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Separation and purification method for geniposide

A technology for separation and purification of geniposide, applied in chemical instruments and methods, organic chemistry, preparation of sugar derivatives, etc., can solve the problems of human and environmental hazards, difficult handling, low yield, etc., and achieves simple methods and easy operations , the effect of improving efficiency

Inactive Publication Date: 2016-05-11
常州市鼎升环保科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The technical problem mainly solved by the present invention: when using common methods to separate and purify geniposide at present, although geniposide can be separated and purified, there are still many impurities, resulting in low yield and low purity, and the extraction The process is complex, difficult to handle, and requires the use of a large amount of toxic reagents, which is harmful to the human body and the environment. A method is provided to extract the juice from gardenia green fruit, extract it with rice wine, and dialyze and concentrate it. After being adsorbed and decolorized by a macroporous resin column, and crystallized with methyl ester, the geniposide crystals were redissolved in ethyl acetate, concentrated again, and finally the concentrated solution was added to an ice-water bath, recrystallized and dried to obtain The separation and purification method of geniposide

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0027]First, collect 500g of immature gardenia green fruit from the beginning of July to the beginning of August, put it into clear water, wash it repeatedly with the hands to remove the remaining dirt on the surface, put it in a juice extractor, and squeeze the juice for 15 minutes to obtain a pulp mixture; Pour the pulp mixture into a 1L beaker, and add rice wine with 1 times the mass of the pulp mixture into the beaker, place it in an ultrasonic oscillator, and vibrate for 1 hour at a frequency of 25KHz and a power of 120W. After the vibration is completed, filter, Remove the filter residue to obtain the filtrate; then put the obtained filtrate into a Soxhlet extractor, extract for 40 minutes, collect the filtrate extract, and move it into a distillation device, heat it in a water bath at 60°C for 35 minutes, and distill and remove the rice wine. Obtain the gardenia green fruit extract; Next, pour the gardenia green fruit extract obtained above into a dialysis bag made of a ...

example 2

[0030] First collect 550g of immature gardenia green fruit from the beginning of July to the beginning of August, put it into clear water, wash it with the hands repeatedly, remove the residual dirt on the surface, put it in a juice extractor, and squeeze the juice for 20 minutes to obtain a pulp mixture; Pour the pulp mixture into a 1L beaker, and add rice wine twice the mass of the pulp mixture into the beaker, place it in an ultrasonic oscillator, and vibrate for 1.5 hours at a frequency of 28KHz and a power of 160W. After the vibration is completed, filter , remove the filter residue, and obtain the filtrate; then put the above obtained filtrate into a Soxhlet extractor, extract for 43 minutes, collect the filtrate extract, and move it into a distillation device, heat it in a water bath at 65°C for 40 minutes, and distill and remove the rice wine , to obtain the gardenia green fruit extract; Next, pour the gardenia green fruit extract obtained above into a dialysis bag made...

example 3

[0033] First, collect 600g of immature gardenia green fruit from the beginning of July to the beginning of August, put it into clear water, wash it with the hands repeatedly, remove the remaining dirt on the surface, put it in a juice extractor, and squeeze the juice for 25 minutes to obtain a pulp mixture; Pour the pulp mixture into a 1L beaker, and add rice wine with 3 times the mass of the pulp mixture into the beaker, place it in an ultrasonic oscillator, and vibrate for 2 hours at a frequency of 30KHz and a power of 180W. After the vibration is completed, filter, Remove the filter residue to obtain the filtrate; then put the filtrate obtained above into a Soxhlet extractor, extract for 45 minutes, collect the filtrate extract, and move it into a distillation device, heat it in a water bath at 70°C for 45 minutes, and distill and remove the rice wine. Obtain the gardenia green fruit extract; Next, pour the gardenia green fruit extract obtained above into a dialysis bag made...

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Abstract

The invention discloses a separation and purification method for geniposide and belongs to the technical field of geniposide separation and purification. After green gardenia fruits are juiced, alcohol extraction is conducted with rice wine, dialysis concentration is conducted, then dialysis concentrated liquor is subjected to adsorption decoloring with a macroporous resin column and crystallized with methyl ester, geniposide crystals are re-dissolved in ethyl acetate, concentration is conducted again, finally, the concentrated liquor is added to an ice-water bath, re-crystallized and then dried, and the separation and purification method for geniposide is obtained. It is proved through an instance that operation is easy and convenient, no toxic reagent is added, environment friendliness is achieved, no impurity exists in prepared geniposide powder products, purity is larger than 98%, the product yield is larger than 97%, and the separation and purification method is suitable for industrial production.

Description

technical field [0001] The invention discloses a separation and purification method of geniposide, belonging to the technical field of separation and purification of geniposide. Background technique [0002] Gardenia is the fruit of Gardenia jasminoides, an evergreen shrub belonging to Rubiaceae. It is a large traditional Chinese medicinal material in China. The main medicinal ingredients of Xiegan Tablets and Yindan Pinggan Capsules are the first-choice drugs for the clinical treatment of jaundice hepatitis in traditional Chinese medicine and the raw materials for extracting natural pigments from gardenia. They are rich in mountainous areas in Fujian, Zhejiang, Jiangxi, Hui, Hunan and other provinces. [0003] Geniposide is a crystalline product extracted and refined from the dried and mature fruit of Gardenia jasminoides of the Rubiaceae plant by high-tech means. Its molecular weight is 388, and its appearance is white needle-like crystals. Water and methanol, ethanol and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/04C07H1/08
CPCC07H17/04C07H1/08
Inventor 许斌张帆
Owner 常州市鼎升环保科技有限公司
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