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Method for preparing po huo glycoside I refined product

A technology of pure baojoside, which is applied in the field of preparing pure baojoside I, can solve the problems of large activity loss of baojoside I, severe hydrolysis environment, and low hydrolysis efficiency, and achieves rapid separation, simple operation process, The effect of increasing selectivity

Inactive Publication Date: 2013-06-19
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The acid-base hydrolysis method is simple, but due to the severe hydrolysis environment, the prepared baojoside I often loses a lot of activity
The enzymatic hydrolysis method mainly uses β-glucosidase, but its activity is low, the hydrolysis efficiency is low, and the waste of raw materials is serious

Method used

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  • Method for preparing po huo glycoside I refined product
  • Method for preparing po huo glycoside I refined product
  • Method for preparing po huo glycoside I refined product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Take icariin 1mg ( figure 1 ), dissolved with citric acid buffer solution of 10ml pH 5.4, added 100ul of 5ug / ul enzyme mother solution, and hydrolyzed for 4 hours at 40 degrees Celsius; centrifuged to precipitate Baojoside I. The enzymatic hydrolysis product baojoside I precipitate was washed with water and centrifuged at 2000r / min for 5 minutes, the supernatant was discarded, and the process of washing, centrifuging and discarding the supernatant was repeated three times. Collect the precipitate, dissolve it with 3ml of cold methanol (-4 degrees Celsius), dissolve it with ultrasound, centrifuge at 2000r / min for 5 minutes, collect the supernatant, dissolve the solid with cold methanol again, dissolve it with ultrasound, centrifuge, and collect the supernatant, repeat three times in total , combined three supernatants to concentrate the obtained baojoside I crude product ( figure 2 ), the conversion rate can reach 98%.

[0031] Baojoside was prepared by Waters 600E pr...

Embodiment 2

[0033] Take 5 mg of icariin, dissolve it in 15 ml of citric acid buffer solution with pH 7, add 500 ul of 5 ug / ul enzyme mother solution, and hydrolyze at room temperature (about 19 degrees Celsius) for 6 hours; centrifuge to precipitate baojoside I. The enzymatic hydrolysis product baojoside I precipitate was washed with water and centrifuged at 2000r / min for 5 minutes, the supernatant was discarded, and the process of washing, centrifuging and discarding the supernatant was repeated three times. Collect the precipitate, dissolve it with 5ml of cold methanol (4 degrees Celsius), dissolve it with ultrasound, centrifuge at 2000r / min for 5 minutes, collect the supernatant, dissolve the solid with cold methanol again, dissolve it with ultrasound, centrifuge, and collect the supernatant, repeat three times in total. The supernatants were combined and concentrated for three times to obtain the crude product of baojoside I, and the conversion rate could reach 97%.

[0034] Baojoside...

Embodiment 3

[0036] Take 25 mg of icariin, dissolve it in 100 ml of citric acid buffer solution with pH 4, add 1 ml of 5 ug / ul enzyme mother solution, and hydrolyze at 80 degrees Celsius for 3 hours; centrifuge to precipitate Baojoside I. The enzymatic hydrolysis product baojoside I precipitate was washed with water and centrifuged at 2000r / min for 5 minutes, the supernatant was discarded, and the process of washing, centrifuging and discarding the supernatant was repeated three times. Collect the precipitate, dissolve it with 8ml of cold methanol (-2 degrees Celsius), dissolve it with ultrasound, centrifuge at 2000r / min for 5 minutes, collect the supernatant, dissolve the solid with cold methanol again, dissolve it with ultrasound, centrifuge, and collect the supernatant, repeat three times in total , the supernatant was combined and concentrated for three times to obtain the crude product of baojoside I, and the conversion rate could reach 97.5%.

[0037] Baojoside was prepared by Waters...

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Abstract

The invention relates to a method for a preparing po huo glycoside I refined product. The method includes the steps of using icariin (purity is larger than 98%) which is self-made through a laboratory as raw materials, carrying out hydrolysis of glucanase, obtaining a po huo glycoside I coarse product with content larger than 90%, using reverse phase efficient preparative chromatography as a purifying method, and obtaining the po huo glycoside I refined product with purity larger than 98%. The method is simple in process procedures, high in purity, low in cost, and suitable for mass production.

Description

[0001] Technical Field The present invention relates to a method for preparing pure baojoside I. It mainly includes glucanase hydrolysis of icariin, and reversed-phase high performance liquid phase preparation and purification of baochoside I. Background technique [0002] Herba Epimedii (Herba Epimedii) belongs to the Berberidaceae (Berberidaceae) Epimedium genus, is a commonly used traditional Chinese medicine, has the functions of strengthening muscles and bones, dispelling rheumatism, and antiviral. Modern pharmacological studies have found that low-molecular-weight compounds after desugaring, such as baojoside I in Epimedium, have higher activity than icariin with a higher content. In the current market, baojoside I is very scarce and expensive, and the demand for baojoside I is increasing, so it is very meaningful to develop a preparation method for baojoside I. According to the existing patents and documents, the main preparation methods of baojoside include acid hydro...

Claims

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Application Information

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IPC IPC(8): C12P19/60C07H17/07C07H1/06
Inventor 肖红斌杨乾栩王莉
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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