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Catalpol preparation method

A catalpol and nanofiltration membrane technology, which is applied in the field of natural medicinal chemistry, can solve the problems of product dead adsorption, large amount of reagents, and high cost, and achieve the effects of high solvent utilization, high product yield, and simple operation

Inactive Publication Date: 2013-08-07
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the serious dead adsorption of the product due to the separation of the silica gel column, the amount of reagents is large, and it is difficult to reproduce the industrial scale-up, resulting in the high production cost of the existing high-purity catalpol
However, the preparation of liquid phase production, the output is small, the cost is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Grind 10kg of fresh rehmannia glutinosa, squeeze the juice, add an equal volume of 95% ethanol to the obtained juice, fully stir, centrifuge, add the centrifugate to a nanofiltration membrane with a molecular cut-off of 200 to concentrate, and spray dry the concentrate to obtain 430g of crude extract, take 4000ml of ethyl acetate The ester was fully dissolved, filtered, the filtrate was passed through a neutral alumina column, and the column solution was concentrated to obtain 35 g of extract. Mix ethyl acetate, methanol, and water in a ratio of 3:1:3, and after fully stratified, take the upper phase and inject it into a high-speed countercurrent chromatography tube as the stationary phase, start the host at a speed of 900 rpm, and pump the lower phase as the mobile phase at the same time. After equilibrium, set the flow rate to 2ml / min, and dissolve the concentrated solution with mobile phase at the same time, inject it into a high-speed countercurrent chromatograph, an...

Embodiment 2

[0019] Grind 10kg of fresh rehmannia glutinosa, squeeze the juice, add an equal volume of 95% ethanol to the resulting juice, fully stir, centrifuge, concentrate the centrifugate with a nanofiltration membrane with a molecular cut-off of 300, and spray dry the concentrated solution to obtain 340g of crude extract, take 3000ml of ethyl acetate The ester was fully dissolved, filtered, the filtrate was passed through a neutral alumina column, and the column solution was concentrated to obtain 27 g of extract. Mix ethyl acetate, methanol, and water in a ratio of 5:2:7, and after fully stratified, take the upper phase and inject it into a high-speed countercurrent chromatography tube as the stationary phase, start the host at a speed of 800 rpm, and pump the lower phase as the mobile phase at the same time. After equilibrium, set the flow rate to 3ml / min, and dissolve the concentrated solution with mobile phase at the same time, inject it into a high-speed countercurrent chromatogra...

Embodiment 3

[0021] Grind 10kg of fresh rehmannia glutinosa, squeeze the juice, add an equal volume of 95% ethanol to the resulting juice, stir well, centrifuge, add the centrifugate to a nanofiltration membrane with a molecular cut-off of 200 to concentrate, spray the concentrated solution to obtain 450g of crude extract, take 3000ml of ethyl acetate The ester was fully dissolved, filtered, the filtrate was passed through a neutral alumina column, and the next column was concentrated to obtain 31 g of extract. Mix ethyl acetate, methanol, and water in a ratio of 6:2:9, and after fully stratified, take the upper phase and inject it into a high-speed countercurrent chromatography tube as the stationary phase, start the host at a speed of 700 rpm, and pump the lower phase as the mobile phase at the same time. After equilibrium, set the flow rate to 1ml / min, and dissolve the concentrated solution with mobile phase at the same time, inject it into a high-speed countercurrent chromatograph, dete...

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Abstract

The invention discloses a simple and efficient catalpol preparation method. The simple and efficient catalpol preparation method comprises the following steps of: a. smashing fresh radix rehmanniae, juicing, adding the same volume of 95% alcohol to obtained juice, fully stirring, centrifuging, concentrating centrifugate by a nanofiltration membrane, and carrying out spray drying on a concentrated solution to obtain a crude extract; b. adding the crude extract to ethyl acetate and completely dissolving; filtrating, processing filtrate by an aluminium oxide column, purifying a reagent, which is recycled from liquid processed by column, by adopting high-speed counter-current chromatography, carrying out online monitoring by an ultraviolet detector, collecting a target component according to an atlas, recovering the reagent, and drying under reduced pressure to obtain the catalpol. The simple and efficient catalpol preparation method has the advantages that the process operation is simple, the product yield is high, and the industrial amplification is easy.

Description

technical field [0001] The invention belongs to the field of natural medicinal chemistry, in particular to a method for preparing catalpol. Background technique [0002] Catalpol is an iridoid glycoside, molecular formula C 15 h 22 o 10 , molecular weight 362.33, CAS number 2415-24-9, structural formula: [0003] . [0004] Catalpol is an active ingredient in Rehmannia Scrophulariaceae, which has physiological activities such as anti-cancer, neuroprotective, anti-inflammatory, diuretic, hypoglycemic and anti-hepatitis virus. [0005] The existing methods for preparing high-purity catalpol use silica gel column separation or preparative liquid phase separation. For example, the method disclosed in the patent (application number: 200810016005.8) "Method for Separating Catalpol from Fresh Rehmannia Rehmanniae" is to crush and homogenize fresh Rehmannia glutinosa to obtain a sample solution containing catalpol; to separate it with a macroporous adsorption resin, and to a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/04C07H1/08
Inventor 刘东锋杨成东
Owner NANJING ZELANG MEDICAL TECH
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