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Method for preparing crotepoxide from caulis piperis kadsurae leaves

A technology of fenugreek and sea breeze vine is applied in the field of astrobiology, can solve the problems of low sample yield, cumbersome operation, unsuitable for mass production and the like, and achieves the effects of high product yield and simple process operation.

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

The existing process is cumbersome to operate, the sample yield is low, and it is not suitable for mass production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Take 5kg of sea breeze vine leaves and crush them, use 6 times the volume of 60% ethanol solution for microwave extraction for 3 times, and ultrasonic for 10 minutes each time, after recovering ethanol from the extract, add it to D101 macroporous resin for adsorption, and elute with 5 times column volume of 75% ethanol solution , the eluate was concentrated to a density of 1.03, and then extracted with ethyl acetate, the extract was passed through a neutral alumina (120 mesh) column, and the reagent was recovered from the column to obtain an extract. Take chloroform, methanol, and water, and mix them in a ratio of 6:5:5. 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, pump the lower phase into the mobile phase, and wait for dynamic equilibrium , the flow rate was adjusted to 2ml / min, the concentrated solution was dissolved in the mobile phase, the sample was injected,...

Embodiment 2

[0020] Take 5kg of sea breeze vine leaves and crush them, use 7 times the volume of 70% ethanol solution for microwave extraction twice, ultrasonic for 15 minutes each time, after recovering ethanol from the extract, add it to HZ816 macroporous resin for adsorption, and elute with 4 times the column volume of 80% ethanol solution , the eluate was concentrated to a density of 1.02, and then extracted with ethyl acetate, the extract was peracidized alumina (180 mesh) column, and the reagent was recovered from the column liquid to obtain the extract. Take chloroform, methanol, and water and mix them in a ratio of 15:9:8. After fully stratifying, 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, the concentrated solution was dissolved in the mobile phase, the sample was injected, the ultravi...

Embodiment 3

[0022] Take 5kg of sea breeze vine leaves and crush them, use 4 times the volume of 90% ethanol solution for microwave extraction for 3 times, ultrasonic for 10 minutes each time, after recovering ethanol from the extract, add it to AB-8 macroporous resin for adsorption, and use 6 times the column volume of 70% ethanol solution For elution, the eluate was concentrated to a density of 1.01, then extracted with ethyl acetate, the extract was passed through a neutral alumina (120 mesh) column, and the reagent was recovered from the column to obtain an extract. Take chloroform, methanol, and water, and mix them in a ratio of 9:7:6. 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 2ml / min, the concentrated solution was dissolved in the mobile phase, the sample was injected, the ...

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PUM

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Abstract

The invention discloses an efficient method for preparing crotepoxide from caulis piperis kadsurae leaves. The method comprises the following steps of: A, crushing caulis piperis kadsurae leaves for, carrying out microwave extraction twice to three times by using 40%-90% alcohol solution, the amount of which is 5-10 times that of caulis piperis kadsurae leaves (each time being 10 minutes-20 minutes), recycling alcohol from the extract liquor and then adding to macroporous resin for adsorbing, eluting by using 70%-90% of alcohol solution, and concentrating the eluant to obtain a concentrated solution; and B, extracting the concentrated solution by ethyl acetate, penetrating the extract liquor through an alumina column, purifying lower column liquor recycling agent 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 crotepoxide. The method for producing crotepoxide is adopted, so that the process is simple and industrial expansion is easy to realize.

Description

technical field [0001] The invention belongs to the technical field of natural organisms, and in particular relates to a method for preparing betelene from leaves of vine leaves. Background technique [0002] Pinotiflorin, Molecular Formula C 18 h 18 o 8 , molecular weight 362.33, CAS number 20421-13-0, molecular structure [0003] I . [0004] Seawind Teng is a plant of the family Piperaceae. Its stems and leaves contain Echinoside, Echinotenone, Echinoquinone, and Echinoside amide. Betone has the highest content and has the effect of suppressing tumors. [0005] Through searching, it is found that the preparation methods of echinoside are mostly obtained by silica gel column separation or preparative liquid phase separation, such as the literature "Study on the components of the ethyl acetate part and the volatile oil part of Caulis chinensis". The existing process is cumbersome to operate, the sample yield is low, and it is not suitable for mass production. Cont...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/04
Inventor 刘东锋杨成东
Owner NANJING ZELANG MEDICAL TECH
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