Method for extracting and producing high-purity xanthohumol from residues generated by extracting hops by carbon dioxide

A carbon dioxide and xanthohumol technology, applied in the separation/purification of carbonyl compounds, organic chemistry, etc., can solve the problems of low sample processing capacity, high production cost, and no industrialization, and achieve simple equipment and high product purity. Effect

Active Publication Date: 2011-09-14
YUMEN TUOPU SCI & TECH DEV CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the method of purifying high-purity xanthohumol in foreign countries mainly adopts the method of preparing liquid chromatography. The patent 200810079205.8 applied by Yang Xiaolan and others of Shanxi University in China uses the method of countercurrent chromatography to prepare high-purity xanthohumol, because the ability to process samples is too small , unable to realize industrialized production; the patent 200810225869.0 and the US patent USP6867332 applied by Gu Fanghong and others of the China Food and Fermentation Industry Research Institute all adopt the method of diatomite adsorption and elution to prepare high-purity xanthohumol, but this method has not yet been industrialized; Guilin The Chinese patent 200810073983.6 applied by Rhine Biotechnology Co., Ltd. uses adsorption resin to purify xanthohumol to more than 90%, but there is no product or sample on the market; the Chinese patent 200910117234.3 applied by the applicant also uses adsorption resin to enrich xanthohumol ; Chinese patent 201010167119.X applied by the applicant obtains high-purity xanthohumol, which is suitable for small-scale production, and the product has been sold on the market, but the production cost is too high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] ① Extract hop residue with 100 kg of carbon dioxide, add 1000 kg of water, adjust and keep the pH value of the solution at 8-10 with lye, stir and wash and filter out the washing liquid, so that the organic acid, residual hop acid, tannin and other substances in the hop residue be removed. The number of washes is 2 times.

[0025] ②Use 600 liters of 50% (volume percentage concentration) alcohol to extract the washed carbon dioxide to extract the hop residue, keep the system temperature at 15-25°C during the extraction process, keep the pH value of the system at 8-10 with lye, and the extraction time For 1 hour, leaching 2 times under the same conditions.

[0026] ③ 1250 liters of leaching solution collected by filtration, neutralized to pH = 6, under reduced pressure distillation at -0.03 to -0.09MPa to recover alcohol, leaving 400 liters of turbid solution. After cooling to room temperature, the solid was collected by filtration and separation. Undried solid weight ...

Embodiment 2

[0034] ① Extract hop residue with 100 kg of carbon dioxide, add 1500 kg of water, adjust with lye and keep the pH of the solution at 8-10, stir and wash and filter out the washing liquid, so that the organic acid, residual hop acid, tannin and other substances in the hop residue be removed. Wash times 1 time.

[0035] ②Use 600 liters of 60% (volume percentage concentration) methanol aqueous solution to extract the washed carbon dioxide extraction hop residue, keep the system temperature at 15-20°C during the extraction process, keep the pH value of the system at 8-10 with lye, and extract The time is 1 hour, leaching twice under the same conditions.

[0036] ③ Filter and collect 1200 liters of leaching solution, neutralize to pH = 6, and recover methanol by distillation under reduced pressure at -0.03 to -0.09 MPa, leaving 500 liters of turbid solution. After cooling to room temperature, the solid was collected by filtration and separation. Undried solid weight 2.7 kg.

[...

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PUM

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Abstract

The invention relates to a method for extracting and producing high-purity xanthohumol from residues generated by extracting hops by carbon dioxide, and belongs to the field of fine chemical industry. The method comprises the following steps of: extracting, recrystallizing, distilling under reduced pressure, heating for dissolving, and the like. Equipment is simple, product purity is between 95 and 99 percent, and the method is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of fine chemicals, and in particular relates to an industrial production method for extracting xanthohumol from hop residue extracted with carbon dioxide and refining it to obtain high-purity xanthohumol. Background technique [0002] After carbon dioxide extracts hops, the residue can be used as feed, but the residue still contains a large amount of polyphenols and flavonoids. Recent studies have shown that these substances have a wide range of physiological and pharmacological activities, including choleretic, anti-ulcer, and protective. Liver, diuretic, anti-viral, anti-cancer and anti-cancer, estrogen effect, etc. In particular, xanthohumol needs to be mentioned. Studies in recent years have shown that xanthohumol induces the catalytic activity of carcinogenic detoxification enzymes by inhibiting the enzymatic activity of the conversion of pre-carcinogens to carcinogens, and inhibits the growth of cancer cells in ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/84C07C45/81
Inventor 刘启民马连清孟立花刘英范玉芳汤学芬
Owner YUMEN TUOPU SCI & TECH DEV CO LTD
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