Method for separating and purifying scopolamine monomer from anisodus acutangulus plant

A technology for separation and purification of scopolamine, applied in the field of separation and purification of scopolamine monomer, which can solve the problems of low purity and low content of scopolamine monomer

Pending Publication Date: 2022-05-17
锦州拾正生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] But, in the existing method for separating and purifying scopolamine monomer from thr

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] A method for isolating and purifying scopolamine monomer from three-thirds plants, comprising the following steps:

[0030] Mix 1000g of 3 / 3 coarse powder with ethylene glycol, perform supercritical extraction, the extraction solvent is carbon dioxide, butane and ethanol, and the volume ratio of the three is 3:0.5:1, and the extract A is obtained. Add ammonia water with a mass fraction of 0.01% to the extract A, slowly adjust the pH to 9, and extract with chloroform to obtain the extract B. Add 5 mL of dilute sulfuric acid with a mass fraction of 1% to the extract B, react for 30 min, and extract with carbon tetrachloride and chloroform in sequence at 60°C to obtain extract C. The extract C was centrifuged at 1000 rpm for 5 minutes to obtain a supernatant, which was dried in vacuum at a drying temperature of 55° C. and a pressure of 0.01 MPa. After drying, the moisture content was 5% to obtain a residue.

[0031] Dissolve the residue in dilute sulfuric acid, then add s...

Embodiment 2

[0033] A method for isolating and purifying scopolamine monomer from three-thirds plants, comprising the following steps:

[0034] Mix 1000g of three-thirds of coarse powder with ethylene glycol, and perform supercritical extraction. The extraction solvents are carbon dioxide, butane and ethanol, and the volume ratio of the three is 3:1:1 to obtain the extract A. Add ammonia water with a mass fraction of 0.5% to the extract A, slowly adjust the pH to 10, and extract with chloroform to obtain the extract B. Add 0.5 mL of dilute sulfuric acid with a mass fraction of 20% to the extract B, react for 40 min, and extract with carbon tetrachloride and chloroform in sequence at 70°C to obtain extract C. The extract C was centrifuged at 2000 rpm for 10 min to obtain a supernatant, which was dried in vacuum at a drying temperature of 65° C. and a pressure of 0.05 MPa. After drying, the moisture content was 10% to obtain a residue.

[0035] Dissolve the residue in dilute sulfuric acid, ...

Embodiment 3

[0037] A method for isolating and purifying scopolamine monomer from three-thirds plants, comprising the following steps:

[0038] Mix 1000g of three-thirds coarse powder with ethylene glycol, perform supercritical extraction, the extraction solvent is carbon dioxide, butane and ethanol, and the volume ratio of the three is 3:0.6:1, and the extract A is obtained. Add ammonia water with a mass fraction of 0.08% to the extract A, slowly adjust the pH to 9.5, and extract with chloroform to obtain the extract B. Add 1 mL of dilute sulfuric acid with a mass fraction of 5% to the extract B, react for 35 minutes, and extract with carbon tetrachloride and chloroform in sequence at 65°C to obtain extract C. The extract C was centrifuged at 1200 rpm for 7 minutes to obtain a supernatant, which was dried in vacuum at a drying temperature of 60° C. and a pressure of 0.02 MPa. After drying, the moisture content was 7% to obtain a residue.

[0039] Dissolve the residue in dilute sulfuric a...

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PUM

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Abstract

The invention provides a method for separating and purifying scopolamine monomers from an anisodus acutangulus plant, and relates to the technical field of scopolamine monomer extraction and separation. The method comprises the following steps: mixing coarse powder of anisodus acutangulus with a solvent, carrying out supercritical extraction to obtain an extract A, adding ammonia water, adjusting the pH value to 9-10, extracting with chloroform to obtain an extract B, adding dilute sulphuric acid, reacting for 30-40 minutes, sequentially extracting with carbon tetrachloride and chloroform to obtain an extract C, centrifuging the extract C to obtain a supernatant, and carrying out vacuum drying to obtain residues; the method comprises the following steps: dissolving residues in dilute sulphuric acid, adding a sodium bicarbonate solution to adjust the pH value to 6.8-7.3, heating, standing at 50-60 DEG C for 1-2 days, adding activated carbon to react, performing ultrafiltration and concentration to obtain a concentrated solution, extracting the concentrated solution with chloroform for 1-3 times, combining extract liquor, and drying by distillation. The scopolamine obtained by the method has higher content and higher purity.

Description

technical field [0001] The invention relates to the technical field of scopolamine extraction and separation, in particular to a method for separating and purifying scopolamine monomers from three-thirds plants. Background technique [0002] Sanfensan root, stem, and leaf all contain scopolane alkaloids, and the roots mainly contain hyoscyamine, anisodamine, anisodine, and rhizogenine. Therefore, Sanfensan is an important resource plant for extracting these alkaloids. [0003] Scopolamine is an organic compound with the chemical formula C 17 h 21 NO 4 , a tropane-type alkaloid, which exists in Solanaceae plants. E. Schmidt was first isolated from scopolamine in 1892. Its effect is similar to that of atropine. Its dilated pupils and inhibition of glandular secretion are stronger than atropine. It has an excitatory effect on the respiratory center, but has a significant inhibitory effect on the cerebral cortex. In addition, it also has the effects of dilating capillaries, ...

Claims

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Application Information

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IPC IPC(8): C07D451/10
CPCC07D451/10Y02P20/54
Inventor 于喜洋刘千驰刘东滨
Owner 锦州拾正生物科技有限公司
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