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Method for preparing jionoside A1 from purple rehmannia

A technology of gionoside and purple rehmannia, which is applied in the field of separation of natural medicines, can solve the problems of undiscovered gionoside A1 research reports and the lack of gionoside A1, and achieves easy industrial preparation, reduced decomposition, and process operation simple effect

Inactive Publication Date: 2012-12-19
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] There are few studies on gionoside A1 in the prior art, and there is no research report on the extraction and isolation of high-purity geenoside A1 from natural plants.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Grind the root of purple rehmannia root, take 2kg, add 10 times of water, heat at 75°C and extract for 2 hours, filter, add 5 times of water, heat to 75°C for 1 hour, combine the extracts, cool to room temperature, filter, add MWCO 2000 Hollow cellulose membrane system ultrafiltration, add appropriate amount of water for dialysis, collect permeate and add hollow cellulose membrane system with a molecular weight cut-off of 500 to concentrate, add an equal volume of ethyl acetate to the concentrated solution to extract twice, and pass the extract through neutral alumina ( Particle size 120-200 mesh) short column, the column passes through the liquid to recover ethyl acetate to a small volume. Take chloroform-methanol-n-butanol-water, mix according to 6:5:3:5, take the upper phase and inject it into the chromatographic column as the stationary phase, turn on the high-speed countercurrent chromatograph, adjust the speed to 800r / min, inject the lower phase as the mobile phase...

Embodiment 2

[0018] Grind the root of purple rehmannia root, take 2kg, add 6 times of water, heat at 75°C for 1 hour, extract twice, cool the combined extract to room temperature, filter, add a hollow cellulose membrane system with a molecular weight cut-off of 6000 for ultrafiltration, add appropriate amount of water Dialyze, collect the permeate and add it to the hollow cellulose membrane system with a molecular weight cut-off of 500 to concentrate. Liquid recovery ethyl acetate to a small volume. Take chloroform-methanol-n-butanol-water, mix according to 4:3:1:3, take the upper phase and inject it into the chromatographic column as the stationary phase, turn on the high-speed countercurrent chromatography, adjust the speed to 900r / min, inject the lower phase as the mobile phase, After equilibrium, adjust the flow rate of the mobile phase to 1ml / min, inject samples, collect the gionoside A1 fraction, separate continuously, combine the fractions to concentrate, and dry under reduced press...

Embodiment 3

[0020] Grind the root of purple rehmannia root, take 2kg, add 6 times of water, heat at 75°C for 1 hour, extract 3 times, cool the combined extract to room temperature, filter, add hollow cellulose membrane system with a molecular weight cut-off of 2000 for ultrafiltration, add appropriate amount of water Dialysis, collect the permeate and add it to the hollow cellulose membrane system with a molecular weight cut off of 200 to concentrate. Liquid recovery ethyl acetate to a small volume. Take chloroform-methanol-n-butanol-water, mix according to 5:4:2:4, take the upper phase and inject it into the chromatographic column as the stationary phase, turn on the high-speed countercurrent chromatography, adjust the speed to 1000r / min, inject the lower phase as the mobile phase, After equilibration, adjust mobile phase flow rate 3ml / min, sample injection, collect gionoside A1 fraction, separate continuously, combine fraction and concentrate, dry under reduced pressure, obtain off-whit...

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Abstract

The invention discloses a method for preparing jionoside A1 from purple rehmannia. The method comprises the following steps of: smashing purple rehmannia root, adding the water of which the volume is 5-10 times of the volume of the smashed purple rehmannia root, heating to 60-75DEG C and extracting by means of heat preservation, filtering extracting solution, adding into an ultrafiltration membrane system for ultrafiltration, adding the penetrating fluid into a nanofiltration membrane system for nanofiltration, extracting the concentrated liquor by adding ethyl acetate, enabling the extract liquor to pass through an alumina column and concentrating, separating the extract liquor by high-speed counter-current chromatography, and drying flow components in a pressure reducing way, thus obtaining the jionoside A1. The method for preparing the jionoside A1 by a membrane separation technology and a high-speed counter-current chromatography separation technology provided by the invention is high in yield and low in pollution.

Description

technical field [0001] The invention belongs to the field of separation of natural medicines, in particular to a method for preparing gionoside A1 from purple rehmannia glutinosa. Background technique [0002] Jionoside A1 (Jionoside A1) is a phenylpropanoid glycoside compound, which is an active ingredient in Dihuang purple, and has a strong immunosuppressive effect. At a dose of 100mg / kg (oral), it inhibits the formation of hemolytic plaque-forming cells (HPFC) in the spleen of mice, with an inhibition rate of 23.0%. Geonoside A1, off-white amorphous powder, molecular formula C 36 h 48 o 20 , the molecular weight is 800.76, and the molecular structure is as follows: [0003] . [0004] Purple Rehmannia is a species of Scrophulariaceae (Scrophulariaceae) Rehmannia glutinosa Root of Libosch.var.purpurea Makino. [0005] In the prior art, there are few studies on gionoside A1, and there is no research report on the extraction and isolation of high-purity gionoside A...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/18C07H1/08
Inventor 刘东锋
Owner NANJING ZELANG MEDICAL TECH
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