Process for preparing jasminodin and genipin-1-beta-D-gentiobioside with cape jasmine fruit

A technology of gentiobioside and geniposide, which is applied in the field of medicine, can solve the problems of high loss of geniposide, cumbersome operation, and high price, and achieve the effect of being suitable for industrial production, overcoming cumbersome operation, and low cost

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

[0007] At present, traditional methods such as column chromatography and recrystallization are used to separate and purify effective monomers in gardenia fruit in the preparation of gardenia fruit at home and abroad. Such methods may require the use of toxic organic solvents, such as silica gel column chromatography using chloroform, Methanol can cause environmental pollution; or the cost is high and the operation is cumbersome, such as neutral alumina packing, which is expensive [Inouye H, et al.Chem Pharm Bull.1970, 18(5): 1066; Inouye H, et al.Phytochemistry .1974, 13: 2219; Endo T, et al.ChemPharm Bull.1973, 21(12): 2684], and the fixed relative sample has irreversible adsorption
There is also the separation and purification of geniposide by preparative liquid chromatography [Wang Lan, Zhang Jian. RP-HP...

Method used

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  • Process for preparing jasminodin and genipin-1-beta-D-gentiobioside with cape jasmine fruit
  • Process for preparing jasminodin and genipin-1-beta-D-gentiobioside with cape jasmine fruit
  • Process for preparing jasminodin and genipin-1-beta-D-gentiobioside with cape jasmine fruit

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1. Preparation of crude extract of gardenia fruit:

[0026] Take 500g of dried gardenia fruit medicinal powder, extract twice with 10 times of 50% ethanol reflux for 2 hours each time, filter, combine the filtrate, concentrate under reduced pressure at 60℃ to dilute extract, vacuum dry to obtain crude gardenia fruit extract The yield is 29.8%.

[0027] 2. Purification:

[0028] (1) Purification with macroporous adsorption resin: Take the above crude extract of Gardenia fruit, add water and suspend the total volume to 2000ml. Add 1500g pretreated 1300 macroporous adsorption resin chromatography column, and adsorb for 2 hours after loading. Elute with 6000ml water (discard). Then it was eluted with 6000ml 20% ethanol. After the ethanol eluted fraction was concentrated under reduced pressure, it was vacuum dried (60°C) to obtain 29.51g of extract powder with a yield of 5.9%. The geniposide and geniposide were detected by HPLC. The total content of Ping-1-β-D-gentioside is 95.3...

Embodiment 2

[0031] 1. Preparation of crude extract of gardenia fruit:

[0032] Take 500g of dried gardenia fruit medicinal powder, extract twice with 10 times the amount of water and reflux for 2 hours each time, filter, combine the filtrate, concentrate under reduced pressure at 60℃ to dilute extract, and vacuum dry to obtain a crude extract of gardenia fruit. The yield was 28.7%.

[0033] 2. Purification:

[0034] (1) Purification with macroporous adsorption resin: Take the above crude extract of Gardenia fruit, add water and suspend the total volume to 2000ml. Add to the chromatographic column containing 1500g pretreated AB-8 macroporous adsorption resin, and adsorb for 2 hours after loading the sample. Elute with 7000ml water (discard). Then eluted with 4000ml 30% ethanol. After the ethanol eluted fraction was concentrated under reduced pressure, it was vacuum dried (60℃) to obtain 32.88g of gardenia fruit macroporous adsorption resin extract powder (geniposide and genipin-1- β-D-gentiosi...

Embodiment 3

[0037] 1. Preparation of crude extract of gardenia fruit:

[0038] Take 500g of dried gardenia fruit medicinal powder, soak it with 10 times 50% ethanol and extract twice for 2 hours each time, filter, combine the filtrate, concentrate under reduced pressure at 60℃ to dilute extract, vacuum dry to obtain crude gardenia fruit extract The yield was 20.3%.

[0039] 2. Purification:

[0040] (1) Purification with macroporous adsorption resin: Take the above crude extract of Gardenia fruit, add water and suspend the total volume to 2000ml. Add 1500g pretreated 1300 macroporous adsorption resin chromatography column, and adsorb for 2 hours after loading. First eluted with 6000ml water (discarded). Then eluted with 8000ml 10% low-concentration ethanol, the ethanol eluted fractions were concentrated under reduced pressure, and then vacuum dried (60°C) to obtain 23.47g of gardenia fruit macroporous adsorption resin extract powder (geniposide and genipin- 1-β-D-gentioside accounted for 97.5...

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Abstract

The present invention relates to medicine technology, and is especially the preparation process of preparing high purity jasminodin and genipin-1-beta-D-gentiobioside through separating and purifying 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 great amount of water and then with low concentration ethanol solution; decompression concentrating to obtain the macroporous adsorbing resin extract of cape jasmine fruit; and final high speed liquid phase chromatographic and preparing liquid phase chromatographic separation to purify and obtain high purity jasminodin and genipin-1-beta-D-gentiobioside. The preparation process of the present invention has high separation efficiency, high product purity and simple operation, and is suitable for industrial production.

Description

Technical field [0001] The invention relates to the technical field of medicine, and is a method for separating and purifying high-purity geniposide and genipin-1-beta-D-gentioside from gardenia fruits. Background technique [0002] Gardenia, also known as Mountain Gardenia, is the fruit of the Rubiaceae plant Gardenia jasminoides Ellis. It is bitter in nature and non-toxic. Gardenia was first published in "Shen Nong's Materia Medica", which has the effects of promoting choleretics, promoting pancreatic secretion, lowering blood pressure, sedation, cooling, antibacterial and anti-inflammatory. Clinically, it is mainly used to treat children with fever, esophagitis and aphthous, sprain trauma, coronary heart disease, acute viral hepatitis hyperbilirubinemia, acute catarrhal conjunctivitis, etc. Its main chemical components are iridoids, flavonoids, triterpenes, organic acid esters, etc., in addition to d-glycosides, sterols, triterpene saponins, long-chain a...

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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