Preparation method for toddalolactone

A technology of double-faced needle and aluminum oxide, which is applied in the biological field and can solve the problems of complex preparation methods, few disclosures, and low extraction efficiency

Inactive Publication Date: 2014-10-01
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Through literature search, the existing methods for preparing Maoliangzhen are less publicly disclosed, and more conventional reagents are used for extraction, the extraction efficiency is low, and the preparation method is complicated

Method used

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  • Preparation method for toddalolactone

Examples

Experimental program
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Effect test

Embodiment 1

[0013] Take Feilongzhang blood and crush it through an 80-mesh sieve, take 5kg and place it in a CO2 supercritical extraction tank for extraction, feed liquid CO2 with a flow rate of 3ml / min / g raw material, and simultaneously feed anhydrous methanol solution with a flow rate of 0.3ml / min / g raw material, extraction pressure 25Mpa, extraction temperature 45°C, extraction 90min, the extract obtained by analysis was dissolved in 85% methanol solution, added 400g basic aluminum alumina to dry and packed, followed by 10 times of column volume petroleum ether, 10 times of column volume Elute with volumetric ethanol solution, collect the ethanol solution to recover to 100ml, add 100ml chloroform, refrigerate and crystallize, filter out the crystals and recrystallize with absolute ethanol solution, dry to obtain 3.5g of ethanol with a content of 98.2%.

Embodiment 2

[0015] Take Feilongzhang blood and crush it through a 60-mesh sieve, take 5kg and place it in a CO2 supercritical extraction tank for extraction, feed liquid CO2 with a flow rate of 4ml / min / g raw material, and simultaneously feed anhydrous methanol solution with a flow rate of 0.2ml / min / g raw material, extraction pressure 18Mpa, extraction temperature 40°C, extraction 60min, the extract obtained by analysis was dissolved in 90% methanol solution, added 300g basic aluminum alumina to dry and packed, followed by 15 times of column volume petroleum ether, 10 times of column volume Elute with volumetric ethanol solution, collect the ethanol solution and recover to 80ml, add 50ml of chloroform, refrigerate and crystallize, filter out the crystals and recrystallize with absolute ethanol solution, dry to obtain 3.8g of staurein with a content of 98.2%.

Embodiment 3

[0017] Take Feilongzhang blood and crush it through a 40-mesh sieve, take 5kg and place it in a CO2 supercritical extraction tank for extraction, feed liquid CO2 at a flow rate of 1ml / min / g of raw materials, and simultaneously feed anhydrous methanol solution at a flow rate of 0.3ml / min / g raw material, extraction pressure 30Mpa, extraction temperature 50°C, extraction 120min, the extracted extract was dissolved with 90% methanol solution, added 350g basic aluminum alumina, dried and loaded into the column, followed by 10 times the column volume of petroleum ether, 10 times the column volume Elute with volumetric ethanol solution, collect the ethanol solution and recover to 80ml, add 80ml of chloroform, refrigerate and crystallize, filter out the crystals and recrystallize with absolute ethanol solution, dry to obtain 3.5g of staurein with a content of 98.1%.

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Abstract

The invention discloses a preparation method for toddalolactone. The method is as follows: (1) crushing asiatic toddalia root into 20-80 meshes, placing into a CO2 supercritical extracting tank for extracting, adding liquid-state CO2 with flow rate of 1-4ml / min / g of raw materials, introducing methanol liquor with flow rate of 0.1-0.4ml / min / g of raw materials, and analyzing to obtain extract with pressure of 18-30 Mpa and extracting time of 60-180 minutes; (2) dissolving the extract by methanol liquor and adding aluminum oxide for drying and packing, eluting by petroleum ether and alcohol liquor in sequence, collecting alcohol liquor to recycle small-size extract, adding proper amount of chloroform, refrigerating and crystallizing, re-crystallizing the crystal substances by alcohol liquor, and drying to obtain the toddalolactone. The method disclosed by the invention is high in extracting efficiency, simple in process operation, small in pollution, and suitable for producing high-purity toddalolactone.

Description

technical field [0001] The invention belongs to the field of biotechnology, and in particular relates to a method for preparing limpetin. Background technique [0002] Toddalolactone, also known as Feilongzhang blood ester, is a coumarin compound with a molecular formula of C16H20O6, a molecular weight of 308.33, and a molecular structural formula: [0003] [0004] Phyllostachysin exists in the plants of Rutaceae (Rutaceae) Zanthoxylum L. Zanthoxylum nitidum (Roxb.)DC.), Maoliangmianzhen ( Zanthoxylum nitidum var.fastuosum), Dragon Palm Blood ( Toddalia asiatica (L.) Lam. [Paullinia asiatica L.]). Through literature search, the existing methods for the preparation of Maoliangzhen are less publicized, and most of them are extracted with conventional reagents, the extraction efficiency is low, and the preparation method is complicated. Contents of the invention [0005] The technical problem to be solved by the present invention is to provide a high-efficiency, ea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/16
CPCC07D311/16Y02P20/54
Inventor 苏刘花
Owner NANJING ZELANG AGRI DEV
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