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Method for preparing natural pyrrole derivative from plant brassica rapa L. by extraction, purification and separation

A technology of pyrrole derivatives and turnips, applied in the field of natural product extraction, can solve problems such as low yield

Inactive Publication Date: 2013-05-01
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] It should be pointed out that the method of extracting and organically synthesizing 4-(formyl-5-hydroxymethyl-1hydro-pyrrol-1-yl)butyric acid from plants belongs to a different field, compared with organically synthesized bioactive substances, The same product extracted naturally tends to have a higher price in the market, but has a lower yield

Method used

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  • Method for preparing natural pyrrole derivative from plant brassica rapa L. by extraction, purification and separation
  • Method for preparing natural pyrrole derivative from plant brassica rapa L. by extraction, purification and separation

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Embodiment 1

[0024] 2. Add 5000ml of 75% ethanol aqueous solution with glacial acetic acid to adjust the pH value to 3.2, soak for 30 minutes, ultrasonically extract (180w, 25°C, 40kHz) for 30min, filter, add 5000ml of 75% ethanol aqueous solution to the filter residue, and then ultrasonicate (180w , 25°C, 40kHz) ultrasonic extraction for 30min, filter, discard the filter residue, combine the two extraction filtrates, and use a rotary evaporator to concentrate the filtrate to a viscous extract to obtain the extract extract;

[0025] 3. Dissolve the extract in 500ml of distilled water, add an equal volume of ethyl acetate to extract 4 times, combine the ethyl acetate extraction phase, evaporate under reduced pressure to remove the ethyl acetate solvent, and obtain 2.55g of crude product;

[0026] 4. Dissolve 200 mg of the crude product described in step 3 in 5 ml of water, and refine using preparative high performance liquid chromatography;

[0027] Chromatographic column packing: C18 bonde...

Embodiment 2

[0040] 2. Add 15000ml PH=5.0 hydrochloric acid aqueous solution and soak for 7 days, filter, discard the filter residue, and use a rotary evaporator to concentrate the filtrate to a viscous extract to obtain the extract extract;

[0041] 3. Dissolve the extract in 1000ml of distilled water, add an equal volume of ethyl acetate to extract 8 times, combine the ethyl acetate extract phase, evaporate under reduced pressure to remove the ethyl acetate solvent, and obtain 7.1g of crude product;

[0042] 4. Dissolve 300 mg of the crude product described in step 3 in 5 ml of water, and refine using preparative high performance liquid chromatography;

[0043] Chromatographic column packing: C8 bonded silica gel column (250mm*30mm)

[0044] The mobile phase A phase is: 20mmol / L ammonium formate aqueous solution with pH=6.4

[0045] The mobile phase B phase is: acetonitrile

[0046] The gradient program is: 0~5min, A: 2%, B: 98%

[0047] 5~15min, A: 15%, B: 85%

[0048] 15~20min, A...

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Abstract

The invention relates to a method for preparing a natural pyrrole derivative, namely 4-(formyl-5-hydroxymethyl-1H-pyrrol-1-yl) butanoic acid, from a plant brassica rapa L. by extraction, purification and separation, belonging to the field of natural product extraction. Currently, all domestic and overseas methods for naturally extracting 4-(formyl-5-hydroxymethyl-1H-pyrrol-1-yl) butanoic acid have the defects of low yield, triviality and complexity, high cost and the like. The invention provides a method for obtaining 4-(formyl-5-hydroxymethyl-1H-pyrrol-1-yl) butanoic acid with the purity of greater than 98% from the plant brassica rapa L. by extraction, purification and separation. The method for preparing the natural pyrrole derivative from the plant brassica rapa L. by extraction, purification and separation is significant to the deep processing and the added value promotion of the brassica rapa L; and the extraction method is simple to operate, the yield and the purity of products are high, and the cost is low.

Description

technical field [0001] The present invention relates to from plant turnip ( Brassica rapa L.) A method for preparing a natural pyrrole derivative, namely 4-(formyl-5-hydroxymethyl-1hydro-pyrrol-1-yl)butanoic acid, by extraction, separation and purification, belongs to the field of natural product extraction. Background technique [0002] Turnip ( Brassica rapa L.) is a plant of the genus Brassica in the family Brassicaceae ("Flora of China", volume 33). Turnip has a long history of use in traditional medicine and ethnic medicine in my country. The ancient name of turnip is fen, which was first recorded in "The Book of Songs", and its medicinal use was first recorded in "Famous Doctors". At present, turnip is widely cultivated in our country. It is mainly called "manjing" in the north, "pancai" in the southeast coastal area, "round root" in the Qinghai-Tibet plateau, and "Qamagu" in Xinjiang. , In Liangshan Prefecture, Sichuan alone, there is an annual output of more th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D207/333
Inventor 陈放彭彤郭亦然唐琳
Owner SICHUAN UNIV
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