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Multistage aqueous two-phase synchronous separation for geniposide and gardenia yellow

A technology of simultaneous separation and gardeniaside, which is applied in the separation/purification of carboxylic acid compounds, chemical instruments and methods, preparation of sugar derivatives, etc., can solve the problem of simultaneous extraction of gardenia yellow, etc. Efficiency and simple operation

Inactive Publication Date: 2015-11-11
SHAOYANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

We use isopropanol-salt two-phase system to extract gardenia fruit raw materials to produce gardenia yellow waste liquid to obtain geniposide crystals with a purity of more than 98.5%, and apply for a patent (patent number 201410721860.4), which has entered the stage of substantive examination. However, none of the reported methods for the extraction of geniposide using two-phase aqueous phases involves the simultaneous extraction of gardenia yellow.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] At room temperature, prepare 10 g of a two-phase system according to the mass percentage of ammonium sulfate and ethanol at 10%, take 1 ml of the concentrated gardenia crude extract, add it to the two-phase system, and stir with constant temperature magnetic force (20°C, 300r / min) For 40 minutes, the gardenia yellow and geniposide were enriched in the upper phase. Let stand for 60 minutes, and centrifuge at 2000 rpm for 30 minutes to separate the rich phase of geniposide and gardenia yellow. Then add this phase to the lower phase of the same two-phase system, and at room temperature, stir with constant temperature magnetic force (20°C, 300r / min) for 40min, and add 10w.% hydrochloric acid at the same time to make geniposide and gardenia yellow respectively Enriched in the lower phase and the upper phase, the enriched phase of geniposide and gardenia yellow is separated, and the upper phase containing gardenia yellow is concentrated and dried under vacuum rotation at -0.0...

Embodiment 2

[0018] At room temperature, 10 g of a two-phase system was prepared according to the mass percentage of sodium carbonate and isopropanol at 20%. Take 1 ml of the concentrated gardenia crude extract and add it to the two-phase system. min) for 40 min, enrich the gardenia yellow and geniposide in the upper phase. Let stand for 60 minutes, and centrifuge at 2000 rpm for 30 minutes to separate the rich phase of geniposide and gardenia yellow. Then add this phase to the lower phase of the same two-phase system, stir at constant temperature (20°C, 300r / min) for 40min at room temperature, add 30w.% hydrochloric acid to make geniposide and gardenia yellow rich Set in the lower phase and the upper phase, separate the enriched phase of geniposide and gardenia yellow, and the upper phase containing gardenia yellow is concentrated and dried under vacuum rotation at -0.04-0.09MPa, 45°C to obtain gardenia yellow The crude product was crystallized, and then recrystallized from acetone to ob...

Embodiment 3

[0020] At room temperature, 10 g of a two-phase aqueous system was prepared with potassium carbonate and propanol at a mass percentage of 30%, and 1 ml of the concentrated gardenia crude extract was added to the two-phase system, and magnetically stirred at a constant temperature (20°C, 300r / min) for 40 min, enrich the gardenia yellow and geniposide in the upper phase. Let stand for 60 minutes, and centrifuge at 2000 rpm for 30 minutes to separate the rich phase of geniposide and gardenia yellow. Add this phase to the lower phase of the same two-phase system, stir at constant temperature (20°C, 300r / min) for 40min at room temperature, and add 10w.% sulfuric acid to enrich geniposide and gardenia yellow respectively. Collected in the lower phase and the upper phase, the enriched phase of geniposide and gardenia yellow was separated. The upper phase containing gardenia yellow was concentrated and dried under the condition of -0.04-0.09MPa and 45°C in a vacuum to obtain a crude...

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Abstract

The invention relates to an extraction and separation method for geniposide and gardenia yellow with high yield and high purity. The invention provides a highly-efficient mild aqueous two-phase technology to realize synchronous separation and purification of the geniposide and the gardenia yellow. The method comprises the following steps: preparing gardenia extract by using gardenia fruit powder as a raw material, then subjecting the obtained gardenia extract to extraction and separation through a multistage low-molecular alcohol-salt aqueous two-phase system, carrying out concentration and drying so as to obtain primary geniposide and gardenia yellow crystals, and carrying out recrystallization so as to obtain geniposide crystal with purity of more than 98.5% and gardenia yellow crystal with a color value of 535. The method provided by the invention has the advantages of simple operation, greenness, high efficiency, economy, time conversation and facilitation to enlargement. Meanwhile, the method initiates application of an aqueous two-phase extraction technology in synchronous separation of the gardenia yellow and the geniposide, and improves separation and purification efficiencies of the geniposide and the gardenia yellow.

Description

technical field [0001] The invention belongs to the technical field of natural product active ingredient extraction, and specifically relates to a method for extracting geniposide and gardenia yellow from gardenia fruit powder with high yield and purity. Background technique [0002] Geniposide is an active ingredient in gardenia fruit, which has anti-oxidation and anti-inflammatory effects, and is widely used in medicine, health care, and biological detection. Geniposide is an iridoid compound, also known as geniposide. In the food industry, it can be mainly made into natural edible colorants gardenia blue and gardenia red. Gardenia Yellow is a mixture whose main ingredients include crocin, crocetin and geniposide. In addition to coloring, gardenia yellow pigment also has certain medical effects such as promoting blood circulation, eliminating phlegm, relieving pain, and lowering blood pressure. However, when the OD value of gardenia yellow is greater than 0.4, gardenia y...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/04C07H1/08C07C13/06C07C1/08C07C57/13C07C51/42
Inventor 张红萍郭晶莹
Owner SHAOYANG UNIV
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