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Method for separating macranthoidin from lonicerae flos

A technology of honeysuckle saponin B and mountain silver flower, which is applied in the field of natural medicinal chemistry, can solve the problems of serious loss of samples separated by silica gel column, unsuitability for industrial production, and large amount of reagents, and achieve continuous preparation, small amount of solvent, large amount of preparation

Inactive Publication Date: 2013-08-28
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Moreover, the loss of samples separated by silica gel column is serious, the amount of reagent is large, the operation is complicated, and it is not suitable for industrial production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Take 500g of mountain silver flower raw material, soak and extract with 7 times the amount of saturated lime water for 3 times, soak for 3 hours each time, combine the extract solution with hydrochloric acid solution to adjust neutrality, add ultrafiltration membrane ultrafiltration with a molecular weight cut-off of 2000 after filtration, and the permeate Concentrate by nanofiltration with a hollow cellulose membrane with a cut-off of 1000, add 95% ethanol to the concentrated solution for precipitation, centrifuge, and concentrate the liquid under reduced pressure to obtain an extract. Take ethyl acetate, n-butanol and water and mix them in a ratio of 3:1:3. After fully layering, take the upper phase as the stationary phase and fill the high-speed countercurrent chromatography tube, turn the host at 800 rpm, and pump the lower phase as the mobile phase. After dynamic balance, the flow rate is adjusted to 2ml / min, and the extract is dissolved with the mobile phase at the...

Embodiment 2

[0019] Take 500g of mountain silver flower raw material, soak and extract 3 times with 5 times the amount of saturated lime water, soak for 2 hours each time, combine the extract solution with hydrochloric acid solution to adjust neutrality, add ultrafiltration membrane ultrafiltration with a molecular weight cut-off of 3000 after filtration, and the permeate Concentrate by nanofiltration with a hollow cellulose membrane with a cut-off of 800, add 95% ethanol to the concentrated solution for precipitation, centrifuge, and concentrate the liquid under reduced pressure to obtain an extract. Take ethyl acetate, n-butanol and water, and mix them in a ratio of 5:2:7. After fully layering, take the upper phase as the stationary phase and fill the high-speed countercurrent chromatography tube, turn the host at 900 rpm, and pump the lower phase as the mobile phase. After dynamic equilibrium, the flow rate was adjusted to 3ml / min, and the extract was dissolved with the mobile phase at t...

Embodiment 3

[0021] Take 1000g of mountain silver flower raw material, soak and extract 2 times with 8 times the amount of saturated lime water, soak for 3 hours each time, combine the extract solution with hydrochloric acid solution to adjust neutrality, add ultrafiltration membrane ultrafiltration with molecular weight cut off 2000 after filtration, and permeate Concentrate by nanofiltration with a hollow cellulose membrane with a cut-off of 600, add 95% ethanol to the concentrated solution for precipitation, centrifuge, and concentrate the liquid under reduced pressure to obtain an extract. Take ethyl acetate, n-butanol and water, and mix them in a ratio of 9:2:7. After fully layering, take the upper phase as the stationary phase and fill the high-speed countercurrent chromatography tube, turn the host at 850 rpm, and pump the lower phase as the mobile phase. After dynamic equilibrium, the flow rate was adjusted to 3ml / min, and the extract was dissolved with the mobile phase at the same ...

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Abstract

The invention discloses an efficient and simple method for separating macranthoidin from lonicerae flos. The method comprises the following steps of: a, soaking and extracting lonicerae flos material, using saturated lime water, the amount of which is 5-8 times that of the lonicerae flos material adjusting the extract liquor to neutral, adding to an ultra-filtration membrane for carrying out ultra-filtration after filtering, concentrating permeate by a sodium filtration membrane, adding alcohol to the concentrated solution for precipitating and centrifuging, and concentrating the liquid under reduced pressure to obtain extract; and b, purifying the extract by adopting high-speed counter-current chromatography, carrying out online monitoring by an ultraviolet detector, collecting target components according to a graph, recycling the reagent, and drying under reduced pressure to obtain the macranthoidin. The method for producing macranthoidin is adopted, so that the process is simple, the yield is high, the pollution is small and the industrial expansion is easy.

Description

technical field [0001] The invention belongs to the field of natural medicinal chemistry, and in particular relates to a method for isolating Lonicerae saponin B from Lonicera japonica. Background technique [0002] High-speed countercurrent chromatography is a continuous and efficient liquid-liquid partition chromatography separation technology, which does not require any solid support or carrier. It uses a two-phase solvent system to establish a special unidirectional hydrodynamic equilibrium in a high-speed rotating helical tube. When one of the phases is used as a stationary phase and the other as a mobile phase, it can be retained during continuous elution. A large number of stationary phases. Since there is no need for a solid support, the separation of substances is achieved based on the difference in their distribution coefficients in the two phases, thus avoiding sample loss, inactivation, denaturation, etc. caused by irreversible adsorption. The sample can better...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00C07H15/256C07H1/08
Inventor 刘东锋杨成东
Owner NANJING ZELANG MEDICAL TECH
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