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Total glucosides extraction method of cardiac glycoside

An extraction method and a technology of cardiac glycosides, which are applied in the field of extracting total cardiac glycosides, can solve the problems of inability to meet large-scale industrial batch production, low content of total cardiac glycosides, and high cost, and achieve process specificity and reliability. Strong operability, high content of cardiac glycosides, and low cost of raw materials

Inactive Publication Date: 2017-09-15
黄惠民
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Chinese patents CN100522184A, CN101336924B, CN 101829173A and CN101336924A disclose that the cardiac glycosides in the crocodile gourd have good medicinal value such as anti-tumor, but the content of total cardiac glycosides in the gourd is very little (about 0.5 %-0.8%), which brought great difficulties to the extraction, separation and further research of cardiac glycosides
[0008] The extraction and s

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Take 1 kg of dry and pulverized croissanthus leaves, percolate with 8 times the amount of 70% ethanol, concentrate the percolation liquid under reduced pressure and recover ethanol to obtain a concentrated extract. The concentrated solution was dispersed with water to obtain a suspension, which was extracted with cyclohexane, the water layer was filtered, and freeze-dried to obtain a powdery solid. The solid was subjected to column chromatography with D-101 macroporous resin, and eluted with water and 95% ethanol, respectively. The ethanol eluate was collected and concentrated under reduced pressure to obtain the extract of croissant melon, which was 0.52 g of off-white powder solid.

[0022] After determination, the content of total cardiac glycosides in the off-white powder solid is 71.3%.

Embodiment 2

[0024] Take 0.2 kg of dry and pulverized croissanthus leaves, extract with 6 times the amount of methanol in a Soxhlet extractor until the extract is colorless. Concentrate the extract under reduced pressure to recover methyl ethanol to obtain a concentrated extract. The concentrated solution was dispersed with water to obtain a suspension, which was extracted with cyclohexane, the water layer was filtered, and freeze-dried to obtain a powdery solid. The solid was subjected to column chromatography with D-101 macroporous resin, and eluted with water and methanol, respectively. The methanol eluate was collected and concentrated under reduced pressure to obtain the croissant melon extract, 0.10 g of off-white powder solid.

[0025] After determination, the content of total cardiac glycosides in the off-white powder solid is 70.2%.

Embodiment 3

[0027] Take 1 kg of dried and pulverized croissanthus leaves, heat and reflux extraction with 10 times the amount of methanol until the extract is colorless. Concentrate the extract under reduced pressure to recover methyl ethanol to obtain a concentrated extract. The concentrated solution was dispersed with water to obtain a suspension, which was extracted with petroleum ether, the water layer was filtered, and freeze-dried to obtain a powdery solid. The solid was subjected to column chromatography with D-101 macroporous resin, and eluted with water and methanol, respectively. The methanol eluate was collected and concentrated under reduced pressure to obtain the croissant melon extract, which was 0.46 g of off-white powder solid.

[0028] After determination, the content of total cardiac glycosides in the off-white powder solid is 70.6%.

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Abstract

The invention relates to a total glucosides extraction method of cardiac glycoside. The method comprises the following steps: (1) rough extracting, namely, preparing leaves, stems, roots, shells, flowers and/ or juice of asclepiadaceae calotropis gigantean calotropis procera as raw medicinal materials; drying the raw medicinal materials, and crushing into a rough powder; roughly extracting the rough powder through an alcohol-water solution of which the concentration is 50-95% and the volume is 5-10 times the rough powder until the extracted solutions are colorless; combining the extracted solutions; performing pressure-reduced concentration to recover a solvent, so as to obtain a rough extractive; (2) extracting, namely, dispersing the rough extractive into water; extracting with a weak-polar organic solvent; filtering, freezing and drying a water layer to obtain powdered solid; (3) separating and purifying, namely, separating powdered solid through a column chromatography method to obtain a calotropis procera extractive in which the content of total glucosides of cardiac glycoside is beyond 70%. The method has the advantages that the cardiac glycoside content is high; the technology specificity and the operability are high; the steps are simple; the reaction yield is high; the raw material cost is low; and the industrial production applies.

Description

technical field [0001] The invention relates to a method for extracting total cardiac glycosides from the horned melon. Background technique [0002] Chinese tree cotton (Calotropis gigantea (Linnaeus) WT. Aiton] is a plant of the genus Calotropis gigantea (Linnaeus) WT. Aiton in the family Aslepiadaceae. Tree cotton (Crow's horn melon) has the functions of eliminating phlegm, relieving asthma, reducing inflammation, deworming, detoxifying, etc. It is used for the treatment of asthma, cough, skin diseases, dysentery, rheumatism, leprosy, ulcers, hemorrhoids and other diseases. Numerous preclinical and clinical studies have shown that the cardiac glycosides in C. gigantea also have broad antitumor activities. Kiss et al. used the active cardiac glycoside compound isolated from the white flower squash as a raw material to obtain a new cardiac glycoside UNBS1450 through structural modification and modification, and semi-artificially synthesized it. In the non-small cell lung ...

Claims

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Application Information

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IPC IPC(8): A61K36/27
CPCA61K36/27A61K2236/333A61K2236/39A61K2236/51A61K2236/55
Inventor 黄惠民肖繁花
Owner 黄惠民