Method for separating and purifying pimpinella anisum coumarin from Toddalia asiatica Lam and application of pimpinella anisum coumarin

A technology of anise coumarin and dragon's palm blood, applied in the field of natural medicinal chemistry

Inactive Publication Date: 2016-03-09
GUIYANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The patent applicant used flying dragon palm blood ( Toddalia asiatica (L.) Lam. ) root or root bark as raw material, crushed and extracted with ethanol solution, and then extracted with solvent system, the chloroform extraction layer was purifie

Method used

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  • Method for separating and purifying pimpinella anisum coumarin from Toddalia asiatica Lam and application of pimpinella anisum coumarin
  • Method for separating and purifying pimpinella anisum coumarin from Toddalia asiatica Lam and application of pimpinella anisum coumarin
  • Method for separating and purifying pimpinella anisum coumarin from Toddalia asiatica Lam and application of pimpinella anisum coumarin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Embodiment 1 (preparation of anise coumarin monomer):

[0033] (1) Take the blood from the flying dragon palm ( Toddalia asiatica (L.) Lam. ) root or root bark 6.0 kg, washed, dried, crushed and passed through 80-mesh sieve;

[0034] (2) Reflux extraction with 10 times the amount (60L) of 70% (v / v) ethanol for 3 times, each time for 1 hour;

[0035] (3) All the extracts were combined, filtered, and the filtrate was distilled under reduced pressure to remove the solvent to obtain 1.2 kg of ethanol extract. Add 2.4 kg of hot water at 60°C to the extract, stir and suspend to obtain a suspension;

[0036] (4) Extract three times with 2 times volume of petroleum ether, chloroform, ethyl acetate and n-butanol in sequence;

[0037] (5) Distill the solvent under reduced pressure respectively to obtain 281 g of chloroform extract, 46 g of ethyl acetate extract and 402 g of n-butanol extract;

[0038] (6) Take 281g of chloroform layer extract and transfer to AB-8 macroporous ...

Embodiment 2

[0045] Embodiment two (HPLC purity analysis):

[0046] The anise coumarin monomer obtained in Example 1 was used for HPLC determination.

[0047] (1) Chromatographic conditions

[0048] Column Diamonsil C 18 (250mm×4.6mm, 5μm)

[0049] Mobile phase methanol: 0.75% glacial acetic acid aqueous solution = 25:75

[0050] Isocratic elution

[0051] Flow rate 1.0mL / min Detection wavelength 320nm

[0052] Column temperature 25°C Injection volume 20μL

[0053] The HPLC chromatogram of anise coumarin under the above-mentioned chromatographic conditions is shown in Figure 4 .

[0054] (2) Sample preparation method

[0055] Take about 0.2g of the monomer, weigh it accurately, put it in a Erlenmeyer flask, add 70% ethanol for ultrasonic dissolution, filter, put the filtrate in a 100mL measuring flask, add 70% ethanol to the mark, shake well, and filter with a 0.45μm filter membrane , that is.

[0056] (3) Measurement results

[0057] The purity was measured by the peak area no...

Embodiment 3

[0058] Example 3 (open ODS column chromatography purification experiment):

[0059] The crude product of anise coumarin was dissolved in methanol and separated by open reverse phase ODS column chromatography. The ODS filler used was Chromatorex ODSDM1020T (FujiSilysia Chemical, Ltd., Aichi, Japan, 100-200 mesh), and 0.5% glacial acetic acid solution (v / v ) and methanol mixed solution for gradient elution, 5-8 retention volumes were collected for each gradient, followed by monitoring with TLC method, in which the 75:15 mixed solvent elution fraction was recrystallized to obtain the monomer, mass spectrometry, 1 H NMR and 13 C nuclear magnetic resonance and other techniques were used for structural identification, and the compound was determined to be pimpinellin.

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Abstract

The invention belongs to the field of natural pharmaceutical chemistry, and relates to a method for separating and purifying high-purity pimpinella anisum coumarin from Toddalia asiatica Lam and application of the pimpinella anisum coumarin to hemostatic activity. According to the method, a Toddalia asiatica Lam extract is used as raw material, and separation and purification are carried out through silica gel column chromatography, high performance liquid chromatography and recrystallization to obtain a high-purity pimpinella anisum coumarin monomeric compound, wherein the purity of the high-purity pimpinella anisum coumarin monomeric compound is above 98.0%. Pharmacodynamics studies show that the pimpinella anisum coumarin has good hemostatic effect which is similar to that of Yunnan Baiyao; and the method is simple and convenient in process, convenient to operate, high in monomer yield which is above 80%, feasible in industrial production and good in market prospect.

Description

technical field [0001] The invention belongs to the field of natural medicinal chemistry, and relates to a method for separating and purifying high-purity anise coumarin monomer from the blood of the ethnic medicine Feilongzhang and its hemostatic application. Background technique [0002] Feilongzhangxue is a plant of Rutaceae Feilongzhangxue Toddalia asiatica (L.) Lam. The dried root or root bark of the root is an ethnic medicine commonly used by ethnic minorities in Southwest China, and its chemical components are mainly concentrated in coumarins and alkaloids [1] , has analgesic, anti-inflammatory, antibacterial, antitumor and other biological activities. At present, a variety of simple coumarin components such as toddalolactone, coumurrayin, suberosin and phellopterin have been isolated from the blood of Feilongzhang [2] . [0003] The content of anise coumarin is relatively high in the blood of Feilongzhang. It has been reported in the literature that it has biolog...

Claims

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Application Information

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IPC IPC(8): C07D493/04A61K31/366A61P7/04
CPCC07D493/04Y02P20/54
Inventor 刘志刚谢晓林
Owner GUIYANG UNIV
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