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Method for simultaneously preparing four drug effect components in Rhizoma Anemarrhenae

A technology for the simultaneous separation of medicinal ingredients, applied in the preparation of sugar derivatives, steroids, chemical instruments and methods, etc., can solve problems such as difficult simultaneous separation, difficult large-scale production, complex processes, etc., to improve resource utilization Efficiency, ease of large-scale production, and the effect of avoiding waste of resources

Inactive Publication Date: 2016-02-17
CHINA PHARM UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The macroporous adsorption resin technology can realize the total flavonoids (Duan Liangliang, etc., Chinese Medicine Research, 2009, 22 (9): 20-22) and total saponins (Chen Zhihong, etc., Applied Chemical Industry, 2008, 37) in Anemarrhena anemarrhena. 8): 841-843; Hu Yangye et al., World Science and Technology-Modernization of Traditional Chinese Medicine, 2012, 14(1): 1232-1236) enrichment; if the single compound timosaponin B-II, A is obtained by macroporous adsorption resin technology -III needs to be combined with silica gel column chromatography, countercurrent chromatography (Meng-ShunLiu, et.SeparationandPurificationTechnology138(2014)138-143), preparative liquid and other technologies to achieve purification, but it is difficult to achieve large-scale due to equipment limitations Production, while the cost is higher; there are also macroporous adsorption resins to separate and prepare timosaponin A-III (Li Zhixiong et al., Chinese patent medicine, 2013, 35 (2): 411-413), B-II (CN1693310A), but now There is a problem that there is only one component in the separation and preparation of the component, and there is no comprehensive preparation and utilization of other components, or the process is complicated, the production cost is high, and it is difficult to achieve large-scale production
It is difficult to realize the simultaneous separation of the four components of Anemarrhena, mangiferin, neomangiferin, timosaponin B-II and timosaponin A-III, through a single macroporous adsorption resin technology

Method used

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  • Method for simultaneously preparing four drug effect components in Rhizoma Anemarrhenae
  • Method for simultaneously preparing four drug effect components in Rhizoma Anemarrhenae
  • Method for simultaneously preparing four drug effect components in Rhizoma Anemarrhenae

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0070] Take 500g Anemarrhena medicinal material and crush it into 60 mesh powder, ultrasonically extract 5000mL of 50% ethanol twice, each time for 0.5h, filter with suction, combine the extracts, recover until there is no alcohol smell, add water to 3000ml, pass through 30 at a flow rate of 2BV / h -60-mesh polyamide column chromatography, followed by elution with 2 times column volume of 15% ethanol at a flow rate of 1BV / h, then eluted with 2 times column volume of 40% ethanol at a flow rate of 1BV / h, combined after loading For the effluent and 15% eluent, recover ethanol, add water to 1000mL, and record as sample 1; recover 40% ethanol to remove ethanol from the eluted part, add water to 2000mL to fully dissolve, and record as sample 2. Sample 1 passes through HPD-400 macroporous resin chromatography column with 2BV / h flow rate, uses 10% ethanol, 20% ethanol, 30% ethanol, 40% ethanol respectively with 1BV / flow rate elution of 1.5 times column volume, reclaims respectively 20 ...

Embodiment 2

[0072] Take 1000g Anemarrhena medicinal material and crush it into 60 mesh powder, reflux extract 10000mL of 70% ethanol twice, each time for 2h, filter with suction, combine the extracts, recover until there is no alcohol smell, add water to 4000ml, and pass through 60 -100 mesh polyamide column chromatography, followed by elution with 2 times column volume of 10% ethanol at a flow rate of 1BV / h, then eluted with 2 times column volume of 50% ethanol at a flow rate of 1BV( / h, combined and loaded After the effluent and 20% eluent, recover ethanol, add water to 2000mL, and record it as sample 1; recover 40% ethanol to remove ethanol from the eluted part, add water to 2000mL to fully dissolve, and record it as sample 2. Sample 1 uses a flow rate of 2BV / h The HPD-100 column chromatography that passed through was eluted with 10% ethanol, 20% ethanol, 30% ethanol, and 40% ethanol with a flow rate of 1BV / flow rate of 2 times the column volume, and the eluted sites of 20% ethanol and 4...

Embodiment 3

[0074]Take 1000g Anemarrhena decoction pieces and grind them into 10-mesh coarse powder, 8000mL of 70% ethanol reflux extraction twice, each time for 3h, filter with suction, combine the extracts, recover until there is no alcohol smell, add water to 4000ml, and pass through 800mL at a flow rate of 2BV / h 30-60 mesh polyamide column chromatography, continued to elute with 2 times column volume of 20% ethanol at a flow rate of 1BV / h, then eluted with 2 times column volume of 50% ethanol at a flow rate of 1BV / h, combined After sampling the effluent and 20% eluent, recover ethanol, add water to 2000mL, and record as sample 1; recover 50% ethanol to remove ethanol from the eluted part, add water to 2000mL to fully dissolve, and record as sample 2. Sample 1 passes through the D-101 resin chromatography column at a flow rate of 2BV / h, and is eluted with 10% ethanol, 20% ethanol, 30% ethanol, and 40% ethanol at a flow rate of 1BV / h with 2 times the column volume respectively, and 20% e...

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Abstract

The invention discloses a method for simultaneously separating and preparing main chemical components neomangiferin, mangiferin, timosaponin BII and timosaponin AIII in Rhizoma Anemarrhenae. The above four components can be effectively separated and prepared through combining polyamide and macro-porous adsorption resin and through carrying out segmented collection. The method has the advantages of environmental protection, repeated use of resin and polyamide, low production, realization of the purity of above prepared samples reaching 90% or above, and realization of large scale production.

Description

technical field [0001] The present invention relates to the technical field of traditional Chinese medicine pharmacy, and relates to a method for simultaneously preparing four medicinal components in Anemarrhena, in particular to the realization of new mangiferin, mangiferin, and timosaponin BII in Anemarrhena by using two kinds of separation materials in combination. Preparation and separation of timosaponin AIII. Background technique [0002] Zhimu is the dry rhizome of Anemarrhena asphodeloides Bge., a plant of Liliacea. It has the effects of clearing away heat and purging fire, promoting body fluid and moistening dryness. Diabetes, intestinal dryness and constipation. Modern pharmacological studies have shown that it has hypoglycemic, anti-senile dementia, anti-tumor, anti-pathogenic microorganisms, anti-platelet aggregation, hypoglycemic, antipyretic, and anti-inflammatory physiological activities (Xu Aijuan et al., Chinese Medicinal Materials, 2008, 31(4): 624 -628; ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/04C07H1/08C07D407/04C07J71/00C07J75/00
Inventor 李萍李会军年四辉
Owner CHINA PHARM UNIV