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Preparation method of mexicanin I

A technology of chrysanthemum and gradient, which is applied in the field of medicine, can solve the problems of literature and patent reports on a large number of methods for preparing chrysanthemum Ⅰ, and achieve easy large-scale production, large extraction driving force, and high resolution Good results

Inactive Publication Date: 2013-01-09
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] After searching, there are no literature and patent reports on a large number of methods for preparing moxijuning Ⅰ

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Extract 10kg of the dry aerial part of Gamania mexicanus in a flash extractor at room temperature with 5 times the amount of 50% acetone solution for 3 times, each time for 10min, combine the extracts, concentrate under reduced pressure to an extract, and use the ratio Carry out 15-stage countercurrent extraction for an 8:2 ethyl acetate-methanol mixed solution, combine the extracts, recover the solvent under reduced pressure, add water to the obtained extract, and absorb it through a pretreated macroporous adsorption resin column. Elute with 15% ethanol solution until the effluent is colorless, then elute with 75% ethanol solution by volume until the effluent is colorless, collect the 75% ethanol eluate to recover ethanol under reduced pressure, concentrate and dry to obtain sample. Weigh 200-300 meshes of activated silica gel and add it to a stainless steel chromatography column with an inner diameter of 80mm and a diameter-to-height ratio of 1:20. Add methanol to the...

Embodiment 2

[0022] Extract 10kg of the dry aerial part of Gamania mexicanus in a flash extractor at room temperature with 8 times the amount of 65% acetone solution for 4 times, each time for 20min, combine the extracts, concentrate under reduced pressure to an extract, and use the ratio Perform 10-stage countercurrent extraction for an 8:2 ethyl acetate-methanol mixed solution, combine the extracts, recover the solvent under reduced pressure, add water to the obtained extract, and absorb it through a pretreated macroporous adsorption resin column. Elute with 15% ethanol solution until the effluent is colorless, then elute with 80% ethanol solution by volume until the effluent is colorless, collect the 80% ethanol eluate to recover ethanol under reduced pressure, concentrate and dry to obtain sample. Weigh 200-300 meshes of activated silica gel and add it to a stainless steel chromatography column with an inner diameter of 100mm and a diameter-to-height ratio of 1:15. Add the above-mentio...

Embodiment 3

[0024] Extract 10 kg of the dry aerial part of Ruthia japonica in a flash extractor at room temperature with 5 times the amount of 70% acetone solution for 3 times, each time for 15 minutes, combine the extracts, concentrate under reduced pressure to an extract, and use a ratio of The 8:2 ethyl acetate-methanol mixed solution was used for 12-stage countercurrent extraction, the extracts were combined, the solvent was recovered under reduced pressure, the obtained extract was dispersed with water, and adsorbed by a pretreated macroporous adsorption resin column. Elute with 15% ethanol solution until the effluent is colorless, then elute with 65% ethanol solution by volume until the effluent is colorless, collect the 65% ethanol eluate to recover ethanol under reduced pressure, concentrate and dry to obtain the sample . Weigh 200-300 meshes of activated silica gel and add it to a stainless steel chromatography column with an inner diameter of 150mm and a diameter-to-height ratio...

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PUM

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Abstract

The invention relates to a preparation method of mexicanin I. The preparation method comprises the technological steps as follows: getting overground part of plant rich in mexicanin I, cracking tissue with acetone, and extracting; concentrating extract liquid under reduced pressure to obtain an extract; carrying out multi-grade counter-current extraction with ethyl acetate-methanol mixed solvent based on ratio of 8: 2; combining the extracting liquids; and recovering the solvent under reduced pressure; subjecting to macroporous absorption resin column; concentrating eluant to obtain crude product; sampling to middle-pressure chromatographic column with silica gel of 200 to 300 meshes; carrying out gradient elution with mixed organic solvent; collecting mexicanin I fraction; and concentrating under reduced pressure; and drying at low temperature to obtain mexicanin I. With the adoption of the preparation method provided by the invention, mexicanin I is high in purity, and easy to be industrially expanded.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a method for preparing moxijuning I. Background technique [0002] Mexieanin Ⅰ (Mexieanin Ⅰ), the molecular formula is C 15 h 18 o 4 , with a molecular weight of 262.31, is a sesquiterpene lactone compound with a CAS accession number of 5945-41-5. Prismatic (chloroform-methanol), mp.257-260°C. Ubiquitous in natural plants, mainly distributed in a variety of plants in the Compositae family, such as Mexican chervil gamanga, bitter chrysanthemum, Mexican chrysanthemum, jaundice leaf chrysanthemum, pilose scapula membranous chrysanthemum and other plants. Pharmacological studies have found that Moxijuning Ⅰ has anti-ulcer effect, and also has certain cytotoxic activity. [0003] After searching, there are no literature and patent reports on a large number of methods for preparing mexijuning I. Contents of the invention [0004] The purpose of the present inventi...

Claims

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Application Information

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IPC IPC(8): C07D307/93
Inventor 苏刘花
Owner NANJING ZELANG AGRI DEV
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