CN102327317A - Preparation method of rabdosia japonica total diterpene - Google Patents
Preparation method of rabdosia japonica total diterpene Download PDFInfo
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- CN102327317A CN102327317A CN201110263982A CN201110263982A CN102327317A CN 102327317 A CN102327317 A CN 102327317A CN 201110263982 A CN201110263982 A CN 201110263982A CN 201110263982 A CN201110263982 A CN 201110263982A CN 102327317 A CN102327317 A CN 102327317A
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- rabdosia japonica
- total diterpene
- rabdosia
- diterpene
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Abstract
The invention discloses a preparation method of rabdosia japonica total diterpene. In the method, total diterpene is extracted from rabdosia japonica by extracting with a solvent and enriching with macroporous resin. The preparation method comprises the following steps of: crushing rabdosia japonica leaves into coarse powder; adding a solvent for extracting; cooling a combined extracting solution and filtering; adding active carbon into the filtrate for decoloring; making the decolored solution pass through an ultrafiltration film of 3,000-10,000 dalton; adsorbing the permeate liquid with pretreated macroporous resin; eluting with an ethanol aqueous solution; and concentrating and drying the obtained eluent to obtain rabdosia japonica total diterpene. The method has the advantages of easiness for operating, low energy consumption, high product quality and the like, and is suitable for industrial production.
Description
Technical field
The invention belongs to the Natural Medicine Chemistry field, relate to a kind of method for preparing of Rabdosia japonica total diterpene.
Background technology
Rabdosia japonica
Rabdosia japonica(Burm.f.) Hara var.glau-cocalyxi (Maxin) Hara is a Labiatae Rabdosia plant; Have another name called Herba Rabdosiae glaucocalycis, be widely distributed in northern China, for a long time; China is among the people as Rabdosia japonica (Burm. f.) Hara usefulness, have be good for the stomach, heat-clearing and toxic substances removing, invigorate blood circulation, anti-inflammation and active anticancer.Rabdosia japonica also has the myocardium protecting action relevant with dosage.Its chemical constituent is mainly diterpene and triterpenoid compound.Shen Xiaodan etc. separate chemical compounds such as obtaining glaucocalyxin, Glaucocalyxin B, blue calyx third element, oleanolic acid, ursolic acid, canophyllal, suberone from Rabdosia japonica.Wherein glaucocalyxin, Glaucocalyxin B, blue calyx third element, Glaucocalyxin D, blue calyx penta element, the own element of blue calyx belong to the Kaurane diterpine compounds; Zhang Bin etc. find that through pharmacological research glaucocalyxin has remarkable inhibition ADP; AA, inductive rabbit platelet such as PAF is assembled.One Chinese patent application number 200910044882.0 employing mtt assay; With A549, LOVO, 6T-CEM, HL-60 cell strain glaucocalyxin, Glaucocalyxin B, blue calyx third element, Glaucocalyxin D, blue calyx penta element, the own element of blue calyx have been carried out the cytotoxic activity experiment; Find that they all have significant cytotoxic activity, can be used for preparing cancer therapy drug.One Chinese patent application number 200910044883.6 employing hepatitis B surface antigen (HBsAg) diagnostic kits and HBcAg (HBeAg) diagnostic kit have carried out anti-hepatitis B surface antigen and HBcAg test to above-mentioned Rabdosia japonica diterpene-kind compound; Find that they all have significant anti-hepatitis B activity, can be used for preparing the medicine of hepatitis B virus.
In the prior art, the method for from the medical material Rabdosia japonica, extracting diterpene-kind compound adopts the method separation and purification of organic solvent extraction, silica gel column chromatography more, and there are defectives such as separation cycle length, cost height in this method.
Summary of the invention
Rabdosia japonica total diterpene according to the invention is the mixture of the diterpene-kind compound of extraction separation from the Rabdosia japonica leaf.
The method for preparing that the purpose of this invention is to provide a kind of Rabdosia japonica total diterpene.
The objective of the invention is to realize through following technical scheme:
A kind of method for preparing of Rabdosia japonica total diterpene is characterized in that: the Rabdosia japonica leaf is ground into coarse powder, is that extraction solvent extracts with ethanol or methanol; With the extracting solution cooled and filtered that merges, filtrating adds active carbon stirs, filters, and it is 1.05-1.12 that destaining solution is concentrated into relative density; Through the daltonian hollow fiber ultrafiltration membrane of 3000-10000, operating pressure is 0.1-0.3MPa again, and permeate is through the good absorption with macroporous adsorbent resin of pretreatment; Earlier use water elution, again with 30-70% ethanol water eluting, the eluting consumption is 3-6BV; Elution flow rate is 0.5-2BV/h, and the eluent concentrate drying that obtains promptly gets the Rabdosia japonica total diterpene.
