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Preparation method of arecoline hydrobromide and solid-liquid-liquid-liquid continuous extraction coupling device

A technology for extracting arecoline hydrobromide, applied in liquid solution solvent extraction, solid solvent extraction, organic chemistry, etc., can solve problems such as low production efficiency, large consumption of hydrobromic acid, and difficulty in meeting the needs of industrial production. Achieve the effect of high purity and high safety

Pending Publication Date: 2022-07-22
CHANGSHA LVYE BIOTECHNOLOGY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Yet the preparation method of existing arecoline hydrobromide, there is the problem of using flammable and explosive organic solvent (ether), highly toxic solvent (such as carbon tetrachloride), hydrobromic acid consumption is too large or production efficiency is low Defects, it is difficult to meet the needs of industrial production

Method used

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  • Preparation method of arecoline hydrobromide and solid-liquid-liquid-liquid continuous extraction coupling device
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  • Preparation method of arecoline hydrobromide and solid-liquid-liquid-liquid continuous extraction coupling device

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preparation example Construction

[0029] The invention provides a preparation method of arecoline hydrobromide, comprising the following steps:

[0030] The areca alkaloid extract is mixed with a solid adsorbent, and adsorbed to obtain an alkaloid solid adsorbate; the solid adsorbent comprises alumina;

[0031] The alkaloid solid adsorbate is subjected to solid-liquid continuous extraction to obtain arecoline extract; the extraction solvent for solid-liquid continuous extraction comprises chlorinated aliphatic hydrocarbons;

[0032] The arecoline extract is mixed with an aqueous hydrobromic acid solution, and liquid-liquid continuous extraction is carried out in the presence of a solid dispersion filler to obtain a crude arecoline hydrobromide salt extract;

[0033] The crude arecoline hydrobromide extract is successively concentrated and recrystallized to obtain arecoline hydrobromide.

[0034] In the present invention, unless otherwise specified, all raw material components are commercially available commod...

Embodiment 1

[0056] (1) it is 10 meshes with betel nut dried fruit powder to particle diameter, obtains betel nut dried fruit powder; 200g of areca nut dried fruit powder is in the hydrochloric acid aqueous solution that 2000mL concentration is 0.5wt%, carries out diafiltration extraction, and gained acid water extract flows through 732 cation exchange resin, the resin saturated with adsorption is rinsed with deionized water, then 800mL of concentrated ammonia water-ethanol solution is added to elute, and the solvent in the obtained eluent is recovered to dryness to obtain the areca alkaloid extract; wherein, The concentration of ammonia water in the concentrated ammonia water-ethanol solution is 17wt%, and the volume ratio of ammonia water to ethanol (volume fraction of 80%) is 0.3:100.

[0057] (2) Stir and mix the areca alkaloid extract with 5 g of alumina for column chromatography, and dry to constant weight at 60° C. to obtain the alkaloid solid adsorbate.

[0058] (3) Use figure 1 T...

Embodiment 2

[0064] The arecoline hydrobromide product is prepared according to the method of embodiment 1, and the difference from Example 1 is that the alumina quality is 10 g; the extraction solvent is dichloromethane; the prepared arecoline hydrobromide product purity is 96.3%, Norarecoline Hydrobromide 2.3%.

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Abstract

The invention provides a preparation method of arecoline hydrobromide and a solid-liquid-liquid-liquid continuous extraction coupling device, and relates to the technical field of alkaloid extraction. According to the method disclosed by the invention, the arecoline selectivity and impurity separation in the areca-nut extract are realized by utilizing solid-liquid continuous extraction, the tedious operation process of arecoline separation is simplified, and the separation efficiency is improved; in the liquid-liquid continuous extraction process, the solid dispersion filler can improve the dispersion degree of the arecoline extraction liquid in a hydrobromic acid aqueous solution and improve the salifying efficiency of arecoline hydrobromide, the use amount of hydrobromic acid is small, and crude arecoline hydrobromide extraction liquid can be efficiently prepared; the crude arecoline hydrobromide extract liquor is concentrated and recrystallized to obtain high-purity arecoline hydrobromide, the operation is simple, and the production efficiency is high. Meanwhile, the chlorinated aliphatic hydrocarbon can be recycled in the solid-liquid continuous extraction and process, the solvent dosage is greatly reduced, and the method is low in production cost, green, environmentally friendly and suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of alkaloid extraction, in particular to a preparation method of arecoline hydrobromide and a solid-liquid-liquid-liquid continuous extraction coupling device. Background technique [0002] Betel nut contains a variety of alkaloids, the content is generally 0.3 to 0.7% of the dry fruit weight. Arecoline alkaloids are mainly arecoline, arecaidine, cuvacoline, cuvacine, areolidine, homoatrecoline, isotope Demethyl arecoline (isoguvacine) and so on. Among them, arecoline, whose chemical name is 1,2,5,6-tetrahydro-1-methyl-3-picolinate methyl ester, can be used in medicine to treat glaucoma, and it can also be used as an anthelmintic for animals. It is often used in the form of hydrobromide. Arecoline hydrobromide is a colorless crystal with a melting point of 169-171°C, bitter in taste, soluble in water and ethanol, and can be used as an antiarrhythmic drug, a molluscicide and an anti-female reproductive rod...

Claims

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Application Information

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IPC IPC(8): C07D211/78B01D11/02B01D11/04
CPCC07D211/78B01D11/02B01D11/04
Inventor 董新荣张琳玉文利新李荣芳谢小红麦金辉王江萍何兴国蒋政云
Owner CHANGSHA LVYE BIOTECHNOLOGY CO LTD
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