Separation method for simultaneously preparing five dopamine compounds from aspongopus

A separation method, the technology of Jiuxiangworm, applied in the separation/purification of carboxylic acid amide, organic chemistry, etc., can solve the problems of low yield, too many types of solvents, complicated technical solutions, etc., achieve high separation efficiency and prolong the use of instruments Cycle time, effect of reducing sample volume

Active Publication Date: 2020-02-21
ZUNYI MEDICAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This patent also uses Jiuxiang insect as a raw material, but only obtains a dopamine compound monomer, the technical scheme is complicated, there are too many types of solvents involved, and the yield is low, so further in-depth research cannot be done

Method used

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  • Separation method for simultaneously preparing five dopamine compounds from aspongopus
  • Separation method for simultaneously preparing five dopamine compounds from aspongopus

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Embodiment 1

[0030] 1. Grind 1Kg of the dried chrysanthemum worm into a coarse powder of 1-5mm, add 5L of 70% ethanol solution, ultrasonically extract 3 times, the ultrasonic time is 60min, 45min, 30min, combine the extract 15L, filter, 60 °C and concentrated in vacuo to no purity, about 2L of solution. Add 800ml of petroleum ether, ethyl acetate, and n-butanol in sequence, extract each solvent 3 times, combine the n-butanol solution, about 2.5L, concentrate in vacuo at 60°C to 200ml, add 200g of 200-mesh silica gel to mix the sample, and perform a silica gel column Chromatography, chloroform-methanol gradient elution, collect 1 / 5-1 / 1 eluted fraction, concentrate to about 100ml, add 50ml of methanol, filter with 0.45μm organic membrane; inject the filtrate to prepare and separate the compound monomer, and Targeted collection of each component greater than 98.0%, combined the same fractions, during this process, the detection wavelength of the ultraviolet detector was set at 280nm, and comp...

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Abstract

The invention discloses a separation method for simultaneously preparing five dopamine compounds from aspongopus, and belongs to the technical field of separation and purification of compound monomers. According to the method, dried aspongopus is used as a raw material, and the five dopamine compound monomers are obtained at the same time through the steps of ethanol extraction, vacuum concentration, step-by-step extraction, silica gel column enrichment and elution, efficient preparative liquid chromatography separation and product recovery; a foundation is laid for deeply researching the medicinal value of the aspongopus medicinal material and the synthesis and development of a new drug, and meanwhile, the development and utilization of traditional aspongopus resources are also facilitated.

Description

technical field [0001] The invention relates to a method for separating and purifying animal compound monomers, in particular to a method for simultaneously preparing five kinds of dopamine compounds from jiuxiang worm, and belongs to the technical field of traditional Chinese medicine. Background technique [0002] This product is stinkbug insect Cotidius chinensis The dry body of Dallas, also known as fart worms, fart worms, fart worms, etc., is distributed in most parts of southern my country and some South Asian countries. As a medicinal and edible insect, Jiuxiang worm was first recorded in "Compendium of Materia Medica". It is a traditional Chinese medicine recorded in the 2015 edition of "Chinese Pharmacopoeia". Insufficient yang. Domestic researchers believe that the nine-scented worm has antibacterial, anti-coagulant, and thrombus-dissolving effects, and has a certain inhibitory effect on cancer cells. However, not many active ingredients have been clearly identi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/24C07C233/18C07D311/60C07D319/20
CPCC07C231/24C07D311/60C07D319/20C07C233/18Y02A50/30
Inventor 侯晓晖徐天天
Owner ZUNYI MEDICAL UNIVERSITY
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