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Preparation method of cycleanine
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A technology of sclerophylline and lye, which is applied in the field of biomedicine, can solve problems such as difficulty in popularization and use, difficulty in obtaining crystallization, interference, etc., and achieve the effect of improving the separation effect
Pending Publication Date: 2022-04-12
SHANXI UNIV OF CHINESE MEDICINE
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[0003] N-butanol extraction is a conventional separation and purification method for water-soluble components. However, due to the special properties of terendrine, there are still many water-soluble impurities in the n-butanol extraction part of Tetradendron, making it difficult to obtain crystallization
It is also reported that medium-pressure preparative chromatography is used to separate the water-soluble alkaloids of Tetradontifolium. However, due to the particularity of the instruments and equipment used, it is difficult to popularize and use them.
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[0040] A kind of preparation method of staphine, comprises the following steps:
[0041] S01. Extracting Fangji Fangji with ethanolaqueous solution to prepare Fangji Fangji extract;
[0042] S02, subjecting the Fangji extract to acid-dissolving and alkali-precipitating treatment, then adding an organic solvent for extraction, and collecting the lye part;
[0043] S03, adjust the pH of the lye part to neutral, add n-butanol for extraction, and collect the n-butanol part;
[0044] S04. Adsorbing the water-soluble alkaloid in the n-butanol portion onto the alumina powder for sample mixing to obtain sample mixing powder;
[0082] 1.1 According to figure 1 Flowchart for the preparation of the n-butanol fraction of Tetradendronis
[0083]Weigh 5kg of Fenfangji decoction pieces, reflux twice with 50L of 95% ethanol, 1h / time, combine the filtrate twice, reclaim the ethanol to obtain the extract, add 1000mL of 1% hydrochloric acid to the extract, stir to dissolve, filter, and collect the filtrate as Acid water part. Add concentrated ammonia water to the acid water part, adjust the pH value to 9-10, and extract 3 times with an equal volume of chloroform. Combine the lye layers, add dilute hydrochloric acid dropwise to adjust the pH to 7, add an equal volume of n-butanol for extraction and extraction three times, and combine the n-butanol fractions.
[0084] 1.2 Identification of water-soluble alkaloids in different extraction parts
[0085] Take 1mg of sclerophylline standard substance, weigh it accurately, dissolve it in methanol and dilute to a 10mL volumetric flask, mix well, filter through a 0....
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Abstract
The invention belongs to the technical field of biological medicines, and particularly relates to a preparation method of cycleanine, which comprises the following steps: extracting stephania tetrandra by using an ethanolaqueous solution to prepare stephania tetrandra extract; the stephania tetrandra extract is subjected to acid dissolution and alkali precipitation treatment, then an organic solvent is added for extraction, and an alkali liquor part is collected; adjusting the pH value of the alkali liquor part to be neutral, adding n-butyl alcohol for extraction, and collecting an n-butyl alcohol part; adsorbing water-soluble alkaloid in the n-butyl alcohol part to aluminum oxidepowder for sample stirring to obtain sample stirring powder; loading the mixed sample powder into a column, then carrying out aluminacolumn chromatography, carrying out gradient elution by adopting dichloromethane-methanol as an eluent, collecting a fraction containing cycleanine, carrying out crystallization treatment on the fraction, and collecting crystals. According to the method, the high-purity cycleanine can be extracted from the stephania tetrandra.
Description
technical field [0001] The invention belongs to the technical field of biomedicine, and in particular relates to a preparation method of sclerophylline. Background technique [0002] Fangji (Stephaniae Tetrandrae Radix) is the dried root of Fangji (Stephaniatetrandra S. Moore), a plant of the family Fangji. Existing studies have shown that Fangji and its alkaloids have definite therapeutic effects in terms of antipyretic, analgesic, anti-inflammatory and diuretic. Effect, and found that it has a good application prospect in the treatment of hypertension, vascular dementia, angina pectoris, fibrosis and tumor prevention and treatment. However, these studies are mainly focused on the fat-soluble components of Fangji. Due to the strong water solubility of Fangji water-soluble alkaloids, it is difficult to separate and purify them. At present, there are few domestic reports on the separation and purification of Fangji water-soluble alkaloids. Therefore, the establishment of ext...
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