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Method for extracting catalpol from rehmannia stem

A technology of rehmannia glutinosa and catalpol, applied in the field of medicine, can solve the problems of cumbersome process, high production cost, and high process cost, and achieve the effects of overcoming technical prejudice, saving industrial cost, and reducing the amount of solvent used

Inactive Publication Date: 2013-01-09
苏州玉森新药开发有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, there are some reports about how to extract catalpol from rehmannia glutinosa in existing literature, as: (1) patent 200710026330.8 adopts rehmannia glutinosa extract to pass through activated carbon column, macroporous resin column, cationic resin column, anion resin column, Nanofiltration membrane separation and purification of catalpol, its defect is more loaded down with trivial details process, high production cost, practicality is not strong; After impurity, separate and purify by macroporous resin, discard 0-50% ethanol eluent, collect 80% ethanol eluting part, finally use methanol-ethanol crystallization to obtain pure catalpol, and its defect is that catalpol is water soluble , the process adopts ethanol extraction, which not only has high cost but also low yield, and collects 80% ethanol elution site, which is inconsistent with the good water solubility of catalpol; Methanol elution silica gel column, the disadvantage is that the process cost is high and complicated, and the practicability is not strong; (4) The macroporous resin AB-8 / ADS-7 involved in the process of purifying catalpol in the patent 200910264454.9 is eluted with 30% ethanol to remove impurities , collect 70-80% of the elution site and use ethyl acetate to crystallize catalpol. The defect is that catalpol has good water solubility and poor solubility in ethyl acetate.
The defects in the above-mentioned patents will lead to poor industrial practicability, or the extraction of catalpol is not high in purity
[0005] The current prior art is to extract rehmannia root or fresh rehmannia root, and no process for extracting catalpol from rehmannia stems has been found.

Method used

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  • Method for extracting catalpol from rehmannia stem
  • Method for extracting catalpol from rehmannia stem
  • Method for extracting catalpol from rehmannia stem

Examples

Experimental program
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Embodiment 1

[0066] Take the rehmannia stem coarse powder, add 12 times the amount of water to 20.0 kg, extract under reflux for 2 times, 1 hour each time, combine the extracts, concentrate under reduced pressure to a relative density of 1.14 (50 ° C), add 95% by volume ratio 1:4 Ethanol was allowed to stand overnight, the supernatant was concentrated under reduced pressure to a relative density of 1.08 (50°C), the concentrated solution was allowed to cool, and an XAD-16 macroporous resin column was added (amount ratio of 1:4, diameter to height ratio of 1:10), First eluted with 2BV water, then eluted with 2.2BV of 6% ethanol, collected the 6% ethanol eluent, concentrated under reduced pressure to a thick paste, mixed with 50-100 mesh silica gel, evaporated to dryness, and added 100-200 mesh silica gel Column (amount ratio of 1:15), eluted with ethyl acetate / methanol 4:1, collected the target fraction, concentrated under reduced pressure, dried, the dried material was recrystallized with 85...

Embodiment 2

[0069] Take the rehmannia stem coarse powder, add 12 times the amount of water to 20.0 kg, extract under reflux for 2 times, 1 hour each time, combine the extracts, concentrate under reduced pressure to a relative density of 1.15 (50 ° C), add 100% by volume ratio 1:3 Ethanol, left standing overnight, the supernatant was concentrated under reduced pressure to a relative density of 1.13 (50°C), the concentrated solution was allowed to cool, and an XAD-16 macroporous resin column was added (amount ratio of 1:4, diameter to height ratio of 1:7), First eluted with 1BV water, then eluted with 3BV of 3% ethanol, collected the 3% ethanol eluent, concentrated under reduced pressure to a thick paste, mixed with 100-200 mesh silica gel, evaporated to dryness, and added a 100-200 mesh silica gel column (the dosage ratio is 1:20), eluted with ethyl acetate / methanol 5:1, collected the target fraction, concentrated under reduced pressure, dried, the dried material was recrystallized with 80%...

Embodiment 3

[0072] Take the rehmannia stem coarse powder, add 12 times the amount of water to 50kg, extract under reflux for 2 times, 1 hour each time, combine the extracts, concentrate under reduced pressure to a relative density of 1.16 (50°C), add 90% ethanol at a volume ratio of 1:5 , left standing overnight, the supernatant was concentrated under reduced pressure to a relative density of 1.10 (50°C), the concentrated solution was allowed to cool, and an XAD-16 macroporous resin column was added (amount ratio 1:4, diameter-height ratio 1:5), first Elute with 1.5BV water, then eluate with 1.5BV 10% ethanol, collect the 10% ethanol eluent, concentrate under reduced pressure to a thick paste, stir in 50-100 mesh silica gel, evaporate to dryness, add 50-100 mesh silica gel Column (amount ratio of 1:5), eluted with ethyl acetate / methanol 3:1, collected the target fraction, concentrated under reduced pressure, dried, the dried material was recrystallized with 95% ethanol, filtered and dried ...

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Abstract

The invention relates to a method for extracting catalpol from rehmannia stem, which belongs to the medicine technical field. The method comprises the following steps: 1) rehmannia stem and water are heated for backflow extraction, an extract is performed pressure reduction and concentration to obtain a concentrate A; 2) 95% of ethanol is added in the concentrate A, standing is carried out for overnight, a supernate is performed pressure reduction and concentration to obtain a concentrate B; 3) a concentrate B is led to a XAD-16 macroporous resin column, elution is carried out by water, then elution is carried out by ethanol, an ethanol eluate is collected, the pressure reduction and concentration are carried out to obtain a stiff paste; 4) silica gel is added in the stiff paste, dried and a silica gel column is added, elution is carried out by ethyl acetate / methanol according to ratio of 4:1, a target fraction is collected, the pressure reduction, concentration and drying processes are carried out; 5) recrystallization is carried out on a dried object, the processes of filtering and drying are carried out to obtain the catalpol pure product. Compared with the prior art, the method of the invention has the characteristics of strong industrialization operationality, high extraction efficiency, resource preservation and environmental protection.

Description

technical field [0001] The invention relates to a method for extracting catalpol from the stem of Chinese medicine rehmannia glutinosa, belonging to the technical field of medicine. Background technique [0002] In 1962, W.H. Lunn et al. first isolated catalpa glycoside from the fresh fruit of the catalpa tree Catalpa ovata, then hydrolyzed catalpaline, and obtained catalpol after recrystallization of the hydrolyzed product. This is the earliest report of catalpol. In 1965, R.B.Duff et al. used activated carbon and diatomaceous earth as fillers. After multiple column chromatography and finally recrystallized with water, they isolated naturally occurring catalpol for the first time from the leaves of Buddleia globosa. [0003] In 1971, Kitagawa Isao and others in Japan studied the hypoglycemic components of Rehmannia glutinosa. They separated R-BP-F, an effective component with significant hypoglycemic effect, from Huaiqing Rehmannia glutinosa. Separation by column chromatog...

Claims

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Application Information

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IPC IPC(8): C07H17/04C07H1/08
Inventor 玄振玉黄孝春
Owner 苏州玉森新药开发有限公司
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