The percent by volume of said extraction solvent ethanol or methanol is 60-95%, and method for distilling is that reflux, extract,, Suo Shi extract, dipping extracts, percolation extracts, one or more combinations of microwave extraction.
Said active carbon is a medicinal carbon, and addition is the 0.5-2% of medical material amount, and bleaching temperature is 50-60 ℃.
That the inventive method has is simple to operate, energy consumption is low, the product quality advantages of higher, is fit to suitability for industrialized production.
The specific embodiment
Embodiment 1:
The Rabdosia japonica leaf is ground into coarse powder, takes by weighing 1kg and place extraction pot, 70% methanol that adds 6 times of amounts carried out heating and refluxing extraction 2 hours, extracted 2 times; Merging extracted twice liquid is put cold, filters, and filtrating adds 1% medicinal carbon heated and stirred, filters; It is 1.08 that decolorization filtering liquid is concentrated into relative density, is that the adjustment operating pressure is 0.2MPa in the 6000 daltonian hollow fiber ultrafiltration membrane systems through molecular cut off again, collects permeate; Permeate is splined on the good macroporous adsorptive resins of pretreatment, after the saturated absorption, water, 60% ethanol elution successively; Collect 60% ethanol elution, rotary evaporation concentrates, and is drying to obtain the Rabdosia japonica total diterpene; The content of total diterpene class is 76%, detects through HPLC, and glaucocalyxin, Glaucocalyxin B, blue calyx third element, Glaucocalyxin D, blue calyx penta element, oneself plain content sum of blue calyx are 46%.
Embodiment 2:
The Rabdosia japonica leaf is ground into coarse powder, takes by weighing 1kg and place extraction pot, 80% ethanol that adds 10 times of amounts carried out microwave extraction 1 hour, extracted 3 times; Merge three extracting solution and put coldly, filter, filtrating adds 1.5% medicinal carbon heated and stirred, filters; It is 1.12 that decolorization filtering liquid is concentrated into relative density, is that the adjustment operating pressure is 0.1MPa in the 10000 daltonian hollow fiber ultrafiltration membrane systems through molecular cut off again, collects permeate; Permeate is splined on the good macroporous adsorptive resins of pretreatment, after the saturated absorption, water, 70% ethanol elution successively; Collect 70% ethanol elution, rotary evaporation concentrates, and is drying to obtain the Rabdosia japonica total diterpene; The content of total diterpene class is 72%, detects through HPLC, and glaucocalyxin, Glaucocalyxin B, blue calyx third element, Glaucocalyxin D, blue calyx penta element, oneself plain content sum of blue calyx are 43%.
Embodiment 3:
The Rabdosia japonica leaf is ground into coarse powder, takes by weighing 2kg and place extraction pot, 60% ethanol that adds 7 times of amounts carries out percolation and extracts, and is light to the percolate complexion changed; The collection extracting solution is put cold, filters, and filtrating adds 2% medicinal carbon heated and stirred, filters; It is 1.05 that decolorization filtering liquid is concentrated into relative density, is that the adjustment operating pressure is 0.3MPa in the 3000 daltonian hollow fiber ultrafiltration membrane systems through molecular cut off again, collects permeate; Permeate is splined on the good macroporous adsorptive resins of pretreatment, after the saturated absorption, water, 30% ethanol elution successively; Collect 30% ethanol elution, rotary evaporation concentrates, and is drying to obtain the Rabdosia japonica total diterpene; The content of total diterpene class is 61%, detects through HPLC, and glaucocalyxin, Glaucocalyxin B, blue calyx third element, Glaucocalyxin D, blue calyx penta element, oneself plain content sum of blue calyx are 40%.
Embodiment 4:
The Rabdosia japonica leaf is ground into coarse powder, takes by weighing 5kg and place extraction pot, 95% methanol that adds 8 times of amounts carries out Suo Shi and extracted 3 hours, extracts 3 times; Merge three extracting solution and put coldly, filter, filtrating adds 0.5% medicinal carbon heated and stirred, filters; It is 1.10 that decolorization filtering liquid is concentrated into relative density, is that the adjustment operating pressure is 0.25MPa in the 4000 daltonian hollow fiber ultrafiltration membrane systems through molecular cut off again, collects permeate; Permeate is splined on the good macroporous adsorptive resins of pretreatment, after the saturated absorption, water, 45% ethanol elution successively; Collect 45% ethanol elution, rotary evaporation concentrates, and is drying to obtain the Rabdosia japonica total diterpene; The content of total diterpene class is 65%, detects through HPLC, and glaucocalyxin, Glaucocalyxin B, blue calyx third element, Glaucocalyxin D, blue calyx penta element, oneself plain content sum of blue calyx are 48%.
