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Method for preparing high-purity geniposide from gardenia yellow pigment waste liquid

A technology for gardenia yellow pigment and gardeniside, which is applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems of failing to effectively recover the gardeniside environment, waste, pollute resources and the like, and achieve Improve the economic efficiency of enterprises, shorten time-consuming, and improve the effect of purity

Active Publication Date: 2018-11-13
郑州中科新兴产业技术研究院 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the problems existing in the prior art, the present invention provides a method for preparing high-purity geniposide from gardenia yellow pigment waste liquid, which mainly solves the problem of failure to effectively recover geniposide during the production process of gardenia yellow pigment. environmental pollution and waste of resources

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A method for preparing high-purity geniposide from gardenia yellow pigment waste liquid, the steps are as follows:

[0026] (1) Concentration of gardenia yellow pigment waste liquid: Take 2000mL of gardenia yellow pigment waste liquid with a 5% geniposide content, and concentrate under reduced pressure at -0.095MPa and 50°C to form an extract. The glycoside content is 30%;

[0027] (2) Resin separation of geniposide: Use HPA200A macroporous resin to dynamically adsorb geniposide to saturation at a column flow rate of 1BV / h; first wash the resin column with 12BV pure water, and discard the eluent; then use 10BV of 30% ethanol aqueous solution was used to elute geniposide, and the eluate was collected;

[0028] (3) Decolorization and impurity removal of the geniposide eluent: Add 15 g of activated carbon to the eluent for decolorization to obtain a geniposide decolorization liquid, which is concentrated under reduced pressure and spray-dried to obtain a crude geniposide;...

Embodiment 2

[0032] A method for preparing high-purity geniposide from gardenia yellow pigment waste liquid, the steps are as follows:

[0033] (1) Concentration of gardenia yellow pigment waste liquid: Take 1000mL of gardenia yellow pigment waste liquid with a geniposide content of 10%, and concentrate under reduced pressure at -0.06MPa and 80°C to form an extract. The glycoside content is 30%;

[0034] (2) Resin separation of geniposide: Use DM131 macroporous resin to dynamically adsorb geniposide to saturation at a column flow rate of 1BV / h; first wash the resin column with 12BV pure water, and discard the eluent; then use 70% ethanol aqueous solution of 5BV elutes geniposide, and collects the eluate;

[0035] (3) Decolorization and impurity removal of the geniposide eluent: Add 15 g of activated carbon to the eluent for decolorization to obtain a geniposide decolorization liquid, which is concentrated under reduced pressure and spray-dried to obtain a crude geniposide;

[0036] (4) R...

Embodiment 3

[0039] A method for preparing high-purity geniposide from gardenia yellow pigment waste liquid, the steps are as follows:

[0040] (1) Concentration of gardenia yellow pigment waste liquid: take 2000mL of gardenia yellow pigment waste liquid with 3% geniposide content, and concentrate under reduced pressure at -0.08MPa and 80°C to form an extract. The glycoside content is 30%;

[0041] (2) Resin separation of geniposide: Use DM131 macroporous resin to dynamically adsorb geniposide to saturation at a column flow rate of 1BV / h; first wash the resin column with 6BV pure water, and discard the eluent; then use The 70% ethanol aqueous solution of 6BV elutes geniposide, and collects the eluate;

[0042] (3) Decolorization and impurity removal of the geniposide eluent: Add 10 g of activated carbon to the eluent for decolorization to obtain a geniposide decolorization liquid, which is concentrated under reduced pressure and spray-dried to obtain a crude geniposide;

[0043] (4) Recr...

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Abstract

The invention discloses a method for preparing high-purity geniposide from gardenia yellow pigment waste liquid. The method comprises the following steps: by taking waste liquid obtained by purifyinggardenia yellow pigment by adopting a macroporous resin method as a raw material, enriching geniposide through vacuum concentration, filtering the material, and feeding obtained filtrate to macroporous resin; removing polar impurities adsorbed in the resin through water washing, then eluting geniposide in the resin through an ethanol solution, and collecting ethanol eluent; decoloring the eluent through active carbon, then performing vacuum concentration and drying treatment to obtain a geniposide coarse product, recrystallizing the geniposide coarse product through an anhydrous ethanol and ethyl acetate mixing solution to obtain the geniposide with the purity more than 98 percent. The method is easy and convenient to operate and favorable for industrial production; the geniposide can be efficiently recycled and is high in purity; the problem of resource waste caused by loss of effective components in a gardenia yellow production process is solved.

Description

technical field [0001] The invention belongs to the field of separation and purification of natural products, and in particular relates to a method for preparing high-purity geniposide from gardenia yellow pigment waste liquid. Background technique [0002] Gardenia is the dry and mature fruit of Gardenia jasminoides of the Rubiaceae family. Its shape is pointed and oblong, and the outer skin has five, seven, and nine edges. Gardenia is divided into mountain gardenia and water gardenia. The production areas of gardenia in my country are distributed in Zhejiang, Jiangxi, Fujian, Anhui, Hunan, Taiwan and other places. Gardenia was first recorded in the earliest surviving pharmacy monograph "Shen Nong's Materia Medica", and it was listed as a middle-grade product: "卮, the old name is Zhi⋯⋯, a tree Dan, born in Chuangu." It is recorded in the Chinese Pharmacopoeia and Materia Medica, " "The Book of Materia Medica" says: "Gardenia jasmine, clearing the heat of Shaoyin, the fiv...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/04C07H1/08
CPCC07H1/08C07H17/04
Inventor 聂毅海彬郑双双张赛陈昂白敬端
Owner 郑州中科新兴产业技术研究院