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Method for preparing picfeltarraenin IA from picria feltarrae lour leaves

A technology for scrophulariside and scrophulariside, which is applied in the field of preparing scrophulariside IA, can solve the problems of small preparation amount, long cycle, low yield and the like, and achieves the effects of fast method, fast separation speed and short cycle.

Inactive Publication Date: 2012-03-28
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As mentioned above, these traditional preparation methods have many defects such as large amount of solvent used, low yield, small amount of preparation, long cycle, etc.

Method used

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  • Method for preparing picfeltarraenin IA from picria feltarrae lour leaves

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Scrophulariaceae bitter leaves were crushed, 2 kg was added to 8 times 80% ethanol and microwave extracted twice, each time for 30 minutes, the combined extract was concentrated to no alcohol, added to D941 anion resin column, eluted with deionized water, combined the next column liquid and The washing liquid was concentrated and dried under reduced pressure to obtain 67 g of extract. The extract was pulverized and 200 ml of acetone solution was added for ultrasonication for 40 minutes, then suction filtered, the solid was dissolved in chloroform, filtered, and the reagent was recovered from the filtrate to obtain 9 g of crude extract.

[0019] Mix ethyl acetate, n-butanol, and water at a ratio of 3:1:5. After mixing and fully stratifying, take the upper phase and fill the high-speed countercurrent chromatography column. At the same time, turn on the main engine at 800rpm, pump into the lower phase, and wait for the system to balance , the flow rate is adjusted to 2ml / m...

Embodiment 2

[0021] Scrophulariaceae leaves were crushed, 2kg was added with 6 times 50% ethanol and microwave extracted 3 times, each time for 30 minutes, the combined extract was concentrated to no alcohol, added to a 330 anion resin column, eluted with deionized water, combined the next column liquid and The washing solution was concentrated and dried under reduced pressure to obtain 75 g of extract. The extract was pulverized and 300ml of acetone solution was added to sonicate for 60 minutes, filtered with suction, the solid was dissolved in chloroform, filtered, and the reagent was recovered from the filtrate to obtain 11g of crude extract.

[0022] Take ethyl acetate, butanol, methanol, and water according to the ratio of 5:3:1:7. After mixing and fully layering, take the upper phase and fill the high-speed countercurrent chromatography column. After equilibrium, the flow rate was adjusted to 3ml / min. At the same time, the mobile phase was used to dissolve the crude extract, and the ...

Embodiment 3

[0024] Scrophulariaceae leaves were crushed, 2 kg was added to 8 times 70% ethanol and microwave extracted twice, each time for 30 minutes, the combined extract was concentrated to no alcohol, added to the D310 anion resin column, eluted with deionized water, combined the next column liquid and The water washing liquid was concentrated and dried under reduced pressure to obtain 72 g of extract. The extract was pulverized and 200ml of acetone solution was added to sonicate for 30 minutes, filtered with suction, the solid was dissolved in chloroform, filtered, and the reagent was recovered from the filtrate to obtain 10g of crude extract.

[0025] Take ethyl acetate, butanol, methanol, and water according to the ratio of 6:3:2:10. After mixing and fully layering, take the upper phase and fill the high-speed countercurrent chromatography column. After equilibrium, the flow rate is adjusted to 1ml / min, and the crude extract is dissolved in the mobile phase at the same time, the sa...

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Abstract

The invention discloses a method for preparing picfeltarraenin IA from picria feltarrae lour leaves. The method comprises the following steps of: i, crushing the picria feltarrae lour leaves, performing microwave extraction for 2 to 3 times and 30 minutes each time by adding 4 to 10BV 50 to 80 percent ethanol, reclaiming the ethanol from the extract, adding anionic resin into the concentrate to remove impurities, performing elution by using deionized water, collecting a column leaking solution and a washing solution, and performing compression and drying to obtain dry extract; ii, performing ultrasonic washing on the dry extract for 30 to 60 minutes by using anhydrous acetone, dissolving the dry extract by using chloroform, filtering the insoluble substances, reclaiming the chloroform, and obtaining a crude extract; and iii, separating the crude extract by adopting high-speed countercurrent chromatography, performing on-line detection by using an ultraviolet detector, collecting the target component, performing reduced pressure drying, and thus obtaining the picfeltarraenin IA. The method has the advantages of high efficiency, short period, high preparation quantity and the like, and is easy and convenient to operate and suitable for industrialized production.

Description

technical field [0001] The invention belongs to the field of biotechnology, and in particular relates to a method for preparing crocus glucoside IA from crocodile scrophulariae leaves. Background technique [0002] Picfeltarraenin IA (Picfeltarraenin IA) is a triterpenoid saponin, which is 3-O-a-L-rhamnopyranosyl-(1,2)-β-D-xylopyranoside , molecular formula: C41H62O13, molecular weight: 762.9, its aglycon structural formula: [0003] [0004] Bitterscrophulariaceae is a dicotyledonous plant medicine Scrophulariaceae, also known as cod gall grass and tetracycline grass. Injuries, bruises, stomachaches, indigestion. Modern studies have found that bitter scrophulariae contains a large amount of triterpene saponins, among which bitter scrophulariae IA has anti-complement, anti-inflammatory and anti-tumor effects. [0005] According to the literature search, most of the methods for preparing matrine IA are solid chromatographic column separation. For example, in the docume...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J17/00
Inventor 刘东锋杨成东
Owner NANJING ZELANG MEDICAL TECH
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