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Method for extracting and purifying vindoline

A purification method and the technology of ventolin, applied in the direction of organic chemistry, etc., can solve the problems of unsuitable industrial production, low content of ventolin, complicated extraction steps, etc., achieve less time consumption, increase content and yield, and meet market demands. effect of demand

Active Publication Date: 2015-02-25
HAINAN XI YUAN CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, it is mainly used to extract the total alkaloids of periwinkle from the stems, leaves, and flowers of the aboveground part of the periwinkle, and then to extract the ventolin through chromatographic column purification and crystallization. This method uses periwinkle The aboveground part is the raw material, the content of Wendolin is small, the extraction steps are cumbersome, time-consuming, and the amount of Wendolin is small, so it is not suitable for industrial production

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  • Method for extracting and purifying vindoline
  • Method for extracting and purifying vindoline
  • Method for extracting and purifying vindoline

Examples

Experimental program
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Effect test

Embodiment 1

[0039] Using fresh whole periwinkle (including root) as raw material, extract and isolate Wendolin according to the following method:

[0040] 1. Extraction and preparation of the crude product of Vendolin:

[0041] (1) Take 100kg of the whole periwinkle plant, add it to 850kg of 5wt% sodium chloride aqueous solution, soak it in ultrasonic for 15 minutes, then take out the periwinkle and put it directly into the cold air with a flow rate of 6.5m / s at -20°C for 40 minutes to freeze-dry. The periwinkle was crushed after freeze-drying.

[0042] (2) Add the periwinkle powder of the whole plant treated in step (1) into 300kg of water, adjust the pH to 1.5 with phosphoric acid, soak in ultrasonic for 3 hours, filter the filtrate, adjust the pH of the filtrate to 8-9 with ammonia water, and adjust the pH , apply high pressure to the filtrate, and spray it from the top of the extraction tank in the form of a spray at a speed of 180 ml / s. The ratio is 4.8:1, the filtrate and the extr...

Embodiment 2

[0052] 1. Extraction and preparation of the crude product of Vendolin:

[0053] Extract the crude product of Vendolin according to the method of Example 1, the difference is: the volume ratio of the filtrate to the extractant in step (2) is 5.5:1, and the extractant is n-bromopropane and ethanol with a volume ratio of 10:0.5 The mixture; in step (4), the volume ratio of dichloromethane and ethyl acetate is 10: 5. The mass of the obtained Wendolin crude product was 50.5g, the yield was 0.505‰, and the HPLC detection purity was 75.5%.

[0054] 2. The refinement of Wendolin:

[0055] Add 50.5g of the crude product of Vendolin to 151.5ml of a mixture of methanol, diethyl ether, petroleum ether and ethyl acetate with a volume ratio of 1:3:0.5:0.5, sonicate at room temperature for 5min, and wait for crystals to form, then incubate at -18°C After standing at low temperature for 24 hours, the crystallization was carried out. The obtained crystals were suction filtered at -18°C and...

Embodiment 3

[0057] The refined ventolin was extracted according to the method of Example 1, except that when refining the ventolin, the volume ratio of methanol, diethyl ether, petroleum ether and ethyl acetate was 1:3.5:0.3:0.6. The obtained high-purity ventolin was 37.1 g, and its purity was 99.5% as detected by HPLC.

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Abstract

The invention discloses a method for extracting and purifying vindoline. The method includes: salting the whole plants of catharanthus roseus, freezing and drying, and crushing; adding the acquired powder into water, adjusting pH and then extracting, adjusting pH and then extracting the extract to obtain coarse vindoline; recrystallizing the coarse vindoline in mixed solvent to obtain pure vindoline. The method has the advantages that the method is simple in step, low in time consumption and fast in product separation, pH gradient separation is used to directly obtain the high-purity coarse vindoline while column chromatography isolation is not needed, the vindoline with the purity above 99% is acquired after recrystallization, purification is simplified, and separation and purification of the vindoline are achieved fast, and the obtained final product is high in yield and purity and capable of satisfying market requirements.

Description

technical field [0001] The invention relates to a method for extracting, separating and purifying ventolin from periwinkle flowers, and belongs to the technical field of medicine extraction. Background technique [0002] Periwinkle is an important medicinal plant of the genus Periwinkle in the family Apocynaceae, native to South Asia, East Africa and tropical America. The whole plant of periwinkle can be used as medicine for pain relief, anti-inflammation, sleep, laxative and diuresis. The whole plant is toxic, and if ingested by mistake, it will cause leucopenia, thrombocytopenia, muscle weakness, paralysis of limbs and other symptoms. Periwinkle flowers, especially the roots, contain a lot of indole alkaloids, which have good medicinal value. Vindoline (also known as Vindoline) is one of the vinca alkaloids. Animal experiments have shown that it has hypoglycemic, diuretic, and blood lipid-lowering effects, and has inhibitory effects on some human pathogenic bacteria. It i...

Claims

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Application Information

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IPC IPC(8): C07D471/20
CPCC07D471/20
Inventor 王洪磊刘艳凤于文辉李宁宁王立成刘小鹏孙芳王龙正
Owner HAINAN XI YUAN CHEM TECH
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