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Method for preparing high-purity soybean saponin A and B

A soybean saponin, high-purity technology, used in steroids, organic chemistry, etc., can solve the problems of reduced distribution efficiency, easy adsorption of samples, large solvent consumption, etc., and achieves easy operation, good reproducibility, and separation efficiency. high effect

Active Publication Date: 2009-03-25
SHANGHAI TAUTO BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It avoids various problems caused by solid supports or carriers, such as samples are easily adsorbed, lost and denatured, so that when other liquid chromatography techniques are used for separation of preparative volumes, the distribution efficiency will be significantly reduced and the solvent consumption will be large

Method used

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  • Method for preparing high-purity soybean saponin A and B
  • Method for preparing high-purity soybean saponin A and B

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] The methyl acetate-n-propanol-ethanol-water system was selected to separate and purify soybean saponins on a semi-preparative countercurrent chromatograph. First divide the above solvent components into a separatory funnel according to the volume ratio of 4:0.8:2:6, shake and let stand to separate layers. After equilibrating for 30 minutes, the upper and lower phases were separated. A semi-preparative countercurrent chromatograph is used, equipped with a polytetrafluoroethylene column, a 20ml injection valve, a column volume of 300ml, a TBP-50A pump, a TBD-23 detector and an N2000 chromatographic workstation. Weigh 100 mg of crude soybean saponin and dissolve it in 10 ml of the upper phase and 10 ml of the lower phase solution for use. Before sample injection, fill the entire column with stationary phase, adjust the speed of the main engine to 950rpm, and pump the mobile phase into the column at a flow rate of 3.0ml / min; The ultraviolet spectrum of the detector is use...

Embodiment 2

[0031] The ethyl acetate-n-butanol-ethanol-water system was selected to separate and purify soybean saponins on a semi-preparative countercurrent chromatograph. The suitable temperature for the experiment is 30°C. First, divide the above solvent components into a separatory funnel according to the volume ratio of 3:0.5:1:8, shake it and let it stand for stratification. After equilibrating for 30 minutes, the upper and lower phases were separated. A semi-preparative countercurrent chromatograph is used, equipped with a polytetrafluoroethylene column, a 20ml injection valve, a column volume of 300ml, a TBP-50A pump, a TBD-23 detector and an N2000 chromatographic workstation. Weigh 150mg crude soybean saponin and dissolve in 10ml upper phase and 10ml lower phase solution for use. Before sample injection, fill the entire column with stationary phase, adjust the speed of the main engine to 650rpm, and pump the mobile phase into the column at a flow rate of 3.0ml / min; The ultravio...

Embodiment 3

[0033]The butyl acetate-n-propanol-ethanol-water system was selected to separate and purify soybean saponins on a semi-preparative countercurrent chromatograph. The suitable temperature for the experiment is 22°C. First, divide the above solvent components into a separatory funnel according to the volume ratio of 4:1:1:6, shake and let stand to separate layers. After equilibrating for 30 minutes, the upper and lower phases were separated. A semi-preparative countercurrent chromatograph is used, equipped with a polytetrafluoroethylene column, a 20ml injection valve, a column volume of 300ml, a TBP-50A pump, a TBD-23 detector and an N2000 chromatographic workstation. Weigh 150mg crude soybean saponin and dissolve in 10ml upper phase and 10ml lower phase solution for use. Before sample injection, fill the entire column with stationary phase, adjust the speed of the main engine to 750rpm, and pump the mobile phase into the column at a flow rate of 4.0ml / min; The ultraviolet spec...

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Abstract

The invention relates to a method for preparing high-purity soybean saponin A and soybean saponin B by high-speed countercurrent chromatography, which comprises the following steps of: (1) selecting a solvent system which is provided with a fixed phase as an upper phase and a mobile phase as a lower phase and has four components with the volume ratio of 1-5 to 0.5-1 to 1-5 to 5-10; (2) using the fixed phase to fill a countercurrent chromatographic column, regulating the rotation speed of a host to be 600 rpm to 1000rpm and pumping the mobile phase into the column at the flow rate of 0.5 ml / min to 4ml / min; (3) after the whole system is in dynamic equilibrium, introducing samples through an introduction valve; and (4) receiving a target composition according to a UV atlas of a detector, compressing, freezing and crystallizing the fraction to obtain monomers of the soybean saponin A and the soybean saponin B. The soybean saponin A and the soybean saponin B prepared by the method can reach quite high purity and the preparation method has simple operation, high separation efficiency, great separation volume, high recovery rate and good repeatability.

Description

technical field [0001] The invention belongs to the field of preparation of soybean saponins, in particular to a method for preparing high-purity soybean saponins A and B by high-speed countercurrent chromatography. Background technique [0002] Soybeans are very rich in nutrients. In addition to being used to make edible oil and feed, they can also be made into soybean foods such as tofu, soymilk, and fermented foods, and are widely eaten. China, Japan, Korea and other East Asian countries have a long history of eating soybean food. In recent years, epidemiological studies have found that compared with Europeans and Americans, women in East Asian countries have milder menopausal symptoms, lower incidence of osteoporosis, breast cancer, prostate cancer and other cancers, and cardiovascular diseases such as myocardial infarction and arteriosclerosis. Rates and mortality are also lower. It is believed that this has a lot to do with the eating habits of the people in this are...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00
Inventor 邓秋云程杰王维娜苏玉萍
Owner SHANGHAI TAUTO BIOTECH CO LTD
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