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Method for extracting and purifying Nazlinin

An extraction and alumina technology, applied in organic chemistry, bulk chemical production, etc., can solve the problems of low total alkaloid content and low yield of Nitraria japonica, and achieve the effects of stable process, low operating temperature and mild operating conditions

Inactive Publication Date: 2012-07-18
江苏博益生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there are few studies on the phytochemical components of Nitraria genus. Li Fangqun et al. extracted 3 times with 95% ethanol for 2 hours each time. The yield was low, and the total alkaloid content of Nitraria was low.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Pulverize the aboveground part of Dongyan, pass through a 20-mesh sieve, weigh 10kg and add it to the extraction kettle, turn on the machine, and adjust the parameters: the temperature of the extraction kettle is 37°C, the pressure of the extraction kettle is 20MPa, the temperature of the separation kettle I is 58°C, and the pressure is 8MPa , the temperature of the separation tank II is 55°C, the pressure is 5MPa, and CO is fed at a flow rate of 18kg / L 2 Extract for 2 hours, analyze the extract, adjust the pH to 8.5 with ammonia water, then add chloroform for extraction several times, collect and combine the chloroform extracts, concentrate under reduced pressure and add alumina medium pressure column (200-300 mesh neutral alumina, column diameter High ratio is 1:7), followed by elution according to the volume ratio of dichloromethane-methanol 20:1, 10:1, 5:1, 7:3, TLC tracking detection, collecting high concentration fractions, recovering reagents, drying The crude pr...

Embodiment 2

[0017] Pulverize the aboveground part of Dongyan, pass through a 20-mesh sieve, weigh 10kg and add it to the extraction kettle, turn on the machine, and adjust the parameters: the temperature of the extraction kettle is 41°C, the pressure of the extraction kettle is 22MPa, the temperature of the separation kettle I is 55°C, and the pressure is 9MPa , the temperature of the separation tank II is 50°C, the pressure is 4MPa, and CO is fed at a flow rate of 20kg / L 2 Extract for 4 hours, analyze the extract, adjust the pH to 8.0 with ammonia water, add chloroform to extract several times, collect and combine the chloroform extracts, concentrate under reduced pressure and add alumina medium pressure column (200-300 mesh neutral alumina, column diameter High ratio is 1:5), followed by volume ratio dichloromethane-methanol 20:1, 10:1, 5:1, 7:3 for elution, TLC follow-up detection, collect high-concentration fractions, recover reagents, dry The crude product of Dongyanning was obtained...

Embodiment 3

[0019] Pulverize the aboveground part of Dongyan, pass through a 20-mesh sieve, weigh 10kg and add it to the extraction kettle, turn on the machine, and adjust the parameters: the temperature of the extraction kettle is 43°C, the pressure of the extraction kettle is 18MPa, the temperature of the separation kettle I is 50°C, and the pressure is 10MPa , the temperature of the separation tank II is 48°C, the pressure is 6MPa, and CO is fed at a flow rate of 15kg / L 2 Extract for 2 hours, analyze the extract, adjust the pH to 10 with ammonia water, then add chloroform for extraction several times, collect and combine the chloroform extracts, concentrate under reduced pressure and add alumina medium pressure column (150-200 mesh neutral alumina, column diameter High ratio is 1:6), followed by elution according to the volume ratio of dichloromethane-methanol 20:1, 10:1, 5:1, 7:3, TLC tracking detection, collecting high concentration fractions, recovering reagents, drying The crude pr...

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PUM

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Abstract

The invention discloses a method for extracting and purifying Nazlinin, which comprises the steps of carrying out supercritical extracting on Nitraria schoberi L. serving as raw material for 2-4 hours in the presence of CO2 serving as a solvent; adjusting the pH value of resolving objects to be 8-10 by using ammonia water; adding chloroform for extraction; adding chloroform extract liquid into an alumina medium-pressure column; washing with water to be neutral; eluting by using dichloromethane-carbinol mixed solution; carrying out TLC (Thin-Layer Chromatography) tracking and detecting; collecting flow components with high concentration; recycling reagents; drying to obtain Nazlinin coarse products; and carrying out half-preparation high-efficiency liquid phase separation to obtain Nazlinin. The method disclosed by the invention is simple in process, small in pollution, and high in yield and the purity of extracted Nazlinin is high.

Description

Technical field: [0001] The invention belongs to the field of extraction and separation of effective plant components, and in particular relates to a method for extracting and purifying Dongyanning. Background technique: [0002] Nazlinin is a white amorphous powder, an indole alkaloid with the molecular formula C 15 h 21 N 3 , with a molecular weight of 243.35, derived from the aerial part of Nitraria schoberi L. of the family Zygophyllaceae. Pharmacological studies have shown that Dongjining has contraction and relaxation effects on blood vessels. The aortic ring test with rabbit endothelium shows that when the concentration is below 40nmol, it has vascular relaxation activity; when the dose exceeds 40nmol, the relaxation activity is transformed into contraction activity. , remove the endothelium, the relaxation activity disappears. [0003] Dongjin, also known as Nitraria xiaoguo, Siberia Nitraria (desert control research), Suanpang (Hexi, Gansu), Kami (Minqin, Gansu)...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/04
CPCY02P20/54
Inventor 陈洪生程志鹏
Owner 江苏博益生物科技有限公司