Embodiment 5:
The Rabdosia japonica leaf is ground into coarse powder, takes by weighing 5kg and place extraction pot, 75% methanol that adds 10 times of amounts floods and extracted 12 hours, filters; 75% methanol of 8 times of amounts of filtering residue reuse floods and extracted 8 hours, and merging extracted twice liquid is put cold, filters; Filtrating adds 1% medicinal carbon heated and stirred, filters, and it is 1.09 that decolorization filtering liquid is concentrated into relative density; Be that the adjustment operating pressure is 0.15MPa in the 8000 daltonian hollow fiber ultrafiltration membrane systems through molecular cut off again, collect permeate; Permeate is splined on the good macroporous adsorptive resins of pretreatment, after the saturated absorption, water, 50% ethanol elution successively; Collect 50% ethanol elution, rotary evaporation concentrates, and is drying to obtain the Rabdosia japonica total diterpene; The content of total diterpene class is 73%, detects through HPLC, and glaucocalyxin, Glaucocalyxin B, blue calyx third element, Glaucocalyxin D, blue calyx penta element, oneself plain content sum of blue calyx are 44%.
Claims (3)
1. the method for preparing of a Rabdosia japonica total diterpene, it is characterized in that: the Rabdosia japonica leaf is ground into coarse powder, is that extraction solvent extracts with ethanol or methanol; With the extracting solution cooled and filtered that merges, filtrating adds active carbon stirs, filters, and it is 1.05-1.12 that destaining solution is concentrated into relative density; Through the daltonian hollow fiber ultrafiltration membrane of 3000-10000, operating pressure is 0.1-0.3MPa again, and permeate is through the good absorption with macroporous adsorbent resin of pretreatment; Earlier use water elution, again with 30-70% ethanol water eluting, the eluting consumption is 3-6BV; Elution flow rate is 0.5-2BV/h, and the eluent concentrate drying that obtains promptly gets the Rabdosia japonica total diterpene.
2. the method for preparing of a kind of Rabdosia japonica total diterpene as claimed in claim 1; The percent by volume that it is characterized in that said extraction solvent ethanol or methanol is 60-95%, and method for distilling is that reflux, extract,, Suo Shi extract, dipping extracts, percolation extracts, one or more combinations of microwave extraction.
3. the method for preparing of a kind of Rabdosia japonica total diterpene as claimed in claim 1 is characterized in that said active carbon is a medicinal carbon, and addition is the 0.5-2% of medical material amount, and bleaching temperature is 50-60 ℃.
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| CN201110263982A CN102327317A (en) | 2011-09-08 | 2011-09-08 | Preparation method of rabdosia japonica total diterpene |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103989740A (en) * | 2014-05-04 | 2014-08-20 | 苏州大学 | Application of rabdosia japonica in preparing anti-acute lung injury drugs |
| CN111153972A (en) * | 2018-11-07 | 2020-05-15 | 上海医药集团股份有限公司 | Isodon glaucocalyx glycoprotein XPS10-1, and preparation method and application thereof |
| CN111153971A (en) * | 2018-11-07 | 2020-05-15 | 上海医药集团股份有限公司 | Isodon glaucocalyx glycoprotein XPS5-1, and preparation method and application thereof |
| CN112047995A (en) * | 2020-09-24 | 2020-12-08 | 深圳市天同玩具有限公司 | Tea saponin draws equipment |
-
2011
- 2011-09-08 CN CN201110263982A patent/CN102327317A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103989740A (en) * | 2014-05-04 | 2014-08-20 | 苏州大学 | Application of rabdosia japonica in preparing anti-acute lung injury drugs |
| CN103989740B (en) * | 2014-05-04 | 2017-06-06 | 苏州大学 | Application of the rabdosia japonica in resisting acute lung injury medicine is prepared |
| CN111153972A (en) * | 2018-11-07 | 2020-05-15 | 上海医药集团股份有限公司 | Isodon glaucocalyx glycoprotein XPS10-1, and preparation method and application thereof |
| CN111153971A (en) * | 2018-11-07 | 2020-05-15 | 上海医药集团股份有限公司 | Isodon glaucocalyx glycoprotein XPS5-1, and preparation method and application thereof |
| CN111153971B (en) * | 2018-11-07 | 2023-04-07 | 上海医药集团股份有限公司 | Isodon glaucocalyx glycoprotein XPS5-1, and preparation method and application thereof |
| CN111153972B (en) * | 2018-11-07 | 2023-04-07 | 上海医药集团股份有限公司 | Isodon glaucocalyx glycoprotein XPS10-1, and preparation method and application thereof |
| CN112047995A (en) * | 2020-09-24 | 2020-12-08 | 深圳市天同玩具有限公司 | Tea saponin draws equipment |
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Application publication date: 20120125 |