Method for extracting chlorogenic acid and neochlorogenic acid from bunge pricklyash leaves

A technology of new chlorogenic acid and chlorogenic acid, which is applied to the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds, etc., can solve the problems of unseen preparation of chlorogenic acid and new chlorogenic acid, and achieve convenient operation , The effect of simple process

Inactive Publication Date: 2014-09-03
SICHUAN UNIV
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

At present, there are no patent documents and non-patent literature reports on the preparation of chlorogenic acid and neochlorogenic acid from Zanthoxylum bungeanum leaves

Method used

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  • Method for extracting chlorogenic acid and neochlorogenic acid from bunge pricklyash leaves
  • Method for extracting chlorogenic acid and neochlorogenic acid from bunge pricklyash leaves
  • Method for extracting chlorogenic acid and neochlorogenic acid from bunge pricklyash leaves

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] (1) Grind 10 g of dried Zanthoxylum bungeanum leaves, with an average particle size of 600 μm, then use 300 mL of methanol with a concentration of 80 wt % as an extractant, shake at room temperature for 36 hours, separate the supernatant, and concentrate and dry the supernatant to obtain methanol extract ;

[0040](2) Disperse the above-mentioned methanol extract in 90ml distilled water, the ratio of solid to liquid is 1g: 30mL, then use 180mL ethyl acetate to shake and extract twice, collect the aqueous phase extract, concentrate and dry, and obtain 2.58g of dried sample, the yield 25.8%;

[0041] (3) Take 1 g of the above-mentioned dried sample, dissolve it in 10 mL of distilled water, put it on a reversed-phase resin SciBioChem MCI-GEL chromatography column, the filler height is 20 cm, and the column diameter is 3.2 cm, and it is eluted with methanol-water gradient, and the concentration is 0 wt%. , 10wt%, 20wt%, 30wt%, 40wt%, 50wt% methanol, the elution flow rate i...

Embodiment 2

[0046] (1) Grind 10 g of dried Zanthoxylum bungeanum leaves, with an average particle size of 500 μm, then use 200 mL of methanol with a concentration of 70 wt % as an extractant, shake at room temperature for 30 h, separate the supernatant, and concentrate and dry the supernatant to obtain methanol extract ;

[0047] (2) Disperse the above-mentioned methanol extract in 50ml of distilled water, the ratio of solid to liquid is 1g: 20mL, then use 100mL of ethyl acetate to shake and extract twice, collect the aqueous phase extract, concentrate and dry, and obtain 2.12g of the dried sample, the yield 21.2%;

[0048] (3) Take 1 g of the above-mentioned dried sample, dissolve it in 10 mL of distilled water, put it on a reversed-phase resin SciBioChem MCI-GEL chromatography column, the filler height is 20 cm, and the column diameter is 3.2 cm, and it is eluted with methanol-water gradient, and the concentration is 0 wt%. , 10wt%, 20wt%, 30wt%, 40wt%, 50wt% methanol, the elution flow...

Embodiment 3

[0053] (1) Grind 10 g of dried Zanthoxylum bungeanum leaves, with an average particle size of 500 μm, then use 100 mL of methanol with a concentration of 60 wt % as an extractant, shake at room temperature for 24 hours, separate the supernatant, and concentrate and dry the supernatant to obtain methanol extract ;

[0054] (2) Disperse the above-mentioned methanol extract in 25ml of distilled water, the ratio of solid to liquid is 1g: 10mL, then shake and extract once with 25mL of ethyl acetate, collect the aqueous phase extract, concentrate and dry, and obtain 2.07g of dried sample, the yield 20.7%;

[0055] (3) Take 1 g of the above-mentioned dried sample, dissolve it in 10 mL of distilled water, put it on a reversed-phase resin SciBioChem MCI-GEL chromatography column, the filler height is 20 cm, and the column diameter is 3.2 cm, and it is eluted with methanol-water gradient, and the concentration is 0 wt%. , 10wt%, 20wt%, 30wt%, 40wt%, 50wt% methanol, the elution flow rat...

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Abstract

The invention discloses a method for extracting chlorogenic acid and neochlorogenic acid from bunge pricklyash leaves. The method is characterized by comprising the following steps of: crushing dried bunge pricklyash leaves till the average particle size is 400-600 micrometers; adding to methanol with the concentration of 50wt%-80wt% according to the material-to-liquid ratio of 1g:(8-30)mL, oscillating at room temperature for 24-36 hours, separating supernatant, concentrating, and drying to obtain a methanol extract; dispersing the methanol extract into distilled water at the material-to-ratio of 1g:(10-30)mL, adding ethyl acetate according to the volume ratio of 1:2, carrying out oscillating extraction for 2-3 times, collecting a water-phase extractive, concentrating and drying, wherein the yield is 19.8%-25.8%; carrying out gradient elution on a reveres-phase resin SciBioChem MCI-GEL chromatographic column positioned on a dried sample by using methanol-water, wherein the filler height is 20cm, the column diameter is 3.2 cm, the concentrations of methanol-water are 0wt%, 10wt%, 20wt%, 30wt%, 40wt% and 50wt%, and the elution flow velocity is1-2mL/min; respectively collecting 10wt% methanol eluent and 20wt% methanol eluent, concentrating, drying, and then separating and purifying by using liquid chromatography to obtain the neochlorogenic acid and the chlorogenic acid, wherein the yield is 0.03%-0.05% and 0.03%-0.06% respectively.

Description

technical field [0001] The invention relates to a method for preparing chlorogenic acid and neochlorogenic acid from prickly ash leaves, and belongs to the technical field of Chinese herbal medicine preparation and chemical industry. Background technique [0002] Chlorogenic acid is a depsipolic acid composed of caffeic acid and quinic acid, also known as coffee tannic acid, which is a kind of plant produced by shikimic acid pathway during aerobic respiration. A phenylpropanoid compound. It widely exists in plants, and its content is higher in honeysuckle and Eucommia. Chlorogenic acid is an important biologically active substance with a wide range of pharmacological effects and biological activities. It is not only the main active ingredient of many medicinal materials and Chinese patent medicines for antibacterial detoxification, anti-inflammatory and choleretic, but also has anti-virus, white blood cell increase, anti-tumor, Effects of lowering blood pressure, lowering ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/732C07C67/48C07C67/56
CPCC07C67/48C07C67/56C07C2601/14C07C69/732
Inventor 高鸿颜欢钟凯黄毅娜周子画
Owner SICHUAN UNIV
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