Method for preparing diphyllin

A technology of lotus leaf and lotus leaf, which is applied in the field of preparation of lotus leaf, can solve the problems of cumbersome operation, low extraction rate, serious sample loss, etc., and achieve the advantages of less solvent consumption, high product purity and short production cycle Effect

Inactive Publication Date: 2012-01-04
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] There are few domestic reports on the preparation of lotus leaf element. Zhang Yongli used alcohol extraction, solvent extraction and various column chromatography to separate and purify the monomer components repeatedly. The operation is cumbersome and the sample loss is serious, so it is not suitable for industrial production.
Chinese patent (Application No. 201010535341.0) discloses a method of ethanol thermal reflux, ethyl acetate-water mixed solvent multi-stage countercurrent extraction, macroporous resin column chromatography, and acetone crystallization to prepare safflower. The extraction rate of this method is low, Unstable process
In the prior art, there is no process report on the separation and purification of lotus leaf by high-speed countercurrent chromatography

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Take the alcoholic extract of the leaves of the southern lotus leaf and dissolve it with 95% ethanol, apply Sephadex LH-20 gel column chromatography, and use dichloromethane-methanol mixed solvent gradient elution, that is, dichloromethane-methanol volume ratio is 10: 1. The mixed solvent of 8:11, 6:1, 4:1, 2:1 was used for elution, and the eluted part containing lindenolin was collected and concentrated by rotary evaporation under reduced pressure to obtain a concentrated solution, which was then separated by high-speed countercurrent chromatography For the concentrated solution, put the solvent system n-hexane-ethyl acetate-methanol-water in a separatory funnel at a volume ratio of 1:0.5:1:0.7 at room temperature and shake it, place it, take the upper and lower phases respectively, and separate the upper phase As the stationary phase, the lower phase is used as the mobile phase. Pump the stationary phase into the chromatographic column. After the column is filled with ...

Embodiment 2

[0015] Take the alcoholic extract of the leaves of the southern lotus leaf and dissolve it with 95% ethanol, apply Sephadex LH-20 gel column chromatography, and use dichloromethane-methanol mixed solvent gradient elution, that is, dichloromethane-methanol volume ratio is 10: 1. The mixed solvent of 8:11, 6:1, 4:1, 2:1 was used for elution, and the eluted part containing lindenolin was collected and concentrated by rotary evaporation under reduced pressure to obtain a concentrated solution, which was then separated by high-speed countercurrent chromatography For the concentrated solution, put the solvent system n-heptane-ethyl acetate-methanol-water at room temperature in a volume ratio of 1:0.7:1:0.7 in a separatory funnel and shake it, place it, take the upper and lower phases respectively, and put the upper The phase is used as the stationary phase, and the lower phase is used as the mobile phase. The stationary phase is pumped into the chromatographic column. After the colum...

Embodiment 3

[0017] Take the alcoholic extract of the leaves of the southern lotus leaf and dissolve it with 95% ethanol, apply Sephadex LH-20 gel column chromatography, and use dichloromethane-methanol mixed solvent gradient elution, that is, dichloromethane-methanol volume ratio is 10: 1. The mixed solvent of 8:11, 6:1, 4:1, 2:1 was used for elution, and the eluted part containing lindenolin was collected and concentrated by rotary evaporation under reduced pressure to obtain a concentrated solution, which was then separated by high-speed countercurrent chromatography For the concentrated solution, put the solvent system n-heptane-ethyl acetate-ethanol-water at room temperature in a volume ratio of 1:0.6:1:0.9 in a separatory funnel and shake it, place it, take the upper and lower phases respectively, and put the upper The phase is used as the stationary phase, and the lower phase is used as the mobile phase. The stationary phase is pumped into the chromatographic column. After the column...

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PUM

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Abstract

The invention discloses a method for preparing diphyllin. The method comprises the step of carrying out separation on ethanol extracts of Diphylleia sinensis or rostellularia procumbens by combining gel column chromatography and high speed counter-current chromatography so as to prepare the diphyllin. According to the invention, the purity of the diphyllin obtained by the method can reach above 97%, and the method has the characteristics of large preparation amount, less solvent consumption, high product purity, short production period and the like.

Description

technical field [0001] The invention belongs to the field of extraction and preparation of effective active ingredients of traditional Chinese medicines, and relates to a method for preparing chrysanthemum leaf element. Background technique [0002] Diphyllin is a recently discovered natural product with a new structure that has anti-tumor activity. Molecular formula: C 21 h 16 o 7 , Molecular weight: 380.353, belonging to 4-benzo-2,3-naphtholactones. It is mainly extracted and isolated from various plants such as Acanthaceae, Berberidaceae, and Rutaceae. Pharmacological studies have shown that Diphyllin has good antitumor activity, and its ED50 for human nasopharyngeal carcinoma cells (KB) is less than 3 μmol / mL. Studies have found that Diphyllin compounds can act on the S phase and G1 phase of the cell division cycle, making cell division stay in the G1 phase, and have a strong inhibitory effect on the S phase. Experiments have shown that when used in HCT116 cells, wi...

Claims

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Application Information

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IPC IPC(8): C07D407/04
Inventor 刘东锋郭琴
Owner NANJING ZELANG MEDICAL TECH
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