprise the steps:
(1) get the euphorbia ebiacteolata Hayata root, be crushed to the 40-60 order, drop in the reactor, add the ethanol of 60%-80%, and regulate pH value to 8-11, obtain the basic solution of ethanol, 70-80 ℃ of left and right sides oil bath backflow 2-4h, suction filtration separates, and gets filtrate;
(2) add alkali in the filtrate of suction filtration and regulate PH to 8-10, leave standstill 24-48h, insolubles is precipitated out, then remove by filter insolubles, be acidified with acid so that PH=2-3 staticly settles, suction filtration obtains filter cake;
(3) with adding silica gel mixed sample behind the dissolution with solvents filter cake, be spin-dried for powdered, adopt sherwood oil, ethyl acetate system, gradient elution, column chromatography for separation, the concentrated solid that obtains of evaporate to dryness;
(4) step (3) gained dissolution of solid is carried out recrystallization in methyl alcohol, namely get root of langdu second element after the filtration.
2. a kind of method of extracting root of langdu second element from euphorbia ebiacteolata Hayata according to claim 1, it is characterized in that: the basic solution solid-liquid ratio of the ethanol in the step (1) is 1:6-10.
3. a kind of method of extracting root of langdu second element from euphorbia ebiacteolata Hayata according to claim 1 is characterized in that: step (2) is described to be added the alkali that alkali regulates among the PH to 8-10 and refers to sodium hydroxide solution, and the acid in being acidified with acid refers to hydrochloric acid.
4. a kind of method of extracting root of langdu second element from euphorbia ebiacteolata Hayata according to claim 1, it is characterized in that: described silica gel particle particle diameter is the 200-300 order.
5. a kind of method of extracting root of langdu second element from euphorbia ebiacteolata Hayata according to claim 1, it is characterized in that: described recrystallization rearing crystal time is 4-6h.
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| CN201210340206.XA CN102898409B (en) | 2012-09-14 | 2012-09-14 | Method for extracting fischeriana B from Euphorbia ebracteolata Hayata |
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| CN201210340206.XA CN102898409B (en) | 2012-09-14 | 2012-09-14 | Method for extracting fischeriana B from Euphorbia ebracteolata Hayata |
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| CN102898409A true CN102898409A (en) | 2013-01-30 |
| CN102898409B CN102898409B (en) | 2015-04-15 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102702157A (en) * | 2012-05-24 | 2012-10-03 | 广东恒健制药有限公司 | Method for preparing 2,4-dihydroxy-6-methoxy-3-methylacetophenone with high purity |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102060827A (en) * | 2010-12-30 | 2011-05-18 | 苏州瑞蓝博中药技术开发有限公司 | Method for extracting new chamaejasmine B from stellera chamaejasme. L |
| CN102078444A (en) * | 2010-12-30 | 2011-06-01 | 苏州瑞蓝博中药技术开发有限公司 | Preparation method of Chinese stellera root total flavonoids |
-
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- 2012-09-14 CN CN201210340206.XA patent/CN102898409B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102060827A (en) * | 2010-12-30 | 2011-05-18 | 苏州瑞蓝博中药技术开发有限公司 | Method for extracting new chamaejasmine B from stellera chamaejasme. L |
| CN102078444A (en) * | 2010-12-30 | 2011-06-01 | 苏州瑞蓝博中药技术开发有限公司 | Preparation method of Chinese stellera root total flavonoids |
Non-Patent Citations (4)
| Title |
|---|
| NING ZHANG: "Two new cytotoxic acetophenone derivatives from Euphorbia ebracteolata Hayata", 《FITOTERAPIA》, vol. 81, no. 2010, 1 December 2009 (2009-12-01), pages 385 - 388 * |
| 张彦龙: "大戟狼毒中3,7,11-十三烯酸-4,8,12-三甲基甲酯的提取", 《哈尔滨商业大学学报》, vol. 18, no. 4, 30 August 2002 (2002-08-30), pages 462 - 464 * |
| 张霞: "狼毒乙素和新狼毒素A的药物代谢及动力学研究", 《浙江大学博士学位论文》, 31 May 2012 (2012-05-31), pages 386 * |
| 王文祥: "月腺大戟根中的乙酰间苯三酚类衍生物", 《药学学报》, vol. 34, no. 7, 30 December 1999 (1999-12-30), pages 514 - 517 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102702157A (en) * | 2012-05-24 | 2012-10-03 | 广东恒健制药有限公司 | Method for preparing 2,4-dihydroxy-6-methoxy-3-methylacetophenone with high purity |
| CN102702157B (en) * | 2012-05-24 | 2014-08-06 | 广东恒健制药有限公司 | Method for preparing 2,4-dihydroxy-6-methoxy-3-methylacetophenone with high purity |
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| CN102898409B (en) | 2015-04-15 |
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Inventor after: Du Shengyan Inventor after: Ren Chao Inventor after: Chen Jinkui Inventor after: Li Jinbu Inventor after: Xu Jie Inventor after: Zhao Qicang Inventor after: Zhao Wei Inventor after: Yang Tao Inventor after: Xie Zhongwei Inventor after: Ma Fei Inventor after: Xue Jianping Inventor after: Ma Shufang Inventor after: Zhu Dehui Inventor after: Sun Jiafeng Inventor before: Ding Yanbin Inventor before: Du Shengyan Inventor before: Zhao Wei Inventor before: Xue Jianping Inventor before: Li Jinbu Inventor before: Li Xueying |
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