A kind of preparation method of total diterpenes of Ruixiang lupus poison

A technology of lupus radix and total diterpenes is applied in the field of preparation of total diterpenes of lupus radix to achieve the effects of enhancing separation ability, reducing sample volume and reducing decomposition.

Active Publication Date: 2019-11-12
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

And so on, there are many reports on the pharmacological effects of Daphne chamaejasme diterpene in the literature, but there are few reports on its extraction and preparation methods, which shows that it is of great significance to engage in research in this area

Method used

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  • A kind of preparation method of total diterpenes of Ruixiang lupus poison
  • A kind of preparation method of total diterpenes of Ruixiang lupus poison
  • A kind of preparation method of total diterpenes of Ruixiang lupus poison

Examples

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Effect test

Embodiment 1

[0022] Take 1 kg of Rhizoma chamaejasma, crush it into a coarse powder, put it in an extraction kettle, add 8L of absolute ethanol to soak for 2 hours, then decoct in a water bath at 50°C for 3 times under reduced pressure, condense and reflux for 2 hours each time. Afterwards, the extracts were combined for 3 times, and dried under negative pressure to obtain 115 g of extract. After ultrasonically dispersing the extract with 0.6L of pure water, add 1.2L of ethyl acetate to the separatory funnel for extraction, and repeat 3 times. Afterwards, the water layer was removed, and the combined ethyl acetate layers were evaporated to dryness under negative pressure to obtain 66 g of extract. After dispersing the extract with 70mL of 80% methanol-water solution, load the sample by wet method, pass through a 40-50μm ODS reverse-phase chromatography column (column length 40cm, inner diameter 8cm), and then fully elute with 80% and 95% methanol-water solution, Pressurize with a medium-p...

Embodiment 2

[0030] Take 2kg of Rhizoma chamaejasma, crush it into coarse powder, put it in an extraction kettle, add 13L of absolute ethanol to soak for 2 hours, then decoct it in a water bath at 55°C for 3 times under reduced pressure, condense and reflux for 2 hours each time. After that, the extracts were combined for 3 times and dried under negative pressure to obtain 227 g of extract. After ultrasonically dispersing the extract with 1.4L of pure water, add 3L of ethyl acetate to the separatory funnel for extraction, and repeat 3 times. Afterwards, the water layer was removed, and the combined ethyl acetate layers were evaporated to dryness under negative pressure to obtain 134 g of extract. After dispersing the extract with 140mL 80% methanol-water solution, load the sample by wet method, pass through a 40-50μm ODS reverse-phase chromatography column (column length 40cm, inner diameter 8cm), and fully elute with 80% and 95% methanol-water solution in sequence , pressurized by a medi...

Embodiment 3

[0032] Take 2 kg of Rhizoma chamaejasma, crush it into a coarse powder, put it in an extraction kettle, add 15L of absolute ethanol to soak for 2 hours, decoct in a water bath at 60°C for 3 times under reduced pressure, condense and reflux for 3 hours each time. Afterwards, the extracts were combined for 3 times and dried under negative pressure to obtain 231 g of extract. After ultrasonically dispersing the extract with 2L of pure water, add 4L of ethyl acetate to the separatory funnel for extraction, and repeat 3 times. Afterwards, the water layer was removed, and the combined ethyl acetate layers were evaporated to dryness under negative pressure to obtain 145 g of extract. After dispersing the extract with 150mL 80% methanol-water solution, load the sample by wet method, pass through a 40-50μm ODS reverse-phase chromatography column (column length 40cm, inner diameter 8cm), and fully elute with 80% and 95% methanol-water solution in sequence , pressurized by a medium-pres...

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Abstract

The invention discloses a method for preparing total diterpenes of Daphne chamaejasme, belonging to the technical field of plant extraction. The total diterpenes in Daphne chamaema were obtained by three steps of ethanol extraction, ethyl acetate extraction and reversed-phase medium pressure column chromatography. The diterpene content in the prepared Daphne chamaejasme total diterpenes is as high as 90%. The method adopts a reverse-phase ODS column, which is eluted with 80% and 95% methanol solutions in sequence, effectively removes non-diterpene impurities, and has a reasonable process, and the method is low in cost, simple in operation steps, easy to scale up, and is very suitable for large-scale Production.

Description

technical field [0001] The invention belongs to the technical field of plant extraction, and relates to a method for preparing total diterpenes in Daphne chamaejasme, in particular to a method for extracting and preparing total diterpenes in Daphne chamaejasme by combining extraction technology and reversed-phase ODS column chromatography technology . Background technique [0002] Stellerachamaejasme (Stellerachamaejasme L.) is a plant of the genus Stellerachamaejasme in the family Stelleraceae. It is commonly known as chrysanthemum and is distributed in China, Russia, Mongolia, North Korea and other countries. Dry and sunny alpine grass slopes, lawns or river beach terraces. It is bitter and pungent in taste, flat in nature, and highly toxic. It enters the lung, spleen and liver meridians, and its roots are used as medicine. Modern pharmacological studies have shown that Daphne chamaejasma has good antitumor activity, and the latest research has also found that it has ant...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): A61K36/83
CPCA61K36/83A61K2236/33A61K2236/331A61K2236/333A61K2236/39A61K2236/51A61K2236/55
Inventor 肖红斌王志鑫洪志来
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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