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Method for extracting irisquinone from Chinese iris seed coat

A technology of equine and seed coat, applied in ion exchange, ion exchange regeneration, solid solvent extraction and other directions, can solve the problems of repeated crystallization product loss, large amount of organic reagents, pollution, etc., and reduce waste generation and extraction time. The effect of shortening and reducing production costs

Inactive Publication Date: 2012-08-29
苏州宝泽堂医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process has a large amount of organic reagents, a large loss of repeated crystallization products, and serious pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Crush the seed coat of iris seeds, add 1kg to the extraction kettle, turn on the machine to adjust the following parameters: extraction temperature is 40℃, extraction pressure is 20MPa, separation reactor I temperature is 50℃, pressure is 5MPa, separation reactor II temperature is 40℃ , The pressure is 4MPa, after the parameters are normal, the CO 2 The flow rate is 20L / h, and the extraction time is 3h. Collect the irisquine extract. After heating, add D101 macroporous resin column for adsorption, elution with ethanol petroleum ether (15:4) mixed solution, collect the eluate and concentrate, and place the concentrated solution for freezing and crystallization , Filter out the crystals, reflux in absolute ethanol for dissolution, add 3% activated carbon to decolorize, filter, freeze crystallization, and dry the crystals at low temperature to obtain a yellow powder product with a content of 95.3%.

Embodiment 2

[0020] Crush the seed coats of iris seeds, add 1kg into the extraction kettle, turn on the machine to adjust the following parameters: extraction temperature is 50℃, extraction pressure is 30MPa, separation reactor I temperature is 60℃, pressure is 8MPa, separation reactor II temperature is 40℃ , The pressure is 5MPa, after the parameters are normal, the CO 2 The flow rate is 20L / h, and the extraction time is 2h. Collect the irisquine extract. After heating, add it to AB-8 macroporous resin column for adsorption, elution with ethanol and petroleum ether (15:4) mixed solution, collect the eluate and concentrate, and place the concentrated solution. Freeze crystallization, filter out the crystalline product, reflux with absolute ethanol to dissolve, add 1% activated carbon to decolor, filter, freeze crystallization, and dry the crystalline product at low temperature to obtain a yellow powder product with a content of 94.8%.

Embodiment 3

[0022] Crush the iris seed coat, take 1kg into the extraction kettle, turn on the machine to adjust the following parameters: extraction temperature is 50℃, extraction pressure is 25MPa, separation reactor I temperature is 50℃, pressure is 6MPa, separation reactor II temperature is 50℃ , The pressure is 5MPa, after the parameters are normal, the CO 2 The flow rate is 204L / h, and the extraction time is 2h. Collect the irisquine extract. After heating, add the HPD-100 macroporous resin column for adsorption. The ethanol petroleum ether (15:4) mixed solution is eluted, the collected eluate is concentrated, and the concentrated solution is placed Frozen crystallization, filter out the crystalline product, reflux with absolute ethanol for dissolution, add 3% activated carbon to decolorize, filter, freeze crystallization, and dry the crystalline product at low temperature to obtain a yellow powder product with a content of 94.3%.

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PUM

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Abstract

The invention provides a method for extracting irisquinone from a Chinese iris seed coat, which comprises the following steps of: crushing the Chinese iris seed coat, adding into an extraction kettle, collecting an irisquinone extract through supercritical CO2 extraction, adding a macro-porous resin column for adsorption after heating, eluting ethanol petroleum ether mixed solution, collecting an eluent for concentration, putting, freezing and crystallizing concentrated solution, filtering a crystal, backwardly flowing and dissolving absolute ethyl alcohol, adding activated carbon to decolor, filtering, freezing and crystallizing, and drying a crystal at a low temperature to obtain a product. The method adopts both supercritical CO2 extraction and macro-porous resin column separation and is a highly-efficient and environmentally-friendly extracting method.

Description

Technical field: [0001] The invention relates to a method for extracting irisquinone from the seed coat of iris seeds, in particular to a method for applying supercritical CO 2 Extraction and macroporous resin separation method of irisquinone. Background technique: [0002] Irisquinone is a quinone compound, soluble in petroleum ether, chloroform, benzene, ether and other non-polar solvents, soluble in methanol, ethanol, etc., but hardly soluble in water. [0003] Irisitin mainly contains Irisitin A (C 24 H 38 O 3 ), iris B (C 24 H 40 O 3 ), solid at room temperature, oily liquid above 47°C, with anti-cancer, cooling blood and hemostasis, clearing away heat and dampness, a radiosensitizer combined with radiotherapy, is a second-class anti-cancer drug. [0004] Essence iris is the seed of the Iridaceae plant Essium iris. The seed coat contains iris A, B, C (pallason A, B, C), lupene-3-one (lupene-3-one), and betulin alcohol (betulin). ), β-sitosterol and phytowax. Kernel oil contain...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C50/28C07C46/10B01D11/02B01D15/08
CPCY02P20/54
Inventor 李法庆刘东锋
Owner 苏州宝泽堂医药科技有限公司