Method for extracting high-purity nobiletin from citrus peels

A technology of nobiletin and citrus, which is applied in the field of extracting high-purity nobiletin, which can solve the problems of high preparation cost and expensive equipment, and achieve the effects of no production equipment, low cost and short production cycle

Active Publication Date: 2013-01-16
SHAANXI HUIKE BOTANICAL DEV CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The chromatographic preparation mainly includes methods such as supercritical fluid chromatography, high-efficiency preparation chromatography, and high-speed countercurrent chromatography to prepare high-purity nobiletin, but these methods are expensive in equipment and high in preparation costs.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Step 1, 1 kg of dried orange peel is pulverized and extracted 3 times with 85% ethanol (or 85% methanol) in mass concentration, combined with 3 filtrates after filtration, and concentrated under reduced pressure to a specific gravity of For the concentrated solution of 1.1, the ethanol (or methanol) used for each reflux extraction is 20kg, the time of each reflux extraction is 2h, and the temperature of each reflux extraction is 70°C;

[0023] Step 2. Add water 5 times the volume of the concentrated solution to the concentrated solution described in step 1, and then add hydrochloric acid with a mass concentration of 0.1% to the concentrated solution after adding water (it can be replaced by sulfuric acid or phosphoric acid with a mass concentration of 0.1%) Until the pH value of the system is 5, stir evenly and let it stand for 24 hours, discard the supernatant to obtain a precipitate, wash the precipitate once with water, centrifuge, collect the solid, and obtain the cr...

Embodiment 2

[0029] Step 1, after crushing 1 kg of dried orange peel, use 40% ethanol (or 50% methanol) for reflux extraction for 3 times, filter and combine the filtrates for 3 times, and concentrate the combined filtrate under reduced pressure to a specific gravity of For the concentrated solution of 1.0, the ethanol (or methanol) used for each reflux extraction is 10kg, the time of each reflux extraction is 1h, and the temperature of each reflux extraction is 85°C;

[0030] Step 2: Add water 3 times the volume of the concentrated solution to the concentrated solution described in step 1, and then add sulfuric acid with a mass concentration of 5% to the concentrated solution after adding water (it can be replaced by hydrochloric acid or phosphoric acid with a mass concentration of 5%) Until the pH value of the system is 3, stir evenly and let it stand for 18 hours, discard the supernatant to obtain a precipitate, wash the precipitate with water for 3 times, centrifuge, collect the solid, ...

Embodiment 3

[0036] Step 1: Grind 1 kg of dried orange peel and extract it twice with absolute ethanol (or absolute methanol) under reflux. After filtering, combine the filtrate twice, and concentrate the combined filtrate under reduced pressure to a concentrated solution with a specific gravity of 1.05. Reflux each time The absolute ethanol (or anhydrous methanol) used for extraction is 5kg, the time of each reflux extraction is 2h, and the temperature of each reflux extraction is 80°C;

[0037] Step 2, in the concentrated solution described in step 1, add the water of 1 times of concentrated solution volume, then add the sodium hydroxide solution that mass concentration is 2% in the concentrated solution after adding water (available mass concentration is the hydroxide of 2% Calcium solution, sodium carbonate solution or sodium bicarbonate solution) until the pH value of the system is 8, stir evenly and let it stand for 12 hours, discard the supernatant to obtain a precipitate, wash the p...

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PUM

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Abstract

The invention discloses a method for extracting high-purity nobiletin from citrus peels. The method comprises the following steps: 1, carrying out reflux extraction of crushed dry citrus peels for 2 to 4 times, combining the filtrate after filtration, and concentrating under reduced pressure to obtain a concentrated solution; 2, adding water into the concentrated solution, then adding an acidic solution or an alkaline solution till the pH value of the system ranges from 3 to 9, standing for removal of the supernatant to obtain a sediment, settling and washing the sediment, centrifuging, and collecting solid to acquire a polymethoxylated flavonoids crude product; 3, conducting ungrease treatment; 4, using an organic solvent to achieve reflux dissolution of the polymethoxylated flavonoids crude product which is subject to ungrease treatment, then adding activated charcoal for reflux decoloration, filtering, standing the concentrated filtrate for crystallization, and filtering the crystallized filtrate to obtain a nobiletin crude product; and 5, recrystallizing to obtain the high-purity nobiletin of which the quality purity is not less than 98 percent. The method provided by the invention has the characteristics of simplicity, feasibility, short production period, no need of expensive production equipment, low cost and the like, and is easy for realizing industrial production of high-purity nobiletin.

Description

technical field [0001] The invention belongs to the technical field of extraction of effective plant components, and in particular relates to a method for extracting high-purity nobiletin from citrus peels. Background technique [0002] Nobiletin (Nobiletin) is a polymethoxylated flavonoid compound unique to the peel of Citrus (Citrus) plants in the family Rutaceae. Nobiletin has a wide range of biological and pharmacological activities, and is used in many fields such as medicine, health care products, cosmetics, and food. Modern medical research shows that nobiletin has a series of effects such as anti-cancer, anti-oxidation, anti-inflammation, anti-mutagenesis, cardiovascular protection, and inhibition of atherosclerosis. Nobiletin has a strong inhibitory effect on malignant tumor cells such as liver cancer, lung cancer, melanoma, squamous cell tumor, and gliosarcoma. At the same time, foreign studies have shown that nobiletin is a new MEK (active mitotic Original prote...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/30C07D311/40
Inventor 阮娜张华陈卫飞魏亚娟
Owner SHAANXI HUIKE BOTANICAL DEV CO LTD
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