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Method for efficiently separating and purifying puerarin

A high-efficiency technology for puerarin, applied in the field of efficient separation and purification of puerarin, can solve the problems of increasing operation difficulty and economic cost, increasing the distribution coefficient and yield of target products, and accelerating system fractionation, etc., and achieves simple operation, conventional equipment, high-efficiency The effect of purity

Active Publication Date: 2016-11-16
陕西乾翔健康科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the existing two-phase extraction technology needs to be supplemented by centrifugation and other operations after the phase separation of the system, thereby accelerating the phase separation of the system, and adding neutral salt KCl to the system to increase the distribution coefficient and yield of the target product increases the operational difficulty and economic cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Preparation of modified dextran

[0025] 10g hexanoic acid, 100g dextran and 0.05g SO 4 2- / ZrO 2 Place the solid superacid catalyst in a rotary evaporator, mix it evenly, react at 150°C, and divide the water under reduced pressure. After the pH test paper detects that the reaction liquid is neutral, stop the reaction, cool to room temperature, filter, and remove the filtrate by distillation. After removing the moisture, 107.2 g of modified dextran was obtained.

[0026] (2) Preparation of puerarin crude extract

[0027] Add 10g of kudzu root powder into 300g of 70% ethanol-water solution, reflux extraction and soaking in a Soxhlet extractor for 12 hours, cool to room temperature, filter, and concentrate under reduced pressure to obtain 32g of puerarin crude extract, the puerarin purity is 28.5 %, the yield is 91.2%. The purity of puerarin was measured by high performance liquid chromatography, the fluidity was 50% methanol-water solution, the flow rate was 1 m...

Embodiment 2

[0031] (1) Preparation of modified dextran

[0032] 10g hexanoic acid, 120g dextran and 0.1g SO 4 2- / ZrO 2 Put the solid superacid catalyst in a rotary evaporator, mix it evenly, react at 160°C, and divide the water under reduced pressure. After the pH test paper detects that the reaction solution is neutral, stop the reaction, cool to room temperature, filter, and remove the filtrate by distillation. After removing the moisture, 107.2 g of modified dextran was obtained.

[0033] (2) Preparation of puerarin crude extract

[0034] Add 10g of kudzu powder to 500g of 60% ethanol-water solution, reflux extraction and soaking in a Soxhlet extractor for 20 hours, cool to room temperature, filter, and concentrate under reduced pressure to obtain 30g of puerarin crude extract, the purity of puerarin is 30.2 %, the yield is 90.8%.

[0035] (3) Aqueous two-phase extraction

[0036] Take 12.8g of puerarin-containing crude extract, 5g of modified dextran and 2.4g of sodium sulfate ...

Embodiment 3

[0038] (1) Preparation of modified dextran

[0039]10g hexanoic acid, 150g dextran and 0.12g SO 4 2- / ZrO 2 Place the solid superacid catalyst in a rotary evaporator, mix it evenly, react at 170°C, and divide the water under reduced pressure. After the pH test paper detects that the reaction solution is neutral, stop the reaction, cool to room temperature, filter, and remove the filtrate by distillation. After removing the moisture, 107.2 g of modified dextran was obtained.

[0040] (2) Preparation of puerarin crude extract

[0041] Add 10g of kudzu root powder into 600g of 50% ethanol-water solution, reflux extraction and soaking in a Soxhlet extractor for 24 hours, cool to room temperature, filter, and concentrate under reduced pressure to obtain 29.5g of puerarin crude extract, the puerarin purity is 31.5%, the yield is 92.9%.

[0042] (3) Aqueous two-phase extraction

[0043] Take 13.6g of puerarin-containing crude extract, 4.4g of modified dextran and 2g of ammonium...

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Abstract

The invention provides a method for efficiently separating and purifying puerarin. The method comprises the steps that puerarin powder is subjected to reflux extraction in a 50-70% alcohol-water solution for 12-24 h to obtain crude extract, modified glucan-inorganic salt two aqueous phase extraction layering is carried out, the upper phase is dialyzed in a dialysis membrane with the molecular mass cut-off of 10000 for 15-20 h to obtain a puerarin water solution, the puerarin water solution is frozen and dried at the temperature of -15--10 DEG C for 8-15 h to obtain puerarin powder, and the modified glucan is caproic acid partially-esterified glucan. The 50-70% alcohol-water solution is adopted as the extraction solution, so that high yield and high purity are obtained, and meanwhile solid and liquid phases can be rapidly separated; the modified glucan / inorganic salt two aqueous phase system is high in selectivity for puerarin, the system phase separation speed is high, and rapid phase separation can be achieved without equipment such as a centrifugal machine; according to the puerarin powder prepared through the method, the puerarin purity reaches up to 97.5%, and the total recovery reaches up to 87.5%.

Description

technical field [0001] The invention belongs to the technical field of biochemical separation, and relates to a method for separating and purifying puerarin, in particular to a method for efficiently separating and purifying puerarin. Background technique [0002] Puerarin, also known as pueraria flavonoids, is a yellow crystal, soluble in water, methanol, ethanol, pyridine, easily soluble in hot water, insoluble in benzene, chloroform, ether, etc. Puerarin is the main active ingredient of kudzu root. It can reduce myocardial oxygen consumption, increase coronary and cerebrovascular blood flow, expand coronary and cerebrovascular blood vessels, and promote blood circulation. It is clinically used to treat hypertension and angina pectoris. , Cerebral insufficiency, cerebral infarction and sudden deafness. Our country is very rich in kudzu root resources. Therefore, the research and development of an optimized process route to obtain high-purity puerarin from puerariae is not...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D407/04
CPCC07D407/04
Inventor 任新年
Owner 陕西乾翔健康科技有限公司
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