Method for preparing high-purity puerarin and daidzein at the same time

A technology of daidzein and puerarin, applied in the direction of organic chemistry, can solve the problems of cumbersome operation and low yield, and achieve the effects of high yield, low production cost and improved utilization value

Inactive Publication Date: 2013-04-24
NANJING UNIV OF TECH +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process is cumbersome to operate,

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Use 500g (absolutely dry) pulverized kudzu root with 5000ml of 85% ethanol solution (the ratio of pueraria to ethanol solution is 1:10), reflux extraction at 90°C for 4 hours, repeat the extraction for 3 times, filter, and depressurize the filtrate Concentrate to dryness to obtain 78g of kudzu root extract extract, add 1560ml of 75% ethanol solution to make it redissolve in the kudzu root extract extract extract, add 780ml of 8% hydrochloric acid aqueous solution, add chloroform 1950ml again, reflux hydrolysis extraction for 8 hours, The temperature is 90°C. Stand to cool and separate the chloroform phase, concentrate under reduced pressure, recrystallize the concentrate 3 times with 50% ethanol to obtain daidzein crystals; Methanol (1:1) recrystallized 3 times to obtain puerarin product. The yield of puerarin was 1.12%, and the purity was 98.6%; the yield of daidzein was 0.49%, and the purity was 95.8%.

Embodiment 2

[0035]Use 3000ml of 55% ethanol solution (the solid-liquid ratio of Pueraria root and ethanol solution is 1:6) to 500g (dry) pulverized kudzu root, reflux extraction at 70°C for 2 hours, repeat the extraction once, filter, and depressurize the filtrate Concentrate to dryness to obtain 37.8g of kudzu root extract extract, add 1520ml of 35% ethanol solution to the kudzu root extract extract to make it redissolve, add 114ml of 3% hydrochloric acid aqueous solution, add 171ml of chloroform again, reflux hydrolysis extraction for 1 hour , the temperature is 60°C. Stand and cool to separate the chloroform phase, concentrate under reduced pressure, and recrystallize the concentrate once with 60% ethanol to obtain daidzein crystals; add water to dilute the acid hydrolyzate by 0.5 times, leave it for 48 hours to precipitate puerarin coarse crystals, and dilute it with acetic acid- Methanol (3:7) recrystallized once to obtain puerarin product. The yield of puerarin was 1.00%, and the p...

Embodiment 3

[0037] Use 4000ml of 75% ethanol solution (the solid-liquid ratio of Pueraria root and ethanol solution is 1:8) to 500g (dry) pulverized kudzu root, reflux extraction at 80°C for 3 hours, repeat the extraction twice, filter, and depressurize the filtrate Concentrate to dryness to obtain 58.6g of kudzu root extract extract, add 1180ml of 60% ethanol solution to the kudzu root extract extract to make it redissolve, add 6% hydrochloric acid aqueous solution 295ml, add chloroform 590ml again, reflux hydrolysis extraction for 4 hours , the temperature is 80°C. Stand to cool and separate the chloroform phase, concentrate under reduced pressure, recrystallize the concentrate 3 times with 40% ethanol to obtain daidzein crystals; Methanol (7:3) recrystallized twice to obtain puerarin product. The yield of puerarin was 1.07%, and the purity was 98.1%; the yield of daidzein was 0.46%, and the purity was 95.2%.

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PUM

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Abstract

The invention relates to a method for preparing high-purity puerarin and daidzein at the same time. The method comprises the following steps of: mixing and extracting crushed kudzu root and ethanol in a feed liquid ratio of 1:6 to 1:10; filtering the obtained mixture, and performing vacuum concentration on the filtrate until the filtrate is dried to obtain a kudzu root extract; re-dissolving the kudzu root extract by using an ethanol solution with appropriate concentration, and then refluxing, hydrolyzing and extracting the mixture for a certain period of time by adding a hydrochloric acid solution and chloroform; standing and cooling; separating the chloroform; performing vacuum concentration; performing recrystallization on the concentrate by adopting the ethanol solution to obtain daidzein crystals; adding water to dilute acid hydrolysate; placing the mixture for 48 to 72 hours to separate out puerarin coarse crystals; and performing recrystallization on the puerarin coarse crystals by using acetic acid-methanol to obtain a puerarin product. By adopting the method, the puerarin and the daidzein in the kudzu root are extracted and separated at the same time, so that the utilization value of the kudzu root is improved, and a traditional Chinese medicinal material resource is fully used. According to the method, hydrolysis and extraction are finished at the same time, so that operation process steps are reduced, the usage amount of the solvents is reduced, the production cost is low, and the yield is high.

Description

technical field [0001] The invention belongs to the field of natural product chemistry, in particular to a method for simultaneously preparing high-purity puerarin and daidzein. Background technique [0002] Pueraria lobata (willd.) Ohwi is a perennial deciduous vine of the leguminous family. It is naturally distributed in temperate and subtropical regions. There are more than 20 species of Pueraria in the world, and 11 species of Pueraria in my country. [0003] The vines, leaves, flowers, seeds and tubers of Pueraria lobata can be used as medicine. Among them, the roots and flowers have the highest utilization value. The tuberous root of Ge, namely " Ge Gen ". It contains a large amount of starch and biologically active ingredients-isoflavones; in addition, it is also rich in protein, essential minerals and trace elements such as calcium, iron, zinc, selenium, and potassium. [0004] Pueraria lobata is described in "Shen Nong's Materia Medica", "Compendium of Materia M...

Claims

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Application Information

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IPC IPC(8): C07D407/04C07D311/36C07D311/40
Inventor 郑涛王舒雅刘晓风孙永明茅建国陈怡露周俊雍晓雨高俊
Owner NANJING UNIV OF TECH
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