Method for preparing high-purity baicalin

A baicalin, high-purity technology, applied in the field of preparation of high-purity baicalin, can solve the problems of cumbersome preparation process, expensive equipment, capillary blockage, etc., and achieve the effect of high separation efficiency, simple operation and low cost

Active Publication Date: 2012-07-18
SHENYANG PHARMA UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In recent years, literature reports mainly contain high-speed countercurrent chromatography (Haitao Lu, Yue Jiang.Feng Chen.Journal of Chromatography A, 1017(2003): 117-123; Sujuan Wu, Ailing Sun, Renmin Liu.Journal ofChromatographyA, 1066 (2005): 243-247.), the shortcoming of this method is to require special instrument, and preparation process is loaded down with trivial details, and the time spent of preparing a large amount of target products is longer; Next also has the method of solvent extraction (Huiru Dong, Pengyu Bi, Shihui Wang.Analytical Letters, 38(2005): 257-270; Emika Ohkoshi, Tomomi Nagashima, et al.Journal of Chromatography A, 1216(2009): 2192-2194.), its shortcoming is that a large amount of Organic solvents can cause serious pollution to the environment; literature has also reported that the main component (Mei-Chih Lin, Ming-Jer Tsai, Kuo-Ching Wen.Journal of Chromatography A, 830( 1999): 387-395.), but the instruments involved in this method a

Method used

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  • Method for preparing high-purity baicalin
  • Method for preparing high-purity baicalin
  • Method for preparing high-purity baicalin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Take 100g of Scutellaria baicalensis, add 600mL of water, heat to 60°C for extraction, extract for 1 hour, extract 3 times, add the extract to the treated HPD-100 macroporous adsorption resin column for adsorption, and elute with 5BV of water. Discard, then elute with 5BV10% ethanol water, recover the solvent, discard the residue, then elute with 40% ethanol water, collect 40% eluate (5BV), concentrate under reduced pressure, and freeze-dry to obtain crude baicalin 6.69g, the crude product is recrystallized with ethanol / water / acetic acid (4 / 6 / 1) to obtain baicalin 4.93g, the content of baicalin is 98.60% through HPLC analysis, as attached Figure 4 shown.

Embodiment 2

[0036]Take 100g of Scutellaria baicalensis, add 700mL of water, heat to 70°C for extraction, extract for 2 hours, extract 3 times, add the extract to the treated HPD-300 macroporous adsorption resin column for adsorption, and elute with 5BV of water. Discarded, then eluted with 5BV20% ethanol water, recovered the solvent, discarded the residue, then eluted with 50% ethanol water, collected 50% eluent (5BV), concentrated under reduced pressure, and freeze-dried to obtain crude baicalin 6.85 g, the crude product was recrystallized with ethanol / water / acetic acid (3:7:1) to obtain 5.12 g of baicalin, and the content of baicalin was 98.32% by HPLC analysis.

Embodiment 3

[0038] Take 100g of Scutellaria baicalensis, add 800mL of water, heat to 80°C for extraction, extract for 3 hours, extract 3 times, add the extract to the treated D-101 macroporous adsorption resin column for adsorption, and elute with 5BV of water. Discarded, then eluted with 5BV30% ethanol water, recovered the solvent, discarded the residue, then eluted with 60% ethanol water, collected 60% eluate (5BV), concentrated under reduced pressure, and freeze-dried to obtain crude baicalin 6.21g, this product was recrystallized with ethanol / water / acetic acid (2:8:1) to obtain 4.73g of baicalin, the content of baicalin was 99.10% by HPLC analysis.

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Abstract

The invention relates to a simple and effective method for preparing high-purity baicalin, and relates to an extraction method of medicinal herb. The method comprises the steps of: extracting the medicinal herb with aqueous solution to obtain extract, adsorbing the extract with screened macroporous adsorbent resin, eluting with 0-30% ethanol water solution to remove impurities, then eluting with 40-60% ethanol water solution, concentrating the eluate under reduced pressure, then carrying out freeze drying to obtain a crude product with baicalin content more than 80%, and recrystallizing the crude product with ethanol/water/acetic acid solvent system to obtain the light yellow product, the purity of which is more than 98% detected by high-performance liquid chromatography. The method provided by the invention is simple in process, low in cost, mild in condition and environment-friendly, and is more suitable for industrial production of high-purity baicalin.

Description

technical field [0001] What this patent relates to is a kind of preparation method that can be used as the raw material medicine of pharmaceutical industry, what specifically relate to is the preparation method of high-purity baicalin (Baicalin). Background technique [0002] Scutellaria baicalensis is the dry root of Scutellaria baicalensis Georgi, a plant in the Labiatae family. It is a commonly used traditional Chinese medicine. Clinically, it is widely used in diseases such as pulmonary fever, hemoptysis, enteritis and dysentery, jaundice, hypertension and suppurative infection. Baicalin is the main medicinal component of Scutellaria baicalensis, which has a variety of significant biological activities, including anti-inflammatory, anti-viral, anti-tumor, chemoprevention, etc. As a medicine, baicalin is clinically used for diseases such as pneumonia, hepatitis, and infection, such as baicalin tablets, baicalin capsules, etc. The structural formula of baicalin is as fol...

Claims

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Application Information

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IPC IPC(8): C07H17/07C07H1/08
Inventor 邱峰杜占权陈丽霞王琨康宁
Owner SHENYANG PHARMA UNIVERSITY
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