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Preparation method of annonanceous acetogenins

A technology for lychees and seeds, which is applied in the field of separation and preparation of custard apple spirit, can solve the problems such as the preparation method of high-content custard apple spirit, and achieve the effects of short preparation period, low solution efficiency and high yield

Inactive Publication Date: 2012-12-19
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there has not been any patent report on the preparation method of high-content Anemona cuspidatum

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Take the custard apple seeds, take 1kg, put them into a supercritical extraction device, the extraction temperature is 35°C, the extraction pressure is 30MPa, CO 2 The flow rate is 15L / h, extract for 20min, add 6 times of 90% ethanol solution to the residue, carry out continuous countercurrent ultrasonic extraction at 45°C for 30min, the ultrasonic frequency is 60KHz, filter to obtain the extract, concentrate and dry under reduced pressure, and obtain the crude extract material; adopt high-speed counter-current chromatography to separate and purify the anemone fruit in the crude extract, and use a volume ratio of 5:4:6:2 petroleum ether-ethyl acetate-methanol-water as a two-phase solvent system, and the upper phase is filled with The high-speed countercurrent chromatographic column is the stationary phase, the main engine is rotated, and the lower phase is pumped into the mobile phase. The crude extract dissolved in the mobile phase is injected by the injection valve, an...

Embodiment 2

[0023] Take the custard apple seeds, take 1kg, put them into a supercritical extraction device, the extraction temperature is 45°C, the extraction pressure is 29MPa, CO 2 The flow rate is 15L / h, the extraction is 50min, the residue is added with 8 times of 80% ethanol solution, and the continuous countercurrent ultrasonic extraction is carried out at 30°C for 70min, the ultrasonic frequency is 60KHz, filtered to obtain the extract, concentrated and dried under reduced pressure, and the crude extract is obtained. thing; using high-speed countercurrent chromatography to separate and purify the anemone fruit in the crude extract, with a volume ratio of 7:4:7:2 petroleum ether-ethyl acetate-methanol-water as a two-phase solvent system, and the upper phase is filled with The high-speed countercurrent chromatographic column is the stationary phase, the main engine is rotated, and the lower phase is pumped into the mobile phase. The crude extract dissolved in the mobile phase is injec...

Embodiment 3

[0025] Take thick custard apple seeds, take 1kg, put them into a supercritical extraction device, the extraction temperature is 38 ° C, the extraction pressure is 26 MPa, CO 2 The flow rate is 18L / h, the extraction is 30min, the residue is added with 7 times of 850% ethanol solution, and the continuous countercurrent ultrasonic extraction is carried out at 35°C for 60min, the ultrasonic frequency is 40KHz, filtered to obtain the extract, concentrated and dried under reduced pressure, and the crude extract is obtained. material; using high-speed counter-current chromatography to separate and purify the anemone fruit in the crude extract, with a volume ratio of 6:4:7:3 petroleum ether-ethyl acetate-methanol-water as a two-phase solvent system, and the upper phase is filled with The high-speed countercurrent chromatographic column is the stationary phase, the main engine is rotated, and the lower phase is pumped into the mobile phase. The crude extract dissolved in the mobile phas...

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PUM

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Abstract

The invention relates to a preparation method of annonanceous acetogenins, which is simple to operate and generates less pollution. The preparation method comprises the following steps: (1) taking Annona crassiflora seed, and extracting grease substances in the medicinal material with a supercritical carbon dioxide fluid; (2) carrying out continuous reflux ultrasonic extraction on the degreased medicinal material with an alcohol solution, filtering to obtain an extracting solution, concentrating and drying to obtain a crude extract; (3) separating and purifying the annonanceous acetogenins in the crude extract by high-speed counter-current chromatography, and collecting the annonanceous acetogenins component, wherein the two-phase solvent system is petroleum ether-ethyl acetate-methanol-water, the upper phase is a stationary phase, and the lower phase is a mobile phase; and (4) carrying out vacuum concentration on the annonanceous acetogenins component, precipitating crystals, filtering out the crystals, adding ethyl acetate to dissolve the crystals under reflux, and standing for recrystallization. The purity of the annonanceous acetogenins product is high; and the invention can easily implement industrialized amplification.

Description

technical field [0001] The invention belongs to the technical field of extraction and separation of traditional Chinese medicines, and relates to a method for separating and preparing custard apple linguine from seeds of custard apple. Background technique [0002] Annona cuspidatum spirit, white amorphous powder, derived from the Annonaceae plant Annona crassiflora Seed. The main active ingredients of the seeds of Annua apple are acetylsarginine compounds, and the main ingredient is Chilingin. Anemone officinalis has anti-tumor activity, and its ED50 (μg / ml) against the following tumor cells is: A-549 (0.006); HT-29 (0.6); MCF-7 (0.004); RPMI-7951 (0.001) ;U-251(0.01). Its strength of action is equivalent to that of doxorubicin. [0003] At present, the annonanceous acetogenins (AAGs), the secondary metabolites of Annonaceae plants, are regarded as potential resources for new antitumor drugs. AAGs can inhibit the replication of human ovarian tumor IA9 cells and induce a...

Claims

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Application Information

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IPC IPC(8): C07D307/58
CPCY02P20/54
Inventor 刘东锋万冬梅
Owner NANJING ZELANG MEDICAL TECH
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