A method for separating and purifying artichoke acid and chlorogenic acid in artichoke by simulated moving bed chromatography

A technology of simulating moving bed, separation and purification, which is applied in the field of extraction and purification of effective components of natural plants, and achieves the effects of stable operation, large processing capacity and easy automatic control.

Active Publication Date: 2021-04-30
华大国询(厦门)生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there is no report on the method of using simulated moving bed chromatography to separate different active components in artichoke.

Method used

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  • A method for separating and purifying artichoke acid and chlorogenic acid in artichoke by simulated moving bed chromatography

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] 1) Artichoke leaves were dried at 60°C for 12 hours, crushed, passed through a 10-20 mesh sieve, and then refluxed with 5 times the amount (mass volume ratio) of 70% ethanol for 3 times, each time for 3 hours, combined extracts, and reduced pressure After concentrating to a relative density of 1.10, add water for water precipitation, filter to remove insoluble matter, and obtain artichoke leaf extract;

[0040] 2) The artichoke leaf extract obtained in step 1) is processed by macroporous resin column chromatography: select D-101 macroporous adsorption resin, load the sample with a volume flow rate of 2BV / h, use 2BV of 1.0wt%NaOH Aqueous solution to elute impurities, wash with 3.5BV of water to neutrality, elute cynaric acid and chlorogenic acid with 5BV of 75% ethanol, the flow rate of mobile phase is 1BV / h; obtain the crude extract, the volume of ethanol in the crude extract Content > 85%;

[0041] 3) The crude extract is distilled under reduced pressure at 50°C, conc...

Embodiment 2

[0054] 1) Artichoke leaves were dried at 60°C for 12 hours, crushed, passed through a 10-20 mesh sieve, and then refluxed with 10 times the amount of 70% ethanol to extract 3 times, each time for 3 hours, combined extracts, concentrated under reduced pressure to a relative density of After 1.10, add water for water precipitation, filter to remove insoluble matter, and obtain artichoke leaf extract;

[0055] 2) The artichoke leaf extract obtained in step 1) is processed by macroporous resin column chromatography: select D-101 macroporous adsorption resin, load the sample with a volume flow rate of 2BV / h, use 1BV of 1.5wt%NaOH Aqueous solution to elute impurities, wash with 3.5BV of water to neutrality, elute cynaric acid and chlorogenic acid with 5BV of 75% ethanol, the flow rate of mobile phase is 1BV / h; obtain the crude extract, the volume of ethanol in the crude extract Content > 85%;

[0056] 3) The crude extract is distilled under reduced pressure at 50°C, concentrated by...

Embodiment 3

[0069] 1) Artichoke leaves are dried at 60°C for 12 hours, crushed, passed through a 10-20 mesh sieve, and then refluxed with 8 times the amount of 80% ethanol for 2 times, each time for 3 hours. The extracts are combined and concentrated under reduced pressure until the relative density is After 1.10, add water for water precipitation, filter to remove insoluble matter, and obtain artichoke leaf extract;

[0070] 2) The artichoke leaf extract obtained in step 1) is processed by macroporous resin column chromatography: select AB-8 macroporous adsorption resin, load the sample with a volume flow rate of 2BV / h, use 1BV of 1.5wt%NaOH Aqueous solution to elute impurities, wash with 3.5BV of water to neutrality, elute cynaric acid and chlorogenic acid with 5BV of 75% ethanol, the flow rate of mobile phase is 1BV / h; obtain the crude extract, the volume of ethanol in the crude extract Content > 85%;

[0071] 3) The crude extract is distilled under reduced pressure at 50°C, concentra...

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Abstract

The invention discloses a method for separating and purifying artichoke acid and chlorogenic acid in artichoke by simulated moving bed chromatography. The SMBC separation technology can continuously feed materials, has high separation degree and large processing capacity, and can improve the utilization of fillers and mobile phases Efficiency, reduce purification cost, belongs to the separation and purification process of green environmental protection. The present invention uses octadecylsilane bonded silica gel as the stationary phase to realize the high-precision separation of artichoke acid and chlorogenic acid in artichokes, and the mass fractions of the separated products all reach more than 75% according to the standard curve calculation. The efficiency is more than 60%; SMBC separation of artichokeic acid and chlorogenic acid not only saves a lot of solvents, but also improves production efficiency, and realizes low-carbon and environmentally friendly production; the present invention combines ethanol reflux extraction method and macroporous resin at the same time Column chromatography impurity removal method reduces water consumption and energy consumption, does not require flocculation to remove impurities, does not require special regeneration of the stationary phase, reduces waste water discharge, and has a simple process.

Description

technical field [0001] The invention belongs to the technical field of extraction and purification of effective components of natural plants, and in particular relates to a method for separating and purifying artichoke acid and chlorogenic acid in artichokes by simulated moving bed chromatography. Background technique [0002] Artichoke Cynara scolymus L., also known as chrysanthemum thistle, artichoke, artichoke, French lily, lotus lily, is a perennial herb of the family Asteraceae. The artichoke is native to the Mediterranean coast and evolved from the artichoke C.cardunculus L. Artichoke is the most cultivated in Italy, and Italy's output accounts for 50% of the world's total, followed by Spain and Argentina. Artichoke has high nutritional value and is a high-grade health-care vegetable. Its leaves contain cynarin (1,5-dicaffeoylquinic acid) and chlorogenic acid, which can protect the liver, protect the liver, and lower cholesterol. active natural ingredients. The rese...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/56C07C67/48C07C69/732
CPCC07C67/48C07C67/56C07C2601/14C07C69/732
Inventor 汤须崇胡婷婷洪俊明杨琼邓爱华黄志宏
Owner 华大国询(厦门)生物科技有限公司
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