A kind of preparation method of momordin Ib

An aqueous solution, column chromatography technology, applied in the direction of steroids, organic chemistry, etc., can solve the problems of inability to meet the application, difficult to realize the industrial production of momordinIb, etc., and achieve the effect of achieving a large amount of acquisition and simple separation and purification operations.

Active Publication Date: 2021-11-26
XISHUANGBANNA TROPICAL BOTANICAL GARDEN CHINESE ACAD OF SCI +1
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  • Application Information

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Problems solved by technology

[0006] It can be seen from the above-mentioned published documents that the currently disclosed preparation methods of momordin Ib are difficult to realize the industrial production of momordin Ib no matter whether it is directly extracted from plants or chemically synthesized, and cannot meet its requirements in the fields of biology, medicine or health care. application

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  • A kind of preparation method of momordin Ib
  • A kind of preparation method of momordin Ib
  • A kind of preparation method of momordin Ib

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preparation example Construction

[0037] The invention provides a kind of preparation method of momordin Ib, comprising:

[0038] 1) Mixing the plant extract containing the triterpene saponin derivative of the structural unit of formula (I) or the plant extract of the triterpene saponin derivative of the structural unit of formula (I) with acid to obtain the extract,

[0039]

[0040] Among them, R 1 , R 2 , R 3 , R 4 independently selected from polysaccharide groups, five-carbon sugar groups or six-carbon sugar groups connected to each other by hydrogen, five-carbon sugars and / or six-carbon sugars, and R 1 , R 2 , R 3 , R 4 not simultaneously hydrogen;

[0041] 2) adjusting the pH of the extract in step 1) to 6.5-7.5 with alkali, and then separating by column chromatography to obtain a sample containing momordin Ib;

[0042] 3) The obtained sample containing momordin Ib is recrystallized to obtain the pure product of momordin Ib.

[0043] According to the present invention, the present invention w...

Embodiment 1

[0054] Take 10kg of dried light-leaved flower branches and leaves plant samples rich in triterpene saponin derivatives (including but not limited to compounds such as momordin Ic) with structural units of formula (I), cross 20 mesh sieves after crushing, add 30 liters of 0.05Mol / L Heat dilute sulfuric acid aqueous solution to reflux and extract 3 times (9, 1, 1 hour), filter the extract while it is hot, combine the 3 extracts and adjust the pH value to 7.0 with dilute NaOH lye, then put it on the medical activated carbon (1000g) column, Elute 30 column volumes with water and 40% ethanol aqueous solution, recover the ethanol in the obtained eluent and discard the impurities, then elute 10 column volumes with 85% ethanol aqueous solution, combine the eluents and recover ethanol , to obtain 43.4 g of a momordin Ib sample with a mass content of 42%. After dissolving 43.4g mass content 42% momordin Ib sample, mix sample with the alumina of mass ratio 1: 1, go up alumina (1085g) col...

Embodiment 2

[0058] Take 10kg of dry light-leaved flower branches and leaves plant samples rich in triterpene saponin derivatives (including but not limited to compounds such as momordin Ic) possessing the structural unit of formula (I), cross 20 mesh sieves after pulverizing, add 30 liters of 0.12Mol / L trifluoroacetic acid aqueous solution heated and refluxed for 3 times (9, 1, 1 hour), filtered the extract while it was hot, combined the 3 extracts and adjusted the pH value to 7.0 with dilute NaOH lye, then applied D101 macroporous resin (10kg ) column, eluted 30 column volumes with water and 40% ethanol aqueous solution successively, reclaimed ethanol in the eluent obtained and discarded this part of impurities, then eluted 40 column volumes with 50% ethanol aqueous solution, and combined the eluted parts Liquid and reclaim ethanol, obtain mass content 51% momordin Ib sample 46g. After 46g mass content 51% momordin Ib sample is dissolved, mix sample with the alumina of mass ratio 1: 1, ...

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Abstract

The present invention provides a kind of preparation method of momordin Ib, by at first the plant that contains the triterpene saponin derivative of formula (I) structural unit or the plant extract that contains the triterpene saponin derivative of formula (I) structural unit and acid Mixing the reaction to obtain an extract, then adjusting the pH of the extract in step 1) to 6.5 to 7.5 with alkali, and then separating by column chromatography to obtain a sample containing momordin Ib; Crystallized to obtain pure momordin Ib. Among them, the present invention uses plants or plant extracts rich in triterpene saponin derivatives with structural units of formula (I) as raw materials for preparing momordin Ib. It was found that the method not only has simple separation and purification operations, but also can realize momordin Ib A large amount is obtained, and the solvents eluted and recrystallized in each step can be recycled many times, which is suitable for industrial production.

Description

technical field [0001] The invention relates to the field of organic synthesis, medicine or functional food, in particular to a preparation method of momordin Ib. Background technique [0002] Momordin Ib is triterpene saponin, CAS No. 26020-14-4, molecular formula C 36 h 56 o 9 , molecular weight 632, chemical structural unit as shown in formula (II): [0003] [0004] Momordin Ib is an important active ingredient in medicinal plants such as Panax japonicas, Calendula officinalis, Acanthopanax gracilistylus and Paris polyphylla var.yunnanensis. It has anti-inflammatory, Anti-platelet aggregation, hypoglycemic and anti-tumor and other biological activities. [0005] At present, there are mainly two kinds of preparation methods about Momordin Ib, extracting from plants and chemical synthesis:) directly extracting from plants, such as existing disclosures from plants such as Achyranthes bidentata and Salicorniaeuropaea Direct extraction and purification to obtain momor...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J63/00
CPCC07J63/008C07J9/00C07J63/00
Inventor 张玉梅李佳李静雅臧奕孙一立
Owner XISHUANGBANNA TROPICAL BOTANICAL GARDEN CHINESE ACAD OF SCI
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