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Method for separating and purifying puerarin monomers

A technology for separation and purification of puerarin, applied in the direction of organic chemistry, can solve the problems of low sample purity, cumbersome operation steps, and low sample recovery rate, and achieve the effect of high product purity, advanced technology and high separation efficiency

Inactive Publication Date: 2012-08-01
BEIJING CENT FOR PHYSICAL & CHEM ANALYSIS
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Most of the existing separation and purification methods of puerarin monomer components adopt the separation and purification method of column chromatography, which is widely used and has the advantages of large sample processing capacity, but the disadvantage of the above method is that the operation steps are cumbersome and the sample recovery rate is low. , the purity of the obtained sample is not high
In addition, there is a method of membrane filtration combined with recrystallization for separation and purification. This method can obtain puerarin monomer with high purity, but it has disadvantages such as high cost and easy secondary pollution, which restricts the development of this technology.

Method used

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  • Method for separating and purifying puerarin monomers
  • Method for separating and purifying puerarin monomers
  • Method for separating and purifying puerarin monomers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Mix ethyl acetate, n-butanol and water in a volume ratio of 12:3:15, place in a separatory funnel, shake fully and let stand to separate layers, take the upper layer solution as the stationary phase and the lower layer solution as the mobile phase , for subsequent use; the puerarin crude product of 150mg (puerarin purity is 50%) is dissolved in 10mL lower floor solution, for subsequent use;

[0027] (2) Use semi-preparative high-speed countercurrent chromatograph, the ternary solvent system that above-mentioned ethyl acetate, n-butanol and water are formed is as separation solvent system; In the chromatographic column of high-speed countercurrent chromatograph, be full of stationary phase, then adjust rotating speed 850r / min to make the host rotate, set the temperature of the constant temperature water bath to 30°C, set the detection wavelength of the ultraviolet detector to 254nm, and then pump the mobile phase into the chromatographic column at 1.5mL / min; Enter p...

Embodiment 2

[0033] (1) Mix ethyl acetate, n-butanol and water in a volume ratio of 5:3:8, place in a separatory funnel, shake fully and let stand to separate layers, take the upper layer solution as the stationary phase and the lower layer solution as the mobile phase , for subsequent use; 200mg puerarin crude product (the purity of puerarin is 65%) was dissolved in 15mL lower layer solution, for subsequent use;

[0034] (2) Use semi-preparative high-speed countercurrent chromatograph, with the ternary solvent system that above-mentioned ethyl acetate, n-butanol and water form as separation solvent system; In the chromatographic column of high-speed countercurrent chromatograph, be full of stationary phase, then adjust rotating speed 950r / min to make the host rotate, set the temperature of the constant temperature water bath to 25°C, set the detection wavelength of the ultraviolet detector to 254nm, and then pump the mobile phase into the chromatographic column at 2mL / min; Crude product ...

Embodiment 3

[0036] (1) Mix ethyl acetate, n-butanol and water in a volume ratio of 7:3:10, place in a separatory funnel, shake fully and let stand to separate layers, take the upper layer solution as the stationary phase and the lower layer solution as the mobile phase , for subsequent use; 250mg puerarin crude product (the purity of puerarin is 80%) is dissolved in 20mL lower layer solution, for subsequent use;

[0037] (2) Use semi-preparative high-speed countercurrent chromatograph, with the ternary solvent system that above-mentioned ethyl acetate, n-butanol and water are formed as separation solvent system; In the chromatographic column of high-speed countercurrent chromatograph, be full of stationary phase, then adjust rotating speed 800r / min to make the host rotate, set the temperature of the constant temperature water bath to 20°C, set the detection wavelength of the ultraviolet detector to 254nm, and then pump the mobile phase into the chromatographic column at 1.5mL / min; Enter pu...

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Abstract

The invention provides a method for separating and purifying puerarin monomers, which adopts high-speed counter-current chromatography and uses a ternary solvent system composed of ethyl acetate, n-butanol and water as a separation solvent system to separate and extract the puerarin monomers from a crude puerarin product. The separating and purifying method of the invention adopts a semi-preparative high-speed counter-current chromatograph to separate and purify the crude puerarin product, allows the crude puerarin product to go through the ternary solvent system, and utilizes the characteristics of high recovery rate and no irreversible adsorption of the high-speed counter-current chromatography to massively prepare the puerarin monomers, and the preparation amount can reach a gram magnitude; and the purity of the prepared puerarin monomers, which is high, reaches above 99%, and a standard sample of the puerarin monomers can be prepared with the high purity puerarin monomers as a raw material. The method of the invention is suitable for different crude puerarin products, and has the advantages of advanced technology, high separation efficiency, good recovery rate, high product purity, large preparation amount and the like.

Description

technical field [0001] The invention relates to a method for separating and purifying puerarin monomer, in particular to a method for separating and purifying puerarin monomer by high-speed countercurrent chromatography. Background technique [0002] Pueraria is a perennial leguminous twining vine, with many side vines and fibrous roots, but the roots are deep, spindle-shaped or long rod-shaped, and the skin is light yellow and wrinkled. It is the main edible and medicinal part. Pueraria lobata is the dried root of Pueraria Lobata (Willd.) Ohwi or P. thomsomi Benth. As a commonly used traditional Chinese medicine, kudzu root was first recorded in "Shen Nong's Materia Medica", and it was listed as a middle-grade product. It has been recorded in herbal medicines since the past dynasties. It is sweet, pungent, and flat in nature. Improve the body's immunity and other functions. At present, kudzu root is widely used in traditional Chinese medicine compound preparations such as...

Claims

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Application Information

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IPC IPC(8): C07D407/04
Inventor 王尉周晓晶张经华王覃杜宁刘清珺武会娟李津廷
Owner BEIJING CENT FOR PHYSICAL & CHEM ANALYSIS
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