Process of preparing high-purity jasminodin with Cape jasmine fruit

A technology of geniposide and fruit, applied in the field of medicine, can solve the problems of residual weak polar impurities, cumbersome operation, environmental pollution, etc., achieve the effects of reducing the interference of weak polar impurities, simple preparation process, and avoiding environmental pollution

Inactive Publication Date: 2005-12-14
SECOND MILITARY MEDICAL UNIV OF THE PEOPLES LIBERATION ARMY
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Problems solved by technology

[0005] At present, traditional methods such as column chromatography and recrystallization are used to separate and purify geniposide when preparing geniposide from gardenia fruits at home and abroad, such as silica gel column chromatography, alumina column chromatography and thin-layer chromatography [Inouye H, et al. al.Chem Pharm Bull.1970,18(5):1066; Inouye H, et al.Phytochemistry.1974,13:2219; Endo T, et al.Chem Pharm Bull.1973,21(12):2684; Li Lirong. Comparison of Geniposide Separation by TLC and Column Chromatography. Chinese Patent Medicine. 1999, 21 (12): 645], this type of method may need to use toxic organic solvents, such as chloroform and methanol, which will cause environmental pollution; or the cost is high and the operation Cumbersome, like neutral alumina filler, expensive
Although geniposide can also be prepared by preparative liquid chromatography [Wang Lan, Zhang Jian. Separation of geniposide monomers by RP-HPLC preparative chromatography. 2003, 25 (9): 764], its pretreatment method is cumbersome to operate , not suitable for large-scale industrial production
It has been reported in the literature that the separation of geniposide by macroporous resins has low cost and does not cause environmental pollution [Lv Maoping, Qiao Qingbin, etc. Research on the separation effect of macroporous resins on geniposide. 2002, 33(9): 794; CN 1546507A " A kind of gardenia extract and its preparation process and its application”; Jin Rixian, Guo Chunyan, etc. Study on the process of enriching geniposide in gardenia with macroporous adsorption resin. 2005, 11(3): 1] , but there are two commonly used elution methods at present. One is to elute directly with high-concentration ethanol after elution with water, which not only cannot remove iridoid glycosides with a slightly stronger polarity than Second, eluting directly with low-concentration ethanol and then eluting with high-concentration ethanol without washing with water will not only fail to remove water-soluble impurities, but also introduce more weakly polar impurities
Therefore, the purity of geniposide obtained by the existing method is relatively low, and it still needs to be further purified by the above-mentioned traditional separation method, and its application in production has certain limitations.

Method used

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  • Process of preparing high-purity jasminodin 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 6000ml of water (discard). Then eluted with 8000ml 10% ethanol (discarded), and finally eluted with 6000ml 20% ethanol. After the 20% ethanol eluted fraction was concentrated under reduced pressure, it was vacuum-dried (60° C.) to obtain 6.42 g of geniposide brown powder, The yield was 1.3%. The pur...

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 6000ml of water (discard). Then eluted with 8000ml 10% ethanol (discarded), and finally eluted with 4000ml 30% ethanol. After the 30% ethanol eluted fraction was concentrated under reduced pressure, it was vacuum-dried (60° C.) to obtain 7.48 g of geniposide brown powder, The yield was 1.5%. The purity of the powder was...

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 6000ml of water (discard). Then eluted with 8000ml 10% ethanol (discarded), and finally eluted with 6000ml 20% ethanol. After the 20% ethanol eluted fraction was concentrated under reduced pressure, it was vacuum-dried (60° C.) to obtain 5.36 g of geniposide brown powder, The yield was 1.1%. The purity of the po...

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Abstract

The present invention relates to medicine technology, and is especially the preparation process of preparing jasminodin 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 great amount of water and then with 10 % concentration ethanol solution to eliminate strong polar iridoid glycoside components and other impurities; selectively eluting jasminodin with low concentration ethanol solution; and decompression concentrating to obtain high purity jasminodin. 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 preparing high-purity geniposide from gardenia fruits. Background technique [0002] Gardenia, also known as Gardenia jasminoides, is the fruit of Rubiaceae Gardenia jasminoides Ellis. It is bitter and cold in nature and non-toxic. Gardenia was first recorded in "Shen Nong's Materia Medica", which has the effects of promoting choleresis, stimulating pancreatic secretion, lowering blood pressure, calming, cooling, antibacterial and anti-inflammatory. The main chemical components of Gardenia are iridoids, flavonoids, triterpenes, organic acid esters, etc., in addition to d-mannitol, sterols, triterpene saponins, long-chain alkanes, alcohols, and pigments, among which cycloalkenes The iridoid glycosides are its main active ingredients such as geniposide, genipin-1-β-D-gentiobioside, hydroxygeniposide, geniposide, gallizine methyl ester, deacetyla...

Claims

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Application Information

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Patent Type & Authority Applications(China)
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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