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Method for purifying troxerutin from troxerutin industrial decoction dreg

A kind of dregs, industrial technology, applied in the field of purification and extraction of troxerutin, can solve the problems of increased production costs, non-compliance, and difficulty in recycling dregs, and achieve the effect of easy operation

Inactive Publication Date: 2016-06-15
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because rutin has many reaction sites, a series of by-products will grow after the reaction is completed. At the same time, a large amount of mucus and colloid will be produced during the recrystallization preparation process, so that a large amount of troxerutin remains in the crystallization mother solution In the process, industrial dregs will be formed, which will be treated as waste, which will greatly increase the production cost and bring about environmental pollution.
[0004] At present, there are about dozens of manufacturers of troxerutin raw materials in China. According to statistics, nearly 1,000 tons of dregs are produced every year. However, due to the inability to handle them, a large amount of dregs are discarded, causing environmental pollution and economic losses.
In addition, there are a large number of reaction by-products, mucus, and colloidal components in the dregs, which make it difficult to recycle the dregs. Currently, it is reported that two organic flocculants are used to treat the crystallization mother liquor, and then the macroporous resin is used for adsorption and elution. Patent report to achieve purification (Chinese patent: a purification process for troxerutin crystallization mother liquor, application number: 201210590546.8)
However, the patent operation steps are cumbersome, and the purified troxerutin content is only 61.8%, which does not meet the 80% troxerutin oral standard stipulated in the 2015 edition of "Chinese Pharmacopoeia".

Method used

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  • Method for purifying troxerutin from troxerutin industrial decoction dreg
  • Method for purifying troxerutin from troxerutin industrial decoction dreg
  • Method for purifying troxerutin from troxerutin industrial decoction dreg

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Take 1g of troxerutin industrial dregs in a 25mL beaker, add 10ml of distilled water to dissolve, let stand for 12h and then filter, discard the filter residue, and keep the filtrate for later use. Take 50g of hydroxypropyl dextran gel LH-20, soak it in 500ml of distilled water overnight, remove the floating matter, pour it into a glass column (diameter-to-length ratio is 1:20, column volume 50mL), wait for the soaking liquid to flow to the liquid surface, add troxerutin dregs filtrate, wait for the filtrate to flow to the liquid surface, then wash the stigma with 1ml of distilled water, add 500ml of distilled water to elute after the stigma is cleaned, start to collect after elution of 100ml, collect 50ml; After being concentrated and dried under pressure, the troxerutin was detected by HPLC up to 85%, and the recovery rate was 88%, which met the oral liquid specification.

Embodiment 2

[0023] Take 1g of troxerutin industrial dregs in a 25mL beaker, add 10ml of distilled water to dissolve, let stand for 12h and then filter, discard the filter residue, and keep the filtrate for later use. Take 50g of hydroxypropyl dextran gel LH-20, soak it overnight with 500ml of methanol-water (30% methanol, volume ratio) solution, remove the floating matter, and pour it into a glass column (the ratio of diameter to length is 1:20, Column volume 50mL), when the soaking liquid flows to the liquid surface, add troxerutin dregs filtrate, wait for the filtrate to flow to the liquid surface, then wash the column head with 1ml distilled water, add 500ml methanol-water (30% methanol ) solution elution, start to collect after elution 100ml, collect 50ml; After 50ml collection liquid is concentrated and dried under reduced pressure, detect through HPLC, troxerutin content is 82.5%, and recovery rate is 80%, meets oral liquid specification.

Embodiment 3

[0025] Take 1g of troxerutin industrial dregs in a 25mL beaker, add 10ml of distilled water to dissolve, let stand for 12h and then filter, discard the filter residue, and keep the filtrate for later use. Take 50g of hydroxypropyl dextran gel LH-20, soak it overnight with 500ml of methanol-water (60% methanol, volume ratio) solution, remove the floating matter, and pour it into a glass column (diameter-to-length ratio of 1:20, Column volume 50mL), when the soaking liquid flows to the liquid surface, add troxerutin dregs filtrate, wait for the filtrate to flow to the liquid surface, then wash the column head with 1ml distilled water, add 500ml methanol-water (60% methanol ) solution elution, start to collect after elution 100ml, collect 50ml; After 50ml collection liquid is concentrated and dried under reduced pressure, detect by HPLC, troxerutin content is 81%, and recovery rate is 82%, meets oral liquid specification.

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Abstract

The invention provides a method for purifying troxerutin from troxerutin industrial decoction dreg. The method comprises the steps that a separated material is pretreated and loaded into a chromatographic column; the troxerutin industrial decoction dreg is dissolved with water, stands and is filtered; filter liquor is sampled, adsorbed and eluted, eluant is concentrated and dried to obtain troxerutin, the content is 80% (HPLC detection), the recovery rate is 80%, and an obtained product meets the oral liquid standard of Chinese pharmacopoeia in 2015 version. Waste resources of synthetic drugs are effectively utilized, regeneration value of troxerutin is improved, and the method is fast, simple and suitable for industrialized production, and has an application prospect in the aspect of recycling troxerutin waste liquor.

Description

technical field [0001] The invention relates to raw materials, in particular to a method for purifying and extracting troxerutin from troxerutin industrial dregs. Background technique [0002] Troxerutine Chinese aliases: hydroxyethyl rutin, toxerutin, trihydroxyethyl rutin, Weinaolutong, vitamin P4, English name: Troxerutine. This product is soluble in water, soluble in methanol and ethanol, insoluble in chloroform. Molecular formula: C 33 h 42 o 19 , molecular weight 742.68. This product can inhibit the aggregation of red blood cells and platelets, prevent thrombus formation, and at the same time increase the oxygen content in the blood, improve microcirculation, and promote the formation of new blood vessels to enhance collateral circulation. It is suitable for hemiplegia and aphasia caused by cerebral thrombosis and cerebral embolism, as well as pre-myocardial infarction syndrome, arteriosclerosis, central retinitis, thrombophlebitis, varicose veins, and edema cause...

Claims

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Application Information

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IPC IPC(8): C07H17/07C07H1/06
CPCC07H1/06C07H17/07
Inventor 李石飞张立伟赖恩义
Owner SHANXI UNIV
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