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Method for separating and purifying bergamottin from Zaoxiang pomelo oil cell layer

A technology for the separation and purification of bergamot, applied in organic chemistry, etc., can solve the problems of waste of resources, discarded pomelo peel, environmental pollution, etc., and achieve the effects of short production cycle, high recovery rate, and guaranteed accuracy

Active Publication Date: 2017-11-24
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Pomelo is a kind of fruit that is abundant in southern my country. However, the pomelo peel, which accounts for 43% to 48% of the whole fruit, is usually discarded during fresh eating or food processing, which not only causes serious waste of resources, but also causes environmental pollution.

Method used

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  • Method for separating and purifying bergamottin from Zaoxiang pomelo oil cell layer
  • Method for separating and purifying bergamottin from Zaoxiang pomelo oil cell layer
  • Method for separating and purifying bergamottin from Zaoxiang pomelo oil cell layer

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Embodiment 1

[0019] Embodiment 1: the present invention carries out the screening determination of influence factor by following test

[0020] 1. Selection of purification materials

[0021] Freeze-dry the collected oil cell layers of 7 pomelo species and grind them into fine powder with a grinding jar. Accurately weigh a certain amount of freeze-dried powder, use petroleum ether (60-90°C) to ultrasonically extract twice at a solid-to-liquid ratio of 1:20, filter and combine the two filtrates, evaporate the filtrate to dryness, and then dissolve the obtained extract in An appropriate amount of chromatographic methanol is used for HPLC analysis of bergamot. HPLC mobile phase includes pure water (A) and chromatographic acetonitrile (B), using 0-1min: 10% B, 1-5min: 10-80% B, 5-10min: 80% B, 10-12min: 80-95 %B,12-15min:95%B,15-19min:95-10%B,19-21min:10%B gradient elution, flow rate is 1ml / min, stationary phase is Waters C18 analytical column (4.6×250 mm, 5 μm), the column temperature is ...

Embodiment 2

[0033] The operating method of the separation and purification bergamot element of the present invention is carried out according to following three steps:

[0034] see figure 1 , (1) Weigh 80g of pomelo oil cell layer freeze-dried powder, add petroleum ether (60-90°C) and ultrasonically extract twice at a solid-to-liquid ratio of 1:20, filter and combine the two filtrates, and put them on a rotary evaporator Evaporate to dryness to obtain the medicinal extract, mix the sample with an appropriate amount of silica gel, evaporate to dryness and make loading powder, pack the column according to the ratio of 1g:50g between the loading amount and the silica gel consumption, add petroleum ether-acetic acid to the silica gel column after adding the loading powder Ethyl ester (13:1) solution eluted bergamot, combined the eluent containing bergamot, and evaporated to dryness on a rotary evaporator at 40°C to obtain 74.6 mg of crude silica gel extract, the content of bergamot in the cru...

Embodiment 3

[0037] The operating method of the separation and purification bergamot element of the present invention is carried out according to following three steps:

[0038] see figure 1, (1) Weigh 90g of pomelo oil cell layer freeze-dried powder, add petroleum ether (60-90°C) and ultrasonically extract twice at a solid-to-liquid ratio of 1:20, filter and combine the two filtrates, and put them on a rotary evaporator Evaporate to dryness to obtain the medicinal extract, mix the sample with an appropriate amount of silica gel, evaporate to dryness and make loading powder, pack the column according to the ratio of 1g:50g between the loading amount and the silica gel consumption, add petroleum ether-acetic acid to the silica gel column after adding the loading powder Ethyl ester (13:1) solution eluted bergamot, combined the eluent containing bergamot, and evaporated to dryness on a rotary evaporator at 40°C to obtain 83.2 mg of crude silica gel extract, the content of bergamot in the crud...

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Abstract

The invention provides a method for separating and purifying bergamottin from a Zaoxiang pomelo oil cell layer. A silica gel column chromatography and HSCCC (high-speed countercurrent chromatography) combined technology is used; the Zaoxiang pomelo oil cell layer freezing dry powder is used as raw materials; silica gel crude extract powder is firstly prepared; then, through the further separation and purification by HSCCC, high-purity bergamottin is obtained. The process is simple; inert gas protection, high temperature and high pressure are not needed; the production period is short; the flow process is safe; the operation is easy; the HPLC (high performance liquid chromatography) is used in the whole process, so that precise and quantitative effects are achieved; the accuracy is high; extracts and solvents used by the HSCCC can be repeatedly used after the recovery; the cost is low. The method has the advantages that the purity of the purified product is high; the recovery rate is high; the purity of the bergamottin obtained through the final purification is greater than or equal to 94 percent; the method is applicable to scientific research and industrial production.

Description

technical field [0001] The invention belongs to the technical field of extraction, separation and purification of active ingredients in natural plants, and in particular relates to a method for separating and purifying bergamot from pomelo oil cell layer, which uses the pomelo oil cell layer as raw material and uses silica gel A method for separating and purifying bergamot with column and HSCCC combined technology. Background technique [0002] Bergamot (bergamottin), alias bergamot pavilion, bergamot pavilion, bergamot, molecular formula: C 21 h 22 o 4 , molecular weight: 338.40, CAS number: 7380-40-7, exists in bergamot, pomelo, grapefruit and other citrus fruits and some traditional Chinese medicinal materials such as notopterygium, insoluble in water, soluble in methanol, ethanol, ethyl acetate and other organic solvents. The structural formula is as follows: [0003] [0004] Bergamotin is a natural furanocoumarin compound. Pharmacological activity studies have...

Claims

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Application Information

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IPC IPC(8): C07D493/04
CPCC07D493/04
Inventor 李鲜刘意隆孙崇德
Owner ZHEJIANG UNIV
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