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Preparation method of stephanine and hydrochloride thereof

A technology of fenugreek and hydrochloric acid, applied in the field of preparation of fenugreek hydrochloride, can solve the problems of low yield, no preparation process, excessive benzene content and the like

Active Publication Date: 2010-11-24
KUNMING INST OF BOTANY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, Stephanine and its salts have cumbersome separation and purification preparation process, low yield, and problems such as excessive benzene content caused by the use of benzene reagent in the purification process. So far, there is no preparation process for industrialized mass production.

Method used

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  • Preparation method of stephanine and hydrochloride thereof
  • Preparation method of stephanine and hydrochloride thereof
  • Preparation method of stephanine and hydrochloride thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Stephanine and stephanine hydrochloride are prepared by extracting, separating and purifying stephania epigaea.

[0034] (1) 250.0Kg ground does not allow rhizomes to be impurity removed, washed, dried, and crushed into coarse powder (passed through a 20-40 mesh sieve);

[0035] (2) The above-mentioned coarse powder is extracted with 1-2% hydrochloric acid aqueous solution by cold soaking for 34 times, and the extraction time is 4 days each time, filtering, merging the filtrate, concentrating, and recovering the solvent;

[0036] (3) Add sodium hydroxide (NaOH) to the residual aqueous solution, adjust the pH to 9, until the alkaloid precipitates, filter, and obtain 52.0Kg of the total alkaloid extract;

[0037] (4) Extraction of total alkaloids was extracted twice with ethanol under reflux, and the extraction time was 3 hours each time, filtered and concentrated to obtain 1.30Kg of stephanine total alkaloids;

[0038] (5) The above extract was dissolved in a small volu...

Embodiment 2

[0045] Extraction, separation and purification from Stephania epigaea to prepare stephanine and stephanine hydrochloride:

[0046] (1) 20Kg ground is not allowed to remove impurities from the rhizome, wash, dry, and pulverize into coarse powder (pass through a 20-40 mesh sieve);

[0047] (2) The above-mentioned coarse powder is extracted with 1-2% acetic acid aqueous solution for 4 times by cold soaking, and the extraction time is 5 days each time, filtering, merging the filtrate, concentrating, and recovering the solvent;

[0048] (3) Add potassium hydroxide (KOH) to the residual aqueous solution, adjust the pH to 9, until the alkaloids are precipitated, and filter to obtain 4.9Kg of the total alkaloid extract;

[0049] (4) Extraction of total alkaloids was extracted twice with ethanol under reflux, and the extraction time was 2 hours each time, filtered and concentrated to obtain 127 g of total alkaloids of stephanine;

[0050] (5) The above extract was dissolved with a sma...

Embodiment 3

[0057] Extraction, separation and purification from the plant S. cepharantha to prepare stephine and stephine hydrochloride:

[0058] (1) 100.0Kg Stephania chinensis is removed from impurities, washed, dried, and crushed into coarse powder (passed through a 20-40 mesh sieve);

[0059] (2) The above-mentioned coarse powder is extracted with 1-2% hydrochloric acid aqueous solution by cold soaking for 3 times, and the extraction time is 2 days each time, filtering, merging the filtrate, concentrating, and recovering the solvent;

[0060] (3) Sodium hydroxide (NaOH) was added to the residual aqueous solution to adjust the pH to 10 until the alkaloids were precipitated and filtered to obtain 18.6Kg of the total alkaloid extract.

[0061] (4) Extraction of total alkaloids was extracted 3 times with ethanol heating under reflux, each extraction time was 2.5 hours, filtered and concentrated to obtain 680 g of total alkaloids of stephanine;

[0062] (5) The above extract was dissolved...

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Abstract

The invention provides a new method for extracting, separating, purifying and preparing stephanine and hydrochloride thereof from plants, which comprises the following steps: alkalifying, depositing and filtering the acid water extracting solution of the plant menispermaceae raw material to obtain total alkaloid extract; extracting the total alkaloid extract with lower alcohol or acetone through refluxing, filtering, concentrating, and purifying the ethanol extract through column chromatography to obtain rough stephanine; further recrystallizing the rough stephanine to obtain the stephanine of which the purity is greater than 98%; and dissolving and acidifying the stephanine to obtain stephanine hydrochloride of which the purity is greater than 98%. The stephanine hydrochloride prepared by the method has the advantages of good color, high purity, no residual organic solvents, no need of repeated column chromatography, simple, safe and easy preparation process, lower cost, short production cycle and easy batch preparation and industrialized production.

Description

Technical field: [0001] The invention belongs to the field of chemistry and chemical engineering, and in particular relates to the extraction and separation of the natural plant physiologically active substance steppine and the preparation of its semi-synthetic product steppine hydrochloride. Background technique: [0002] Stephine, also known as stephine, cephalic stephine, golden thread clitoconine, bean flower vine. The English name is Cepharanthine, and the transliteration is Xifa Ansheng. Chemical name: 6', 12'-dimethoxy-2, 2'-dimethyl-6, 7-[methylenebis(oxy)]Oxyacan-than. Stephanine was first discovered in 1934 by the Japanese Maito Heisaburo from Stephania cepharantha (Stephania cepharantha), and then successively from plants such as S. sasakii and S. epigaea The compound was isolated. my country, especially the southwest region, is rich in such plant resources. Stephanine is a naturally occurring bisbenzylisoquinoline tertiary amine (bisbenzylisoquinolines.BBI) a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D491/22
Inventor 杨崇仁张颖君许敏曾恕芬张潇元陈江王东朱宏涛
Owner KUNMING INST OF BOTANY - CHINESE ACAD OF SCI
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