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Method for separating and purifying geniposide by using isopropanol-salt double-aqueous-phase system

A two-phase system, separation and purification technology, applied in chemical instruments and methods, organic chemistry, preparation of sugar derivatives, etc., to achieve the effects of simple operation, improved efficiency, and easy scale-up

Inactive Publication Date: 2015-02-18
SHAOYANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Isopropanol has the advantages of low price, low toxicity, and low viscosity. Currently, the use of isopropanol as an extractant and inorganic salts to form a two-phase aqueous system to separate and purify geniposide has not been reported.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] At room temperature, 20 mL of a two-phase aqueous system was prepared according to the mass percentage of sodium carbonate and isopropanol at 10%, and 5 mL of concentrated gardenia yellow waste liquid was added to the two-phase aqueous system, and magnetically stirred at a constant temperature (10°C, 300 r / min) for 40 minutes. At the same time, adjust the pH=9 to enrich the geniposide, let it stand for 80 minutes, and centrifuge at 1500rpm for 30 minutes to separate the geniposide-rich phase, then concentrate and dry it under the condition of -0.06MPa and 20°C in a vacuum to obtain geniposide crystals Crude. Recrystallize with 8 times the volume of ethyl acetate to obtain geniposide crystals. The purity of geniposide was determined to be 98.5%, and the product yield reached 98.2%.

Embodiment 2

[0017] At room temperature, 20 mL of a two-phase aqueous system was prepared according to the mass percentage of sodium carbonate and isopropanol at 30%, and 5 mL of concentrated gardenia yellow waste liquid was added to the two-phase aqueous system, and magnetically stirred at a constant temperature (35°C, 300r / min) for 30 minutes. At the same time, adjust the pH=9 to enrich the geniposide, let it stand for 60 minutes, and centrifuge at 1000rpm for 20 minutes to separate the geniposide-enriched phase, then concentrate and dry it under the condition of -0.04MPa and 50°C in a vacuum to obtain geniposide crystals Crude. Recrystallize with 4 times the volume of petroleum ether to obtain geniposide crystals. The purity of geniposide was determined to be 96.7%, and the product yield reached 96.6%.

Embodiment 3

[0019] At room temperature, 20 mL of a two-phase aqueous system was prepared according to the mass percentage of sodium carbonate and isopropanol at 30%, and 5 mL of concentrated gardenia yellow waste liquid was added to the two-phase aqueous system, and magnetically stirred at a constant temperature (50°C, 300r / min) for 60 minutes. At the same time, adjust the pH to 12 to enrich geniposide, let it stand for 100 minutes, and centrifuge at 2000rpm for 40 minutes to separate the geniposide-rich phase, then concentrate and dry it under vacuum rotation at -0.09MPa and 90°C to obtain geniposide crystals Crude. Recrystallize with 10 times the volume of acetone to obtain geniposide crystals. The purity of geniposide was determined to be 96.9%, and the product yield reached 95.4%.

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Abstract

The invention relates to a method for separating and purifying geniposide by using an isopropanol-salt double-aqueous-phase system. The invention provides an efficient and gentle method for separating and purifying geniposide by using a double-aqueous-phase technique. The method comprises the following steps: producing a waste gardenia yellow liquid from a cape jasmine fruit raw material, performing extraction separation and concentration drying on the waste gardenia yellow liquid by using the isopropanol-salt double-aqueous-phase system, thereby obtaining a primary geniposide crystal product, and further recrystallizing, thereby obtaining geniposide crystal of which the purity is greater than 98.5%. By adopting the method, a natural geniposide product with high purity is separated and purified from a medical resource for both food and medicine. The method is simple and convenient to operate, environmentally friendly, high in efficiency, economical, time-saving and easy to amplify. The method is not only used for widening the double-aqueous-phase system for extracting geniposide and improving the efficiency in separating and purifying geniposide, but also is used for extracting and producing other pigments.

Description

technical field [0001] The invention belongs to the technical field of extracting active components of natural products, and in particular relates to a method for extracting geniposide with high yield and purity from gardenia fruit. 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 glycoside compound, also known as geniposide. In the food industry, it can be mainly made into natural edible colorants gardenia blue and gardenia red. Among the 56 kinds of blue pigments listed in my country's GB2760-2007 "Hygienic Standards for the Use of Food Additives", there are only two kinds of blue pigments: gardenia blue pigment and phycocyanin (ie, phycocyanin pigment). At present, the supply of natural blue pigment is in short supply in both domestic and foreign markets, so active development of high-e...

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 张红萍李婷李永斌
Owner SHAOYANG UNIV
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