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Separating purification method for atalantia buxifolia alkali

A technology for separation and purification of agaric, which is applied in the field of separation and purification of agaric in wine cake, and can solve problems such as extraction and purification methods of agaric in wine cake that have not yet been seen, and achieve large sample loading, high extraction rate, and good separation effect Effect

Inactive Publication Date: 2012-08-08
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there is no report on the extraction and purification method of agarine from wine cake in China

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Dry and pulverize the black root of the single-leaf wine cake, take 5kg, feed from the feed port at the head of the continuous countercurrent ultrasonic extraction equipment, add 12 times of 90% ethanol solution from the solvent inlet at the tail of the continuous countercurrent ultrasonic extraction equipment, and carry out at 55 ° C. Continuous countercurrent ultrasonic extraction was carried out for 20min, the ultrasonic frequency was 80KHz, the extract was concentrated and dried to obtain an ethanol extract, which was dissolved in an aqueous hydrochloric acid solution with pH 2, filtered, and the filtrate was adjusted to pH 11 with concentrated ammonia or sodium hydroxide aqueous solution, extracted with chloroform, and the extract was concentrated, It was injected into a preparative high performance liquid chromatograph, the acetonitrile-0.05% ethylenediamine aqueous solution with a volume ratio of 43:57 was the mobile phase, and the ultraviolet detection wavelength ...

Embodiment 2

[0018] Dry and pulverize the black root of the single-leaf wine cake, take 5 kg, feed from the feed port at the head of the continuous countercurrent ultrasonic extraction equipment, and add 5 times of 90% ethanol solution from the solvent inlet at the tail of the continuous countercurrent ultrasonic extraction equipment, and carry out at 25 ° C. Continuous countercurrent ultrasonic extraction was carried out for 120min, the ultrasonic frequency was 30KHz, the extract was concentrated and dried to obtain an ethanol extract, which was dissolved in an aqueous hydrochloric acid solution with pH 3, filtered, and the filtrate was adjusted to pH 9 with concentrated ammonia or sodium hydroxide aqueous solution, extracted with chloroform, and the extract was concentrated, Inject into a preparative high performance liquid chromatograph, the acetonitrile-0.05% ethylenediamine aqueous solution with a volume ratio of 43:57 is the mobile phase, the ultraviolet detection wavelength is 347 nm,...

Embodiment 3

[0020] Dry and pulverize the black root of the single-leaf wine cake, take 5kg, feed from the feed port at the head of the continuous countercurrent ultrasonic extraction equipment, and add 10 times of 90% ethanol solution from the solvent inlet at the tail of the continuous countercurrent ultrasonic extraction equipment, and carry out at 45 ° C. Continuous countercurrent ultrasonic extraction was carried out for 80min, the ultrasonic frequency was 50KHz, the extract was concentrated and dried to obtain an ethanol extract, which was dissolved with an aqueous hydrochloric acid solution of pH 3, filtered, and the filtrate was adjusted to pH 10 with concentrated ammonia or sodium hydroxide aqueous solution, extracted with chloroform, and the extract was concentrated, It was injected into a preparative high performance liquid chromatograph, the acetonitrile-0.05% ethylenediamine aqueous solution with a volume ratio of 43:57 was the mobile phase, and the ultraviolet detection wavelen...

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Abstract

The invention relates to the technical field of extraction of plant effective components, in particular to a separating purification method for atalantia buxifolia alkali. The technical scheme of the method comprises the following steps of (1) performing continuous countercurrent ultrasonic extraction on single leaf atalantia buxifolia roots by utilizing 90% ethanol solution, and obtaining ethanol extract; (2) utilizing acid water of pH2-3 to dissolute the ethanol extract, and filtering the extract; (3) mixing concentrated ammonia or sodium hydroxide solution with filtrate till a pH value reaches 9-11, and utilizing an organic solvent to extract the filtrate; and (4) concentrating extract liquid, filling the extract liquid into a preparation type high performance liquid chromatograph, and obtaining an atalantia buxifolia alkali product. The separating purification method for the atalantia buxifolia alkali can extract and separate a product with the purity of 95% above from raw materials and achieve the effective separation of the atalantia buxifolia alkali.

Description

technical field [0001] The invention belongs to the technical field of plant active ingredient extraction, and relates to a method for separating and purifying protidine from wine cakes. Background technique [0002] Atalaphylline, molecular formula C 23 H 23 NO 4 , the molecular weight is 377.44, mp.205-207℃, is from the single leaf wine cake Atalantia monophylla An acridine alkaloid isolated from the root of . Experimental studies have shown that protamine has antimalarial activity: at 10 μg / ml in vitro, the inhibition rate of Plasmodium yoelii is 94±4% (same as chloroquine diphosphate); mice were intraperitoneally injected with 50 mg / ml kg, it has obvious preventive effect on Plasmodium (P.berghei and P.vinckei). Protidine also has anti-cancer effect, can inhibit the growth of mouse leukemia cell L1210, ED 50 is 1.0 μg / ml. [0003] At present, there is no report in China on the extraction and purification method of protamine in wine cakes. SUMMARY OF THE INVENTIO...

Claims

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Application Information

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IPC IPC(8): C07D491/052
Inventor 刘东锋万冬梅
Owner NANJING ZELANG MEDICAL TECH
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