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Method for extracting dictyota dichotoma lactone

A technology of reticulin lactone and extract, applied in the direction of organic chemistry, etc., to achieve good adsorption performance, high product purity, and good separation effect.

Inactive Publication Date: 2012-09-12
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no relevant report on the separation and purification method of reticulide

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Weigh 1kg of nettleweed, dry and pulverize, extract twice with 90% ethanol under reflux, combine the extracts, concentrate to obtain the extract extract, add water to disperse, add to AB-8 macroporous adsorption resin column, first fully rinse with water , the flow rate is controlled at 6BV / h, and then eluted with 3 times the column volume of 50% ethanol, the elution flow rate is controlled at 4BV / h, the eluate is collected, concentrated under reduced pressure, and loaded onto a 200-mesh high-pressure silica gel column with a diameter of Height ratio 1:18, column pressure 2.2-3.5MPa, elution with hexane-acetone (9:1), high-performance liquid phase monitoring, collection of high-concentration alginate flow segmented, concentrated, and placed at -10°C Crystallization under the conditions, the crystals were filtered out, refluxed with hexane to dissolve the crystals 6 times, and the crystals were dried to obtain 0.31 g of diticrolactone with a content of 98.1%.

Embodiment 2

[0022] Weigh 1 kg of nettleweed, dry and pulverize it, extract it four times with 70% ethanol ultrasonically, combine the extracts, concentrate to obtain the extract extract, add water to disperse it, add it to a D101 macroporous adsorption resin column, and rinse it fully with water at a flow rate of Controlled at 1.5BV / h, and then eluted with 7 times the column volume of 80% ethanol, the elution flow rate was controlled at 2BV / h, the eluate was collected, concentrated under reduced pressure, and loaded onto a 400-mesh high-pressure silica gel column with a diameter of high Ratio 1:10, column pressure 3.5MPa, hexane-acetone (15:1) elution, high-performance liquid phase monitoring, collect the high-concentration stream of netdigalactone, concentrate, and place it at -10°C for crystallization , filtered out the crystals, refluxed the hexane to dissolve the crystals three times, and dried the crystals to obtain 0.33 g of diticrolactone with a content of 95.5%.

Embodiment 3

[0024] Weigh 10kg of nettleweed, dry and pulverize, use 80% ethanol to ultrasonically extract 3 times, combine the extracts, concentrate to obtain the extract extract, add water to disperse, add to D101 macroporous adsorption resin column, first fully rinse with water, flow rate Controlled at 2BV / h, and then eluted with 5 times the column volume of 60% ethanol, the elution flow rate was controlled at 3BV / h, the eluate was collected, concentrated under reduced pressure, and loaded onto a high-pressure silica gel column with a packing of 300 meshes. 1:15, column pressure 2.2-3.5MPa, elution with hexane-acetone (10:1), high-performance liquid phase monitoring, collecting high-concentration stream of alginate, concentrated, and placed at -10°C Crystallized, filtered out the crystals, refluxed with hexane to dissolve the crystals 5 times, dried the crystals to obtain 2.4 g of diticrolactone with a content of 96.1%.

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PUM

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Abstract

The invention discloses a method for extracting dictyota dichotoma lactone, which comprises steps of regarding dictyota dichotoma as a raw material, regarding 70%-90 % of alcohol as an extraction solvent, performing ultrasound extraction or reflux extraction for 2-4 times, performing filtration, filtrate combination and concentration, adding macroporous resin columns for absorption, using 50%-80% of alcohol to elute effective constituents, concentrating eluate, feeding the concentrated solution to a high-pressure silica gel column, using hexane-acetone for elution, enabling the eluate to subject to concentration and crystallization, enabling hexane to flow back and dissolve the crystal, performing recrystallization and obtaining the dictyota dichotoma lactone. The dictyota dichotoma lactone produced by the method is high in extraction rate, simple in process and specific.

Description

technical field [0001] The invention relates to a method for extracting diticolide from plants, in particular to a method for extracting diticolide from dicytoides. Background technique [0002] Dictyolactone belongs to diterpenoids, crystalline (hexane), mp64-65℃, [α]25 / D-165°(c=0.94, methanol). Molecular formula: C 20 h 30 o 2 , molecular weight: 302.46, structural formula: [0003] . [0004] Dictyolide is the main active chemical component in Dictyospermum. It has weak antifungal activity, strong cytotoxic activity and inhibits the binding of vasopressin (VP) to pig kidney, with an IC50 of 66 μM. Previous studies have shown that the MIC (μg / mL) of reticoidide to Aspergillus fumigatus and Microsporum canis are 180 and 170 respectively, and the ED50 (μg / mL) to P388, P388 / DOX, KB, NSCLCN6-L16 cell lines mL) were 2.8, 2.4, 4.9, 0.3, respectively, and its anti-NSCLCN6-L16 activity was stronger than that of 6-mercaptopurine. [0005] At present, Digyrolactones are mai...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/93
Inventor 刘东锋吴艳波
Owner NANJING ZELANG MEDICAL TECH
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