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Isolation and purification method of geniposide

A technology for separating and purifying gardenia glycosides, which is applied in the directions of organic chemistry, pharmaceutical formulations, and medical preparations containing active ingredients, etc., can solve the problems of waste of resources, unreasonable utilization of gardenia, and reduce the preparation cost and recovery rate. High and low energy consumption

Inactive Publication Date: 2007-09-19
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But every year tens of thousands of tons of gardenias in the whole country are not rationally utilized, wasting precious resources

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Use gardenia produced in Putian, Fujian as raw material, wash fresh gardenia with water, dry (air-dried, oven-dried or sun-dried), crush, and pass through a 16-40 mesh sieve to obtain gardenia powder. Put 2.7kg of gardenia powder into In the extraction tank, use 5 times the dry weight of gardenia powder (W / W) in 75% methanol aqueous solution, reflux extraction at 80°C for 1 hour, filter, and the filtrate is at -0.06~-0.095MPa, 50~80°C , the solvent was recovered under reduced pressure, and concentrated in vacuo to obtain the crude extract of geniposide.

[0034] Add distilled water to adjust the concentration of the extract to 3 degrees Baume, use HZ816 macroporous adsorption resin, and use 0.96 times the flow rate (V / V) of the resin volume / hour to dynamically adsorb the gardenia yellow pigment to saturation, and the leakage liquid is at -0.05 Under the conditions of ~-0.09MPa and 50~65℃, the solvent is recovered under reduced pressure, and the crude geniposide is obtai...

Embodiment 2

[0037] Put 2.6kg of degreased Gardenia powder of 16~40 meshes into the extraction tank, extract 2 times at 50°C with 25% aqueous methanol solution of 20 times the dry weight (W / W) of Gardenia powder, each time for 3 hours, combine the extracts, filter, the filtrate is under the conditions of -0.06~-0.095MPa, 50~80°C, recover the solvent under reduced pressure, and concentrate in vacuum to form the crude extract of geniposide, the concentration of the extract reaches 7.5 degrees Baume .

[0038] Under the condition of stirring speed of 68r / min, HZ801 macroporous adsorption resin was directly used to enrich and adsorb gardenia yellow pigment to saturation. The solvent was recovered under pressure and concentrated in vacuo to obtain crude geniposide.

[0039] Under the condition of 70°C, fully extract the geniposide in the crude geniposide with 3 times the amount (W / W) of ethyl acetate, separate the ethyl acetate extract, and slowly cool until the geniposide begins to precipitat...

Embodiment 3

[0041] Fresh gardenia was washed, crushed, and passed through a 10-30 mesh sieve, and 2.9kg of gardenia (in terms of dry weight, W / W) was put into the extraction tank, and 40 times of the dry weight of gardenia powder (W / W) was used % methanol-acetone (1:1) aqueous solution, reflux extraction at 68°C for 3 hours, filtered, and the filtrate was recovered under reduced pressure at -0.06~-0.095MPa, 50~80°C, and concentrated in vacuo to obtain Glycoside crude extract extract.

[0042] Add distilled water to adjust the extract concentration to 3 degrees Baume, use HZ806 macroporous adsorption resin, and use 0.59 times the resin volume / hour upper column flow rate (V / V), dynamically adsorb gardenia yellow pigment to saturation, and the leakage liquid is at -0.05 Under the conditions of ~-0.09MPa and 50~65℃, the solvent is recovered under reduced pressure, and the crude geniposide is obtained by vacuum concentration.

[0043] Under the condition of 62°C, use 5 times the amount (W / W) ...

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Abstract

The invention provides a separation method of the geniposide, including: extracting the geniposide from the Gardenia to produce a concrete with a hydrophilic organic water solution; removing the gardenia yellow pigment of the concrete by a large-hole adsorbed resin; depressed recovery of the solvent of the transudate, and concentrating to a coarse geniposide in vacuum; fully extracting the coarse product by hot ethylhexoate, cryogenic treatment of the extract, getting the geniposide crystal; crystallizing the ethylhexoate and acetone solvent and removing the impurities in room temperature; an obtaining the geniposide crystal with a purity >=98%. The invention separates the highly purified geniposide crystal. It has a cheap material, an easy and effective preparation craft, a broad extension and a novel design.

Description

technical field [0001] The invention relates to a green chemical production method for separating and purifying medicinal active ingredients from plants, and more particularly relates to a method for separating and purifying geniposide. Background technique [0002] Gardenia is the fruit of the evergreen shrub Gardenia (Gardenia) Rubiaceae (Rubiaceae), which is a large amount of traditional Chinese medicinal materials in China. The main medicinal ingredients of Lingling Injection, Longdan 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 abundant in Fujian, Zhejiang, Jiangxi, Huizhou, Mountainous areas in Hunan and other provinces. [0003] Gardenia has been recorded in famous medical works of all dynasties from "Compendium of Materia Medica" to "Chinese Pharmacopoeia". Oral administration of Gard...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/04A61K36/744
Inventor 陈剑锋陈浩郭养浩
Owner FUZHOU UNIV
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