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Method for preparing baliospermin

A kind of cannabinoid and ethyl acetate technology, applied in the direction of organic chemistry, etc., to achieve the effect of high extraction rate, low energy consumption and low cost

Inactive Publication Date: 2015-01-07
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In the prior art, there is no report on the preparation process applicable to the industrialized large-scale production of canthidin

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Take 2 kg of the root of the root of the plant and cut it into small pieces, then put it into a high-speed tissue masher, keep it at 10,000 rpm for 10 minutes, add 6 kg of water, and then add 0.5% cellulase. Enzymolysis for 30 minutes, then drying at 65°C, adding 8L of 60% ethanol to heat and reflux for extraction once, extracting for 2 hours, collecting the extract, filtering, recovering the ethanol from the filtrate under reduced pressure, and using n-butanol-water with a volume ratio of 10:1 The mixed solution was subjected to 5-stage countercurrent extraction, the extracts were combined, the reagent was recovered under reduced pressure, and the concentrated solution was added to the magnesium oxide column chromatography (the ratio of concentrated solution to magnesium oxide was 1:3), and the volume ratio of n-hexane-ethyl acetate was 5 : 1, 3: 1, 1: 1, 1: 3 for gradient elution, the amount of each gradient is 400ml, the combined canthoridine fractions are collected, ...

Embodiment 2

[0018] Take 2 kg of the root of the mountain spot seed and cut it into small pieces, then put it into a high-speed tissue grinder, keep it at 10,000 rpm for 10 minutes, add 6 kg of water, and then add 0.5% cellulase. Enzymolysis for 30 minutes, then drying at 70°C, adding 10L of 70% ethanol to heat and reflux extraction for 3 times, extracting for 1.5 hours, collecting the extract, filtering, recovering the ethanol from the filtrate under reduced pressure, and using n-butanol with a volume ratio of 10:1- The water mixed solution is subjected to 6-stage countercurrent extraction, the extracts are combined, the reagent is recovered under reduced pressure, and the concentrated solution is added to the magnesium oxide column chromatography (the ratio of concentrated solution to magnesium oxide is 1:5), and the volume ratio of n-hexane-ethyl acetate is 5:1, 3:1, 1:1, 1:3 for gradient elution, the amount of each gradient is 400ml, the combined canthoridine fraction is collected, conc...

Embodiment 3

[0020] Take 2 kg of the root of the safflower seed and cut it into small pieces, then put it into a high-speed tissue grinder, keep it at 10,000 rpm for 10 minutes, add 10 kg of water, and then add 0.5% cellulase. Enzymolysis for 30 minutes, then drying at 75°C, adding 6L of 65% ethanol to heat and reflux for extraction twice, extracting for 2 hours, collecting the extract, filtering, recovering the ethanol from the filtrate under reduced pressure, and using n-butanol-water with a volume ratio of 10:1 The mixed solution was subjected to 5-stage countercurrent extraction, the extracts were combined, the reagents were recovered under reduced pressure, and the concentrated solution was added to magnesium oxide column chromatography (the ratio of the concentrated solution to magnesium oxide was 1:4), and the volume ratio of n-hexane-ethyl acetate was 5 :1, 3:1, 1:1, 1:3 for gradient elution, the amount of each gradient is 400ml, the pooled canthidin fractions were collected, concen...

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Abstract

The invention discloses a method for preparing baliospermin. The method comprises the following steps: by using roots of baliospermum montanum root as a raw material, firstly separating substances to be extracted from the raw material by virtue of a method of tissue crushing, cellulase enzymolysis and ultrasonic extraction; and then, carrying out multi-stage counter current extraction and magnesium oxide chromatographic technique on a normal butanol-water mixed solution to separate and extract the baliospermin. The method disclosed by the invention has the characteristics of high extraction ratio, simple operating process, low energy consumption, low cost and the like.

Description

technical field [0001] The invention belongs to the field of traditional Chinese medicine chemistry and relates to a method for preparing canthidin. Background technique [0002] Baliospermin, the molecular formula is C32H50O8, the molecular weight is 562.74, and the structural formula is [0003] [0004] Spotted element comes from the root of Euphorbiaceae (Euphorbiaceae) mountain spot seed Baliospermum montanum (Willd.) Muell.-Arg. Caterpillar has anti-cancer effects. For P388 lymphocytic leukemia at 0.2 mg / kg in vivo, T / C was 131. The ED50 of P388 in vitro was 0.6 μg / mL. [0005] In the prior art, there is no report on the preparation process applicable to the large-scale industrial production of canthidin. Contents of the invention [0006] The purpose of the present invention is to provide a method for preparing canthoselin, which has high extraction rate, simple operation process, low energy consumption and low cost. [0007] To achieve the above object, the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D301/32C07D303/32
CPCC07D301/32C07D303/32
Inventor 刘东锋杨成东
Owner NANJING ZELANG MEDICAL TECH
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