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Process of preparing total iridoid glycoside with cape jasmine fruit

A technology for total iridoid glycosides and fruits, applied in the field of medicine, can solve the problems of complicated operation, reduced yield and high cost, and achieve the effects of simple preparation process, reduced elution and reduced loss

Inactive Publication Date: 2005-12-14
SECOND MILITARY MEDICAL UNIV OF THE PEOPLES LIBERATION ARMY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Commonly used purification methods include n-butanol extraction, neutral alumina column chromatography, silica gel column chromatography, etc. These methods may require the use of toxic organic solvents, such as n-butanol, which will cause environmental pollution; or the cost is high and the operation is cumbersome , such as neutral alumina filler, expensive
Adopting macroporous adsorption resin to purify Gardenia fruit extract [CN 1193766C "Gardenia total glycoside composition for treating hepatitis and its preparation method"; CN1546507A "A kind of Gardenia extract and its preparation process and its application"] can reduce It is cost-effective and does not pollute the environment. However, the commonly used elution method is to elute with a large amount of water first and then with high-concentration ethanol. Due to the excessive amount of water washing, there are a large amount of effective iridoid glycosides with strong polarity. loss and reduce the yield; and because it is easy to elute many weakly polar impurities with high-concentration ethanol and affect the purity, the active ingredient of iridoid glycosides in the extract is single, and the main component is geniposide, accounting for about 100% of the total. More than 90% iridoid glycosides; and it is necessary to further purify and remove impurities by means of the above-mentioned organic solvent extraction or column chromatography, so there are still defects such as polluting the environment or high cost

Method used

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  • Process of preparing total iridoid glycoside with cape jasmine fruit
  • Process of preparing total iridoid glycoside with cape jasmine fruit

Examples

Experimental program
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Effect test

Embodiment 1

[0015] 1. Preparation of gardenia fruit crude extract: take 500g of dried gardenia fruit medicinal material powder, extract twice with 10 times the amount of 50% ethanol under reflux, each time for 2 hours, filter, combine the filtrates, concentrate under reduced pressure at 60°C until dilute paste, and vacuum-dried to obtain the crude extract of Gardenia fruit, with a yield of 26.6%.

[0016] 2. Purification: take the above-mentioned gardenia fruit crude extract, add water and suspend, and the total volume is 2000ml. Add it to a 1300 macroporous adsorption resin chromatography column equipped with 1500 g of pretreated, and absorb for 2 hours after loading the sample. Elute with 1500ml of water (discard). Then eluted with 6000ml of 20% ethanol, and the ethanol eluted fraction was concentrated under reduced pressure, then vacuum-dried (60° C.) to obtain 46.59 g of total iridoid glycoside powder, with a yield of 9.3%. Gained powder is detected by ultraviolet spectrophotometry ...

Embodiment 2

[0018] 1. Preparation of crude gardenia fruit extract: Take 500 g of dried gardenia fruit medicinal material powder, extract twice with 10 times the amount of water, 2 hours each time, filter, combine the filtrates, concentrate under reduced pressure at 60°C to dilute extract, The crude extract of Gardenia fruit was obtained by vacuum drying with a yield of 28.7%.

[0019] 2. Purification: take the above-mentioned gardenia fruit crude extract, add water and suspend, and the total volume is 2000ml. Add it to a 1300 macroporous adsorption resin chromatography column equipped with 1500 g of pretreated, and absorb for 2 hours after loading the sample. Elute with 1500ml of water (discard). Then elute with 4000ml 30% ethanol, after the ethanol eluate fraction is concentrated under reduced pressure, vacuum-dry (60 ℃), obtain the total iridoid glycosides powder 49.30g, record the total iridoid glycosides purity to be 80.8%, The yield is 9.9%, and the content of geniposide is 64.8%. ...

Embodiment 3

[0021] 1. Preparation of gardenia fruit crude extract: Take 500g of dried gardenia fruit crude powder, soak and extract with 10 times the amount of 50% ethanol for 2 times, each time for 2 hours, filter, combine the filtrate, concentrate under reduced pressure at 60°C to dilute paste, and dried in vacuum to obtain the crude extract of Gardenia fruit, with a yield of 20.3%.

[0022] 2. Purification: take the above-mentioned gardenia fruit crude extract, add water and suspend, and the total volume is 2000ml. Add it to the chromatographic column equipped with 1500g pretreated AB-8 macroporous adsorption resin, and absorb for 2 hours after loading the sample. Elute with 1500ml of water (discard). Then elute with 8000ml 10% ethanol, after the ethanol eluate fraction is concentrated under reduced pressure, vacuum-dry (60 ℃), obtain total iridoid glycosides powder 40.62g, record total iridoid glycosides purity to be 89.2%, The yield is 8.1%, and the content of geniposide is 55.2%. ...

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Abstract

The present invention relates to medicine technology, and is especially the preparation process of preparing total iridoid glycoside with cape jasmine fruit. The preparation process includes soaking or refluxing cape jasmine fruit with water or water solution of ethanol to obtain coarse extract; eluting in macroporous adsorbing resin first with small amount of water and then with low concentration ethanol solution to purify; and decompression concentrating to obtain high purity total iridoid glycoside. The preparation process of the present invention has simple operation, low cost, high product purity, no environmental pollution and high yield, and is suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of medicine, and relates to a method for extracting total iridoid glycosides from gardenia fruits. Background technique [0002] Gardenia, also known as Gardenia jasmine, is the fruit of Gardenia jasminoides Ellis. Gardenia plants are cultivated in most parts of the country. There are wild species in various parts of the south, mainly distributed in Jiangxi, Hunan, Zhejiang, Fujian, Sichuan and other places. It was recorded as early as in "Shen Nong's Materia Medica", and since then it has been discussed and supplemented in herbal medicines and medical prescriptions of successive dynasties, such as "Bielu of Famous Doctors", Tao Hongjing's "Compendium of Materia Medica" and so on. Fructus Gardeniae is cold in nature, bitter in taste, and returns to the Heart, Liver, Lung, Stomach, and Sanjiao Meridians. It is often used for fever, upset, jaundice, red urine, bloody stranguria and p...

Claims

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Application Information

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IPC IPC(8): C07H17/04
Inventor 范国荣周婷婷柴逸峰吴玉田洪战英
Owner SECOND MILITARY MEDICAL UNIV OF THE PEOPLES LIBERATION ARMY
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