Method for two-pot two stage countercurrent dynamic extraction of gardenia yellow pigment

A gardenia yellow pigment, countercurrent technology, applied in the direction of chemical instruments and methods, preparation of organic compounds, separation/purification of carboxylic acid esters, etc., can solve the problem of easy fading and greening of gardenia yellow pigment and the problem of gardenia oil It is easy to extract and clean, and the yellow pigment of gardenia is turbid, so as to reduce the loss of leachate, shorten the leaching time, and not easy to fade and turn green

Inactive Publication Date: 2016-06-15
江门市林业科学研究所
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  • Abstract
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Problems solved by technology

The disadvantages are (1) the large amount of ethanol is used, and the subsequent distillation and concentration consumes a lot of energy; (2) the extraction process is slow and the production capacity is small; (3) the gardenia yellow pigment is prone to fading and greening, and the overall loss is large; (4) the gardenia yellow The seed oil is not easy to extract, and the gardenia yellow pigment is turbid when used; (5) when refining the gardenia yellow pigment, the useful ingredients such as geniposide are not obtained together, resulting in waste

Method used

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  • Method for two-pot two stage countercurrent dynamic extraction of gardenia yellow pigment

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Experimental program
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Effect test

Embodiment 1

[0029] Such as figure 1 Shown, a kind of double-tank secondary countercurrent dynamic extraction method of gardenia yellow pigment comprises the following steps:

[0030] a. Grinding the shelled gardenia fruit to obtain a powder with a size of 80 meshes, using petroleum ether at 90-120°C as the extraction solvent, the ratio of solid to liquid is 1:6g / ml, and under the condition of 85°C, the petroleum ether is refluxed double Two-stage countercurrent dynamic leaching of tanks, each extraction time of each extraction tank is 1 hour, to obtain gardenia oil petroleum ether leaching solution and medicinal residue; the leaching solution is concentrated at 70-90°C to recover petroleum ether and obtain high-purity gardenia oil , adding an appropriate amount of petroleum ether with a boiling range of 60 to 90°C to the dregs to elute the gardenia oil to obtain degreasing gardenia powder;

[0031]B. with the 55% ethanol solution (55~65% ethanol solution specific gravity of 100kg degreas...

Embodiment 2

[0035] A method for dynamically extracting gardenia yellow pigment in double-tank secondary countercurrent, comprising the following steps:

[0036] a. Grinding the shelled gardenia fruit to obtain a powder with a size of 80 meshes, using petroleum ether at 90-120°C as the extraction solvent, the ratio of solid to liquid is 1:6g / ml, and under the condition of 85°C, the petroleum ether is refluxed double Two-stage countercurrent dynamic leaching of tanks, each extraction time of each extraction tank is 1 hour, to obtain gardenia oil petroleum ether leaching solution and medicinal residue; the leaching solution is concentrated at 70-90°C to recover petroleum ether and obtain high-purity gardenia oil , adding appropriate amount of petroleum ether at 60-90°C to the medicinal dregs to elute gardenia oil to obtain degreasing gardenia powder;

[0037] b. Add 100kg of oil-removed gardenia powder and 1012kg of 60% ethanol solution to extraction tank 1, the ratio of solid to liquid is 1...

Embodiment 3

[0041] A method for dynamically extracting gardenia yellow pigment with two-stage countercurrent in double tanks, is characterized in that it comprises the following steps:

[0042] a. Crush the shelled gardenia fruit to obtain a powder with a size of 80 meshes. Use petroleum ether at 90-120°C as the extraction solvent, and the ratio of solid to liquid is 1:6g / ml. Two-stage countercurrent dynamic leaching of tanks, each extraction time of each extraction tank is 1 hour, to obtain gardenia oil petroleum ether leaching solution and medicinal residue; the leaching solution is concentrated at 70-90°C to recover petroleum ether and obtain high-purity gardenia oil, medicinal dregs, adding appropriate amount of petroleum ether at 60-90°C to elute gardenia oil to obtain degreasing gardenia powder;

[0043] b. Add 100kg degreased gardenia powder and 1188kg65% ethanol solution into extraction tank 1, the ratio of solid to liquid is 1:12g / ml, the pH value is 6.0~8.0, the extraction tempe...

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Abstract

The invention discloses a method for two-pot two stage countercurrent dynamic extraction of a gardenia yellow pigment. The method comprises the following steps: 1, crushing decorticated cape jasmine fruits to obtain 80 mesh powder, and deoiling to obtain cape jasmine oil and deoiled cape jasmine powder; 2, adding an ethanol solution used as an extract solution to the deoiled cape jasmine powder, and carrying out ethanol refluxing two-pot two stage countercurrent dynamic extraction to respectively obtain a leachate 1, a leachate 1' and low-liquid medicine residues; 3, carrying out low temperature concentration on the above leachates to recover most of ethanol, and adding the obtained solution used as a sample solution to pretreated macro-porous adsorption resin to carry out column purification in order to obtain the purified gardenia yellow pigment, geniposide and chlorogenic acid; and 4, adding the low-liquid medicine residues to a proper amount of water, carrying out vacuum distillation condensation to recover water-containing ethanol, and stopping the vacuum distillation condensation until the concentration of ethanol in the medicine residues is lower than 5%. The method has the advantages of stable extraction process, no dead corners of materials in extraction pots, difficult fading and greening of the gardenia yellow, and high extraction efficiency.

Description

technical field [0001] The invention belongs to the technical field of natural pigment extraction, in particular to a method for dynamically extracting gardenia yellow pigment from gardenia fruits in double-tank secondary countercurrent flow. Background technique [0002] Gardenia, aliases: yellow gardenia, mountain gardenia, white toad, is the fruit of Rubiaceae gardenia. The fruit of gardenia is a traditional Chinese medicine, which belongs to the first batch of medicinal and edible resources promulgated by the Ministry of Health. There are also many yellow pigments in gardenia. This kind of yellow pigment is not only non-toxic and harmless, but also edible. It is a rare edible natural pigment and has almost all the effects of gardenia. It is very popular among people favorite. [0003] Gardenia yellow pigment is a rare water-soluble carotenoid. Its main components are crocetin and crocetin. Fading and greening will occur. [0004] The traditional process of extracting...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B61/00C07C67/48C07C67/56C07C69/732C07H17/04C07H1/08C11B1/10
CPCC09B61/00C07C67/48C07C67/56C07H1/08C07H17/04C11B1/102C07C69/732
Inventor 陈润强刘新华税珺梁日高马锡权刘一贞李妙嫦袁全孙
Owner 江门市林业科学研究所
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