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Method for purifying schaftoside

A technology of schaftoside and purification method, which is applied in the field of natural plant extraction, can solve the problems of long preparation period, cumbersome operation, and small preparation amount, and achieve the effects of small solvent consumption, good separation effect, and reduced loss

Inactive Publication Date: 2012-01-25
苏州宝泽堂医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] There are few studies on the extraction of schiaftosides in the prior art. The method used in the document "Study and Application of Active Components of Desmodium Glycyrrhiza and Rheum officinale" is 80% ethanol reflux extraction, the extract is concentrated and alcohol-free, then added with water to precipitate, and the supernatant is taken The liquid is extracted with petroleum ether, the aqueous phase is concentrated and subjected to silica gel column chromatography, and then separated by polyamide column chromatography and gel column chromatography, and finally the schaftoside product is obtained by preparing a high liquid phase. Although this method obtains a high-content product, But the operation is cumbersome, the preparation cycle is long and the preparation amount is small

Method used

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  • Method for purifying schaftoside

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Take 1kg of Herba Desmodium, crush it, add 8L of 5% sodium bicarbonate solution to heat and extract 5 times, each time for 3 hours, the extraction temperature is 60°C, collect the extract, add 1mol / L hydrochloric acid at room temperature to adjust to pH2, add An equal amount of water-saturated n-butanol was extracted twice, and the extract recovered n-butanol to obtain a dry product;

[0026] Measure chloroform-methanol-n-butanol-water according to the volume ratio (8:7:2:8), mix evenly, let stand and separate layers, take the upper layer as the stationary phase, and the lower layer as the mobile phase, and use the above dry matter with the following The phase is dissolved to make a sample solution. First pump the stationary phase to fill the chromatographic column. Turn on the main engine and set the rotation speed of the helical column coil to 950r / min to make the solenoid rotate clockwise. Pump the mobile phase, and when the mobile phase flows out from the port of th...

Embodiment 2

[0029] Take 5kg of Herba Desmodium, crush it, add 90L of 5% sodium bicarbonate solution to heat and extract twice, each time for 1h, the extraction temperature is 100°C, collect the extract, add 0.5mol / L hydrochloric acid at room temperature to adjust to pH5, Add an equal amount of water-saturated n-butanol to extract 3 times, and recover the n-butanol from the extract to obtain a dry product;

[0030] Measure chloroform-methanol-n-butanol-water according to the volume ratio (12:9:2:8), mix evenly, let stand and separate layers, take the upper layer as the stationary phase, and the lower layer as the mobile phase, and use the above dry matter with the lower The phase is dissolved to make a sample solution. First pump the stationary phase to fill the chromatographic column, turn on the main engine and set the rotation speed of the helical column coil to 750r / min, so that the solenoid rotates clockwise. min pumped the mobile phase, and when the mobile phase flowed out from the p...

Embodiment 3

[0033] Take 10kg of Herba Desmodium, crush it, add 100L of 5% sodium bicarbonate solution to heat and extract 3 times, each time for 2 hours, the extraction temperature is 80°C, collect the extract, add 0.8mol / L hydrochloric acid at room temperature to adjust to pH3, Add an equal amount of water-saturated n-butanol to extract 3 times, and recover the n-butanol from the extract to obtain a dry product;

[0034] Measure chloroform-methanol-n-butanol-water according to the volume ratio (11:10:2:8), mix evenly, let stand and separate layers, take the upper layer as the stationary phase, and the lower layer as the mobile phase, and use the above dry matter with the lower The phase is dissolved to make a sample solution. First pump the stationary phase to fill the chromatographic column. Turn on the main engine and set the rotation speed of the helical column coil to 900r / min to make the solenoid rotate clockwise. Pump in the mobile phase, and when the mobile phase flows out from th...

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Abstract

The invention provides a method for purifying schaftoside and in particular relates to a method for purifying schaftoside from snowbellleaf tickclover herb. The method comprises the following steps: grinding snowbellleaf tickclover herb, adding 5% of sodium bicarbonate solution for heating extraction, adding extract to be acidic, adding water saturated n-butanol for extraction, using extract to recover n-butanol to obtain dried matters and then separating the dried matters by high-speed counter-current chromatography to obtain high-content schaftoside. The method has the following advantages: the high-speed counter-current method is adopted to purify schaftoside; the process has strong specificity; and the product has high yield and purity.

Description

technical field [0001] The invention belongs to the field of natural plant extraction, and relates to a method for purifying schaftoside, in particular to a method for purifying schaftoside by high countercurrent chromatography. Background technique [0002] Desmodium broadleaf: leguminous plant Desmodium broadsighten Desmodium styracifolium (Osb.) The dry aboveground part of Merr., also known as money grass, Guangdong money grass, copper money grass, ground money, fake peanuts, horseshoe grass. It was first recorded in "Lingnan Herbal Medicine", and it is a variety recorded in the National Pharmacopoeia. "Chinese Pharmacopoeia 2010" adopts schiaftoside as the content index, and stipulates that the content of schiaftoside should not be less than 0.13% when calculated as a dry product. At present, there are few reference substances of schaftoside in the market, and the price is relatively high. [0003] The whole herb of Desmodium radix contains alkaloids, flavonoid glycosi...

Claims

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Application Information

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IPC IPC(8): C07D407/14
Inventor 李法庆刘东锋
Owner 苏州宝泽堂医药科技有限公司
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