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Method for preparing and partially-synthesizing chlorogenic acid from processing residual liquid of aqua lonicerae foliae

A technology for honeysuckle dew and chlorogenic acid, which is applied in the field of chemical substances or pharmaceutical manufacturing, can solve the problems of difficult to scale up production of separation technology, low yield of chlorogenic acid, low utilization rate of raw materials, etc., and achieves simple process and improved utilization of raw materials. rate, the effect of solving the low yield

Inactive Publication Date: 2011-01-12
WUHAN JUHUI GREEN IND DEV
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0014] The present invention provides a method for preparing and semi-synthesizing chlorogenic acid from honeysuckle dew processing raffinate, the purpose of which is to solve the existing extraction and preparation of chlorogenic acid technology, which consumes a large amount of organic solvents and causes environmental pollution; or uses more complicated methods Separation technology is difficult to scale up production; or the extraction efficiency is not high, and the utilization rate of raw materials is low, etc.
The invention uses honeysuckle dew processing residual liquid as raw material to realize the comprehensive utilization of resources, and can make full use of the caffeoylquinic acid substances in the extraction process, and after the compounds are hydrolyzed into caffeic acid and quinic acid, they are synthesized Chlorogenic acid, solving the problem of low yield of chlorogenic acid in the existing preparation

Method used

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  • Method for preparing and partially-synthesizing chlorogenic acid from processing residual liquid of aqua lonicerae foliae

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) Precipitation step

[0033] Get 100ml honeysuckle dew processing residual liquid, add 2% trichloroacetic acid aqueous solution (V / V) 10ml, add volume and honeysuckle dew processing residual liquid volume ratio is 1: 10 (V / V), add hexadecyl trimethyl Ammonium bromide (CTAB) 2.0g, the ratio of its added quality to the volume of honeysuckle dew processing raffinate is 0.02g / ml (mass to volume ratio), after stirring and reacting at 60°C for 60min, leave it standing at 4°C for 24 hours, filter the The obtained filtrate was concentrated to 10ml, and its volume was 1 / 10 of the volume of the honeysuckle dew processing residual liquid to obtain 10ml of precipitated liquid.

[0034] (2) Macroporous adsorption resin separation step

[0035] After the precipitated solution obtained is loaded onto the AB-8 macroporous adsorption resin, it is eluted with 5% ethanol aqueous solution (V / V), and the flow rate is 3 column volumes per hour, discarding the eluent, and then using 60% ...

Embodiment 2

[0045] (1) Precipitation step

[0046] Get 200ml honeysuckle dew processing residual liquid, add 5% trichloroacetic acid aqueous solution (V / V) 10ml, add volume and honeysuckle dew processing residual liquid volume ratio is 1: 20 (V / V), add hexadecane hydroxide simultaneously Trimethylamine bromide (CTA-OH) 16.0g, the ratio of its added mass to the volume of honeysuckle dew processing residual liquid is 0.08g / ml (mass volume ratio), stirred and reacted at 20°C for 40min, then stood at 25°C for 8 hours , the filtrate obtained after filtering is concentrated to 10ml, its volume is 1 / 20 of the volume of the honeysuckle dew processing residual liquid, and 10ml of precipitation solution is obtained.

[0047] (2) Macroporous adsorption resin separation step

[0048] After loading the obtained precipitate solution onto the XDA-1 macroporous adsorption resin, elute it with 20% ethanol aqueous solution (V / V), the flow rate is 1 column volume per hour, discard the eluate, and then use ...

Embodiment 3

[0058] (1) Precipitation step

[0059] Get 300ml honeysuckle dew processing raffinate, add 3% trichloroacetic acid aqueous solution (V / V) 20ml, add volume and honeysuckle dew processing raffinate volume ratio is 1: 15 (V / V), add hexadecylpyridinium simultaneously (CP-OH) 18.0g, the ratio of its added mass to the volume of honeysuckle dew processing residual liquid is 0.06g / ml (mass volume ratio), stirred and reacted at 40°C for 20min, left standing at 10°C for 18 hours, filtered to obtain The filtrate is concentrated to 10ml, and its volume is 1 / 30 of the volume of the honeysuckle dew processing residual liquid to obtain 10ml of precipitated liquid.

[0060] (2) Macroporous adsorption resin separation step

[0061] After loading the obtained precipitate solution onto D101 macroporous adsorption resin, elute with 10% ethanol aqueous solution (V / V), the flow rate is 2 column volumes per hour, discard the eluate, and then use 30% ethanol The aqueous solution (V / V) was eluted at...

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Abstract

The invention discloses a method for preparing and partially-synthesizing chlorogenic acid from the processing residual liquid of aqua lonicerae foliae, which belongs to a method for manufacturing chemical substances or medicines and solves the problem of the existing chlorogenic acid extraction and preparation technology that a large amount of organic solvent is used and causes environmental pollution, or the production is difficult to expand as a relatively complex separation technology is used, or the extraction efficiency is low, the utilization rate of raw materials is relatively low and so on. The method comprises a deposition step, a separation step by using macroporous absorption resin, an acid hydrolysis step, a separation step by using ion exchange column, a semi-synthesis step and a crystallization step. The invention realizes comprehensive utilization of resources by adopting the processing residual liquid of aqua lonicerae foliae as a raw material, and can make full use of the caffeoylquinic acid substances during the extraction, hydrate the compounds into caffeic acid and quinic acid, then synthesize the chlorogenic acid and finally obtain chlorogenic acid with the purity over 99% through the crystallization step. The process of the invention is simple and can be easily expanded to industrial production while greatly improving the utilization rate of the raw material.

Description

technical field [0001] The invention belongs to the production method of chemical substances or medicines, and in particular relates to a method for preparing and semi-synthesizing chlorogenic acid by using honeysuckle dew processing residual liquid as a raw material. Background technique [0002] Chlorogenic acid (Chlorogenic acid), chemical name: 3-caffeoylquinic acid, is a depsipolic acid generated from caffeic acid (Caffeic acid) and quinic acid (Quinic acid, 1-hydroxyhexahydrogallic acid). A phenylpropanoid compound produced by plants through the shikimate pathway during aerobic respiration. [0003] Chlorogenic acid has pharmacological effects such as antibacterial, anti-inflammatory, detoxification, choleretic, blood pressure lowering, increasing white blood cells, significantly increasing gastrointestinal motility and promoting gastric juice secretion, and has strong inhibition on Escherichia coli, Staphylococcus aureus, pneumococcus and viruses Function: It has obv...

Claims

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Application Information

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IPC IPC(8): C07C69/732C07C67/08
Inventor 杨俊林秀忠林承成
Owner WUHAN JUHUI GREEN IND DEV
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