High purity separating and purifying method for naringin, syinaringin, hesperidin and neohesperidin

A technology for separation and purification of neohesperidin, which is applied in the field of separation and purification of active ingredients in traditional Chinese medicine, can solve the problems of irreversible adsorption, environmental pollution, time-consuming and labor-intensive, etc., and achieve large preparation volume, high separation efficiency, and avoid tailing phenomenon Effect

Inactive Publication Date: 2005-03-02
SECOND MILITARY MEDICAL UNIV OF THE PEOPLES LIBERATION ARMY
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Problems solved by technology

[0008] Using traditional separation and preparation methods such as ordinary column chromatography, recrystallization and high performance liquid chromatography to separate effective monomers in plants is not only time-consuming and laborious, but also pollutes the environment [C.L Ky, M.Noir

Method used

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  • High purity separating and purifying method for naringin, syinaringin, hesperidin and neohesperidin
  • High purity separating and purifying method for naringin, syinaringin, hesperidin and neohesperidin
  • High purity separating and purifying method for naringin, syinaringin, hesperidin and neohesperidin

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Embodiment 1

[0026] 1. Weigh 200g of the crude drug of Citrus aurantii, grind it into a coarse powder, put it in a 2000ml round bottom flask, add 1600ml of 60% ethanol, reflux extraction twice, each time for 1.5h, filter, combine the filtrate, and evaporate it under reduced pressure with a rotary evaporator ethanol (temperature 60°C) to obtain a water suspension.

[0027] 2. Take 500g of 905-type macroporous adsorption resin, soak it with 95% medicinal ethanol, make it fully swell, and then change the liquid several times until adding 1ml of ethanol soaking solution to 5ml of water does not show white turbidity. Pack the resin into a column (6.0×70 cm), and rinse the resin with distilled water until there is no alcohol smell.

[0028] 3. Add the water suspension obtained by extracting Fructus Fructus Aurantii to the pretreated chromatographic column, after adsorbing for a period of time, elute with water, 20% ethanol, and 70% ethanol in turn, receive the 70% ethanol eluate, and use Concen...

Embodiment 2

[0046] 1. Weigh 200g of Qingpi crude drug, grind it into a coarse powder, put it in a 2000ml round bottom flask, add 1600ml of 60% ethanol, reflux extraction twice, each time for 1.5h, filter, combine the filtrate, and use a rotary evaporator to evaporate the ethanol under reduced pressure (temperature 60° C.), to obtain extract.

[0047] 2. Take Qingpi extract and add 500ml of water to suspend it, degrease with petroleum ether twice, 500ml each time, separate the water layer, extract with n-butanol 3 times, each time 500ml, recover the n-butanol extract under reduced pressure To the extract, the obtained extract was vacuum-dried to obtain light yellow powder, weighing 15.8g, and the extraction rate was 7.9%.

[0048] 3. Use high-speed countercurrent chromatography (Shenzhen Tongtian Biochemical Co., Ltd.) to separate and purify the n-butanol extract of Qingpi.

[0049] The used solvent system and volume ratio of a crude extract separation and separation result are the same a...

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Abstract

The high speed countercurrent chromatographic process of separating and purifying naringin, syinaringin, hesperidin and neohesperidin includes the step 1 of compounding solvent system comprising fixed phase and flowing phase and including ethyl acetate, fatty alcohol and water, filling the column of chromatograph with the fixed phase, rotating the column, pumping the flowing phase into the column, leading in sample via the valve and accepting the target component based on detection spectrogram; and the step 2 of high speed countercurrent chromatographic separating and purifying the obtained matter in the step 1, with the solvent system comprising chloroform, fatty alcohol and water. The said process is suitable for the separation and purification of one or more of naringin, syinaringin, hesperidin and neohesperidin in natural product or extract in high efficiency and is simple and feasible.

Description

technical field [0001] The invention relates to a method for separating and purifying active ingredients of traditional Chinese medicines, more specifically, the invention relates to a method for separating and preparing high-purity naringin, naringin rutin, hesperidin and neohesperidin by high-speed countercurrent chromatography. Background technique [0002] Citrus aurantium is the dried immature fruit of Citrus aurantium L. and its cultivars of Rulaceae plant. There are three main types of chemical components: volatile oil, flavonoids and alkaloids, among which naringin, naringin, hesperidin and neohesperidin are its flavonoids. The main components, the structure is as follows. [0003] [0004] Naringin Neohesperidin [0005] [0006] Naringel Rutin Hesperidin [0007] Modern pharmacological research shows that flavonoids of Citrus aurantii have a wide range of pharmacological activities, such as anti-oxidation, ...

Claims

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Application Information

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IPC IPC(8): C07H1/06C07H17/07
Inventor 范国荣彭金咏吴玉田洪战英柴逸峰汪学昭
Owner SECOND MILITARY MEDICAL UNIV OF THE PEOPLES LIBERATION ARMY
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