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Preparation method of bubble-shaped annonaceous acetogenins

A kind of custard apple, bubble-like technology, applied in the field of natural medicinal chemistry, to achieve the effect of simple operation, large processing capacity and fast separation speed

Inactive Publication Date: 2013-08-28
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Through literature search, there is no method for preparing vesicular custard from the bark of vesicular custard apple in China

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Grind the bark of custard apple in bubble shape, take 1kg and put it into a supercritical extraction kettle, and feed it with liquid CO 2 , set the extraction pressure to 28MPa, and the temperature to 48°C. After reaching the above parameters, adjust the liquid CO 2 The flow rate is 4ml / g crude drug / min, 95% ethanol solution is used as entrainer, the entrainer dosage is 15% of the total extraction solvent, dynamic extraction is carried out for 100min, the analysis is carried out at a pressure of 7.5MPa and a temperature of 40°C, and the obtained extract is dissolved in methanol , add a small amount of neutral magnesia to mix the sample, evaporate the solvent, put it on the magnesia column by dry method, gradient elution with petroleum ether-acetone 20:3, 11:3, 5:3 mixed solvent, collect the eluate and concentrate under reduced pressure to obtain crude extract. Take n-hexane, ethyl acetate, methanol, and water and mix them according to 6:8:4:5. After the mixture is full...

Embodiment 2

[0026] The foamy custard apple bark is crushed, and 2kg is added to a supercritical extraction kettle, and liquid CO 2 , set the extraction pressure to 35MPa, and the temperature to 50°C. After reaching the above parameters, adjust the liquid CO 2 The flow rate is 5ml / g crude drug / min, 95% ethanol solution is used as entrainer, the amount of entrainer is 12% of the total extraction solvent, dynamic extraction is carried out for 50min, and the analysis is carried out at a pressure of 9MPa and a temperature of 38°C. After the obtained extract is dissolved in methanol, Add a small amount of neutral magnesia to mix the sample, evaporate the solvent, put it on the magnesia column by dry method, and elute with petroleum ether-acetone 20:3, 10:3, 5:3 mixed solvent gradient elution, collect the eluate and concentrate under reduced pressure to obtain crude Extract. Take n-hexane, ethyl acetate, methanol, and water and mix them according to 7:7:3:4. After mixing and layering, take the ...

Embodiment 3

[0028] The foamy custard apple bark is crushed, and 2kg is added to a supercritical extraction kettle, and liquid CO 2 , set the extraction pressure to 30MPa and the temperature to 60°C. After reaching the above parameters, adjust the liquid CO 2 The flow rate is 3.5ml / g crude drug / min, 95% ethanol solution is used as entrainer, the amount of entrainer is 14% of the total extraction solvent, dynamic extraction is carried out for 80min, and the analysis is carried out at a pressure of 8MPa and a temperature of 45°C, and the obtained extract is dissolved in methanol , add a small amount of neutral magnesia to mix the sample, evaporate the solvent, put it on the magnesia column by dry method, gradient elution with petroleum ether-acetone 20:3, 9:3, 5:3 mixed solvent, collect the eluate and concentrate under reduced pressure to obtain crude extract. Take n-hexane, ethyl acetate, methanol, and water and mix them according to 5:6:5:3. After mixing and layering, take the upper phase...

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PUM

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Abstract

The invention discloses a preparation method of bubble-shaped annonaceous acetogenins. The method comprises the following steps of: a, taking bubble-shaped sweetsop barks and crushing, adding the crushed bubble-shaped sweetsop barks into a supercritical extraction kettle, and carrying out supercritical CO2 extraction by taking ethanol as an entrainer; b, purifying an extractive by adopting neutral magnesium oxide column chromatography, carry outing gradient elution by utilizing a petroleum ether-acetone mixing agent, collecting an elution solution and decompressing and concentrating to obtain a rough extract; and c, carrying out high-speed countercurrent chromatography separation on the rough extract, monitoring by an ultraviolet detector, collecting target components, refrigerating and crystallizing to obtain the bubble-shaped annonaceous acetogenins. When the preparation method is used for preparing the bubble-shaped annonaceous acetogenins, the process is simple and the efficiency is high, and the content of the obtained products is high, so that the preparation method is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of natural medicine chemistry, and in particular relates to a preparation method of bubbly anemone. Background technique [0002] Bullatanocin, CAS No. 129138-51-8, molecular formula C 37 h 66 o 8 , the molecular weight is 630.93, and the structural formula is: [0003] . [0004] Blistered custard fruit is derived from custard apple (Annonaceae) Annona bullata An acetaminophenin compound from the bark of Rich. Studies have shown that custardin has cytotoxic activity, and its cytotoxic effect on lung and colon cancer cell lines is 10,000 times stronger than that of doxorubicin. The LC50 of sea shrimp test (BST) is 0.43 μg / mL; it has anti-tumor effect . The ED50 of A-549, MCF-7 and HT-29 are 5.15×10 -10 μg / mL, 0.0242μg / mL and 1.66×10 -11 μg / mL. The IC50 of rat mitochondria bioassay is 50.7nM / Lt / mg protein. At present, the secondary metabolites of Annonaceae plants, acetylsarginine compounds of Annonaceae, ...

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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