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Method for separating and purifying chlorogenic acid by utilizing temperature to induce aqueous two-phase system

A two-phase system, temperature-induced technology, applied in the separation/purification of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of difficult polymer recovery, hindering the application of two-phase technology, etc., To achieve the effect of environmental protection, short time consumption and high yield

Inactive Publication Date: 2013-12-04
BIOCHEM ENG COLLEGE OF BEIJING UNION UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the difficulty of polymer recovery, the application of aqueous two-phase technology has been hindered to some extent.

Method used

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  • Method for separating and purifying chlorogenic acid by utilizing temperature to induce aqueous two-phase system
  • Method for separating and purifying chlorogenic acid by utilizing temperature to induce aqueous two-phase system
  • Method for separating and purifying chlorogenic acid by utilizing temperature to induce aqueous two-phase system

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 1) Extraction of crude chlorogenic acid: crush 1.5 kg of Eucommia ulmoides leaves, put them into an extraction tank, add 10 L of water, heat to reflux for 2 hours, and concentrate to an extract, which is crude chlorogenic acid with a content of 13.37%.

[0021] 2) Two-phase aqueous phase separation: prepare EOPO / salt two-phase aqueous system, in which EOPO (molecular weight: 2000) is 10 mL, water is 15 mL, and the concentration of dipotassium hydrogen phosphate is 0.1 g / mL. Add 100 mg of crude chlorogenic acid to the aqueous two-phase system, mix well, and centrifuge at 2000 r / min for 3 minutes to separate the organic phase (rich in EOPO) and the aqueous phase, and the chlorogenic acid is enriched in the organic phase (upper phase ), impurities are enriched in the aqueous phase.

[0022] 3) Temperature-induced aqueous two-phase separation: The organic phase (rich in EOPO) was subjected to temperature-induced phase separation. After 20 minutes in a water bath at 60°C, t...

Embodiment 2

[0035] 1) Extraction of crude chlorogenic acid: crush 1.5 kg of Eucommia ulmoides leaves, put them into an extraction tank, add 10 L of water, heat to reflux for 2 hours, and concentrate to an extract, which is crude chlorogenic acid with a content of 13.37%.

[0036] 2) Two-phase aqueous phase separation: prepare EOPO / salt two-phase aqueous system, in which EOPO (SDP35, molecular weight 2750) 10mL, water 15mL, and salt are respectively selected from KH 2 PO 4 、K 2 HPO 4 、Na 2 SO 4 , NH 4 Cl, the concentration is 0.1g / mL respectively. Add 100 mg of crude chlorogenic acid to the two-phase aqueous system, mix well, and centrifuge at 2000 rpm for 3 minutes to separate the organic phase (rich in EOPO) and the aqueous phase, and the chlorogenic acid is enriched in the organic phase (top phase), impurities are enriched in the aqueous phase.

[0037] 3) Temperature-induced aqueous two-phase separation: The organic phase (rich in EOPO) was subjected to temperature-induced phase...

Embodiment 3

[0043]1) Extraction of crude chlorogenic acid: crush 1.5 kg of Eucommia ulmoides leaves, put them into an extraction tank, add 10 L of water, heat to reflux for 2 hours, and concentrate to an extract, which is crude chlorogenic acid with a content of 13.37%.

[0044] 2) Two-phase aqueous phase separation: Prepare EOPO / salt two-phase aqueous system, in which EOPO (SDP35, molecular weight 2750) 5, 10, 15mL, water 10, 15, 20mL, dipotassium hydrogen phosphate 1.0, 1.5, 2.0g. Add 100 mg of crude chlorogenic acid to the aqueous phase system, mix well, and centrifuge at a speed of 2000r / min for 3 minutes to separate the organic phase (rich in EOPO) and the aqueous phase, and the chlorogenic acid is enriched in the organic phase (upper phase). Impurities are enriched in the aqueous phase.

[0045] 3) Temperature-induced aqueous two-phase separation: The organic phase (rich in EOPO) was subjected to temperature-induced phase separation. After 20 minutes in a water bath at 60°C, the so...

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Abstract

The invention relates to a method for separating and purifying chlorogenic acid by utilizing temperature to induce an aqueous two-phase system, which comprises the following steps: (1) smashing folium cortex eucommiae to be placed in an extracting tank, adding 5 to 7 times of water in weight, heating and back flowing for 1.5 to 2 h, and concentrating until paste is soaked, that is chlorogenic acid crude product; (2) mixing EOPO and water according to the volume ratio of (1-3):(1-4), then adding salt in the mixture, uniformly mixing, adding the chlorogenic acid crude product in the solution, uniformly mixing, centrifugally separating water phase and organic phase rich in EOPO, enriching chlorogenic acid in organic phase, and enriching impurity in water phase; (3) water bathing the organic phase gained in the step (2) at the temperature of 50 to 70 DEG C for 10 to 30 min, grouping the solution into two phases automatically, centrifugally separating the organic phase and the water phase, enriching the chlorogenic acid in water phase, and enriching EOPO in organic phase to be recycled; (4) cooling the obtained water phase to the room temperature, placing overnight, dissolving out crystal, and filtering to obtain chlorogenic acid pure product. The method is simple in technology and short in time consumption, reduces the material consumption, facilitates industrial pilot plant test enlargement, and is higher in yield coefficient.

Description

technical field [0001] The invention relates to a method for separating and purifying chlorogenic acid by using a temperature-induced two-phase system, and belongs to the technical field of biochemical industry. Background technique [0002] Chlorogenic acid is a depsipolic acid produced from caffeic acid and quinic acid, and is a phenylpropanoid compound. It has a high content in plants honeysuckle and Eucommia ulmoides, and is easily soluble in organic solvents such as water, ethanol, acetone, etc. The traditional extraction method uses isoamyl alcohol method and uses its acidic extraction. Since chlorogenic acid is a lipid formed from caffeic acid and quinic acid, it is easily hydrolyzed when extracted with acid and alkali, and the yield is not high. [0003] Patent document CN101781211A discloses a method for extracting chlorogenic acid in sunflower meal. In this method, sunflower meal is crushed, and cellulase with a concentration of 1% and protease with a concentratio...

Claims

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Application Information

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IPC IPC(8): C07C69/732C07C67/48C07C67/56
Inventor 霍清薛明德杨晓芳
Owner BIOCHEM ENG COLLEGE OF BEIJING UNION UNIV
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