Method for extracting carboxylic acid from juniperus chinensis

A technology of cypress acid and cypress, applied in the preparation field of extracting cypress acid from plants, achieving the effects of less pollution, large-scale production operations, and low energy consumption

Inactive Publication Date: 2012-01-25
SUZHOU PAITENG BIOLOGICAL MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In the prior art, there is no report on the preparation process applicable to the industrialized large-scale production of high-purity cinnamon acid

Method used

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  • Method for extracting carboxylic acid from juniperus chinensis

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Embodiment 1

[0024] Get cypress bark 10Kg, pulverize, add to CO 2 In the supercritical extractor, ethanol is used as the entrainer, the entrainer accounts for 1% by volume of the total extraction solvent, the extraction pressure is 10MPa, the temperature is 40°C, CO 2 The flow rate is 1ml / g crude drug·min, the extraction time is 80min, and the extract is obtained, which is adsorbed by D101 macroporous adsorption resin, washed with water to remove impurities, eluted with 30% ethanol, collected 3 times the column volume eluate, passed through a 201×7 type Strongly basic styrene-type anion-exchange resin adsorption, eluted with 0.4mol / L NaOH solution, collected and eluted, filtered, passed through 001×7 type strongly acidic styrene-type cation-exchange resin, collected effluent, filtered, Concentrate, add ethyl acetate to crystallize, separate and crystallize, wash and dry to obtain 26.7g of acanthusic acid, which is detected by HPLC with a purity of 95.5%, UV, IR, MS, 2 HNMR, 13 The data c...

Embodiment 2

[0026] Get cypress bark 10Kg, pulverize, add to CO 2 In the supercritical extractor, ethanol is used as the entrainer, the entrainer accounts for 3% by volume of the total extraction solvent, the extraction pressure is 30MPa, the temperature is 50°C, CO 2 The flow rate is 3ml / g crude drug·min, the extraction time is 120min, and the extract is obtained, adsorbed by D101 macroporous adsorption resin, eluted with water to remove impurities, eluted with 50% ethanol, collected 8 times the column volume eluate, passed through a 201×4 type Strongly basic styrene-type anion-exchange resin adsorption, eluted with 0.4mol / L NaOH solution, collected and eluted, filtered, passed through 001×4 strong acidic styrene-type cation-exchange resin, collected effluent, filtered, Concentrate, add ethyl acetate to crystallize, separate and crystallize, wash and dry to obtain 28.9g of acanthusic acid, detected by HPLC, the purity is 93.4%, UV, IR, MS, 2 HNMR, 13 The data characterizing its physical...

Embodiment 3

[0028] Get cypress bark 10Kg, pulverize, add to CO 2 In a supercritical extractor, ethanol is used as an entrainer, and the volume percentage of the entrainer in the total extraction solvent is 2%, the extraction pressure is 20MPa, the temperature is 45°C, CO 2 The flow rate is 2ml / g crude drug·min, the extraction time is 100min, and the extract is obtained, which is adsorbed by D101 macroporous adsorption resin, washed with water to remove impurities, eluted with 40% ethanol, collected 5 times the column volume eluate, passed through D201 strong base Adsorbed with a strong styrene-type anion exchange resin, eluted with 0.4mol / L NaOH solution, collected and eluted, filtered, passed through a D001 type strongly acidic styrene-type cation-exchange resin, collected the effluent, filtered, concentrated, and added acetic acid Ethyl ester was crystallized, separated and crystallized, washed, and dried to obtain 24.2 g of cinnamon acid, which was detected by HPLC with a purity of 97....

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Abstract

The invention relates to a method for extracting carboxylic acid from juniperus chinensis, which is easy and convenient to operate and has small pollution and low energy consumption. The method comprises the following process steps of: smashing juniperus chinensis bark; adding into a CO2 supercritical extractor to obtain an extract; adsorbing with D101 macroporous absorption resin, eluting with water to remove impurities; eluting with 30-50 percent ethanol; adsorbing with strongly alkaline styrene anion-exchange resin; eluting with a 0.4 mol/L NaOH solution; collecting and eluting; filtering; passing through the strongly alkaline styrene anion-exchange resin; collecting an effluent liquid; filtering; concentrating; adding ethyl acetate for crystallizing; separating crystals; and washing and drying. Due to the adoption of the method for preparing carboxylic acid, the product purity is high and industrial amplification is easy to realize.

Description

technical field [0001] The present invention relates to a kind of preparation method of incandine acid, especially a kind of preparation method of extracting incandine acid from plants. Background technique [0002] Carboxylic acid, molecular formula: C20H30O2, molecular weight: 302.456, CAS registration number: 2761-77-5, mainly exists in various plants of Araucaceae and Cupressaceae. Juniperus chinese Rich in bark. Its molecular formula is as follows. [0003] [0004] Modern studies have shown that acanthusic acid has very strong anti-tumor, anti-inflammatory, and antibacterial activities, and it is also used as a raw material for the synthesis of other active derivatives. [0005] In the prior art, there is no report on the preparation process applicable to the industrialized large-scale production of high-purity cinnamon acid. Contents of the invention [0006] The technical problem to be solved by the present invention is to provide a kind of preparation metho...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C61/35C07C51/42
CPCY02P20/54
Inventor 王峰王琳张发成
Owner SUZHOU PAITENG BIOLOGICAL MEDICAL TECH
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