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Method for preparing curcumin, demethoxycurcumin and bisdemethoxycurcumin

A technology of bis-demethoxycurcumin and demethoxycurcumin, applied in the field of phytochemistry, can solve the problem of not being able to obtain curcumin monomer pigments, etc., and achieve low solvent consumption, strong operability, and short process Effect

Inactive Publication Date: 2009-11-25
河北泽华生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this method is prepared through industrial chromatography, it still cannot obtain three monomeric pigments of curcumin, demethoxycurcumin and bisdemethoxycurcumin

Method used

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  • Method for preparing curcumin, demethoxycurcumin and bisdemethoxycurcumin
  • Method for preparing curcumin, demethoxycurcumin and bisdemethoxycurcumin
  • Method for preparing curcumin, demethoxycurcumin and bisdemethoxycurcumin

Examples

Experimental program
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Effect test

Embodiment 1

[0031] aContinuous countercurrent extraction: Grind turmeric (purchased from Myanmar) into turmeric powder of 40-60 meshes, weigh 4.0 kg, and conduct continuous countercurrent extraction with 16L80% methanol-HCl aqueous solution with a pH value of 5.0 at room temperature for 4 hours and then filter. Gained filtrate is concentrated under reduced pressure (-0.08~0.1Mpa) at 60 ℃ to a relative density of 0.9 to obtain 200 grams of curcumin oleoresin;

[0032] B chromatographic separation: the above-mentioned curcumin oleoresin is loaded on the chromatographic column top of HZ-816 chromatographic resin (resin volume is 6L), the chromatographic column column length is preferably 500~1200mm, and the chromatographic column column length of this embodiment is 1000mm , The chromatographic column inner diameter is preferably 80~160mm, and the present embodiment chromatographic column inner diameter is 140mm, and the mass ratio of the loading amount of curcumin oleoresin and chromatographi...

Embodiment 2

[0034] Embodiment 2: the difference between this embodiment and embodiment 1 is that

[0035] aContinuous countercurrent extraction: After turmeric (purchased from Myanmar) is crushed into 40-60 mesh turmeric powder, 5.0 kg is weighed, and 20L80% methanol-HCl water with a pH value of 5.0 is used for continuous countercurrent extraction at room temperature for 6 hours and then filtered. The filtrate was concentrated under reduced pressure (-0.08~0.1Mpa) at 60°C to a relative density of 1.2 to obtain 250 grams of curcumin oleoresin.

[0036]b Chromatographic separation: the above-mentioned curcumin oleoresin is loaded on the top of the chromatographic column of HZ-818 chromatographic resin (resin volume is 8L), and the length of the chromatographic column is 1000mm, and the inner diameter is 110mm. The mass ratio of the amount of curcumin oleoresin loaded to the chromatographic separation medium was 1:100 (W / W). Then use mobile phase volume concentration as 50% ethanol water so...

Embodiment 3

[0038] aContinuous countercurrent extraction: After crushing turmeric (purchased from Myanmar) into 40-60 mesh turmeric powder, weigh 10.0 kg, carry out continuous countercurrent extraction with 40L80% ethanol-HCl aqueous solution with a pH value of 5.0 at room temperature for 5 hours and then filter , the filtrate was concentrated under reduced pressure (-0.08~0.1Mpa) at 60°C to a relative density of 1.1 to obtain 500 grams of curcumin oleoresin.

[0039] b Chromatographic separation: the above-mentioned curcumin oleoresin is loaded on the top of the chromatographic column of HZ-801 chromatographic resin (resin volume is 16L), the length of the chromatographic column is 1200mm, and the inner diameter is 200mm. The mass ratio of the amount of curcumin oleoresin loaded to the chromatographic separation medium was 1:100 (W / W). Then use the mobile phase volume concentration as 50% methanol water, 80% methanol water and 90% methanol water gradient elution, each elution volume is 4...

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Abstract

The present invention discloses a method for preparing curcumin, demethoxycurcumin and bisdemethoxycurcumin, which comprises the following steps: continuously executing countercurrent extraction to the turmeric with the methanol-acid solution or ethanol-acid solution, after filtering the extracted solution, condensing into the oleoresin with the relative density of 0.9-1.2; placing the oleoresin on the chromatographic separation medium for gradient elution, and after fraction-collecting the eluent, respectively obtaining the curcumin crystal, demethoxycurcumin crystal and bisdemethoxycurcumin crystal after condensing. The invention adopts a technique in which HZ-816, HZ-818 or HZ-801 is used as the chromatographic separation medium and the alcohol-water is used as the elution solvent. Three monomeric compounds of curcumin, demethoxycurcumin and bisdemethoxycurcumin are simultaneously obtained. The purity of each monomeric compound is more than 95%, and the recovery rate of the sample is more than 70%. The method of the invention further has the advantages of less intercrossing of compounds in the separation process, short flow path, strong operability, low consumption of the solvent, high extraction rate and excellent stability of the extraction solution. Furthermore the obtained product can be widely applied for the fields of medicament, food, etc., and is suitable for large-scale production.

Description

technical field [0001] The invention belongs to the field of phytochemistry, and in particular relates to a separation and purification method for preparing high-purity curcumin, demethoxycurcumin and bisdemethoxycurcumin from turmeric. Background technique [0002] Curcumin is a phenolic pigment extracted from the rhizome of the genus Curcuma longa in the family Zingiberaceae. Due to its stable color and low toxicity (LD50 > 2g / kg in mice), it has been widely used in food additives and dyes. middle. The yellow substance of turmeric is a slightly acidic phenolic substance, mainly containing 3 main components: curcumin I (47%); curcumin II, namely demethoxycurcumin (17%); curcumin III, namely bis Demethoxycurcumin (36%) has anti-tumor, anti-inflammatory, anti-oxidation and hypolipidemic effects, and its structural formula is as follows: [0003] [0004] curcumin [0005] [0006] Demethoxycurcumin [0007] [0008] Bisdemethoxycurcumin [0009] Preliminary s...

Claims

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Application Information

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IPC IPC(8): C07C49/255C07C49/248C07C45/79C09B61/00A23L1/275A61P35/00A61P29/00A61P39/06A61P3/06A23L5/43A23L5/47
Inventor 王辉樊书旗杨贵国张彬
Owner 河北泽华生物科技有限公司
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