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Method for refining crude baicalin

A technology of crude baicalin and refining method, which is applied in the field of alcohol precipitation to separate and refine baicalin, and achieves the effects of simple process, reliable powder injection quality and easy production

Active Publication Date: 2015-02-25
HEBEI YILING MEDICINE INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] On this basis, further refining can make the content reach more than 90%. For example, Chinese patent CN101475618A is to dissolve the crude baicalin with alkali, add alcohol to precipitate some impurities, filter, and then use acid to precipitate baicalin. This refining method It can increase the content of baicalin to 92%. Although it can meet the production needs of injections, it still contains a large amount of impurities, which inevitably brings adverse drug reactions and quality problems.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033]a. 0.3Kg of crude baicalin, add 2.5L of deionized water, heat and stir in a water bath to form a homogeneous body, adjust the pH to 6.44 with 30% sodium hydroxide solution to dissolve, filter, and add 2.5L of 95% baicalin to the filtrate After stirring with ethanol, immediately adjust the pH to 2.08 with 2mol / L HCL, heat it to 50°C with stirring and keep it warm for 40 minutes, leave it at room temperature for 12 hours, filter, then add 600ml of 50% medicinal ethanol on the filter cake and let it settle naturally until it does not drip , then suction filtered and dried to obtain Intermediate A;

[0034] b. Add 1.5L deionized water to intermediate A, stir to form a homogeneous body, adjust pH 6.80 with 30% sodium hydroxide solution to dissolve, filter, add 9.1L 95% medicinal ethanol adjusted pH 2.20 with hydrochloric acid and stir in the filtrate Evenly placed for 3h, filtered. Add 1.0L deionized water to the precipitate, stir to form a homogeneous body, then add 1.0L of...

Embodiment 2

[0037] a. 0.3Kg of crude baicalin, add 2.0L of deionized water, heat and stir in a water bath to form a homogeneous body, adjust the pH to 6.80 with 20% sodium hydroxide solution to dissolve, filter, and add 2.2L of 95% baicalin to the filtrate After mixing with ethanol, immediately adjust the pH to 2.05 with 4mol / L HCL, heat it to 75°C for 30 minutes under stirring, leave it at room temperature for 16 hours, filter, then add 600ml of 50% medicinal ethanol on the filter cake and let it settle naturally until it does not drip , then suction filtered and dried to obtain Intermediate A;

[0038] b. Add 1.8L deionized water to intermediate A, stir to form a homogeneous body, adjust pH 6.80 with 40% sodium hydroxide solution to dissolve, filter, add 8L 95% medicinal ethanol to the filtrate, stir well, and immediately adjust pH 5 with hydrochloric acid. 3, then place for 2h, filter. Add 1.0L deionized water to the precipitate, stir to form a homogeneous body, then add 1.0L of 95% m...

Embodiment 3

[0041] a. Add 0.3Kg of crude baicalin with 2.0L of deionized water, heat and stir in a water bath to form a homogeneous body, adjust the pH to 7.0 with 20% sodium hydroxide solution to dissolve, filter, and add 2.0L of 95% medicinal product to the filtrate Immediately adjust the pH to 2.08 with 2N HCL after stirring the ethanol, heat it to 78°C and keep it warm for 30 minutes under stirring, place it at room temperature for 12 hours, filter, then add 400ml of 50% medicinal ethanol on the filter cake and let it settle naturally until it does not drip, then suction filter, Dry to obtain Intermediate A;

[0042] b. Add 1.5L of deionized water to intermediate A, stir to form a homogeneous body, adjust the pH to 6.50 with 40% sodium hydroxide solution to dissolve, filter, add 11.0L of 95% medicinal ethanol to the filtrate, stir well, and immediately adjust the pH to 4 with hydrochloric acid .9, then placed for 1h, filtered. Add 0.8L deionized water to the precipitate, stir to form...

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PUM

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Abstract

The invention discloses a method for refining crude baicalin and relates to the technology of glycosides extraction such as acid protection and alcohol precipitation and is used for refining baicalin. In the invention, alcohol, hydrochloric acid, sodium hydroxide and de-ionized water are adopted to remove impurities of different polarities stepwise, the obtained sample is baicalin exclusively, the purify of the baicalin is as high as over 99 percent, and the total transfer rate of the baicalin is over 85 percent.

Description

technical field [0001] The invention relates to a method for refining crude baicalin, in particular to a method for separating and refining baicalin by alcohol precipitation. Background technique [0002] The main purpose of the production process of traditional Chinese medicine preparations is to enrich the active ingredients and remove invalid impurities. Baicalin is one of the active ingredients in Scutellaria baicalensis, which has antibacterial, antiviral, anti-inflammatory, antihypertensive, sedative, hepatoprotective, choleretic, and other pharmacological effects. The content of baicalin in Scutellaria baicalensis is high (7.0-20%), and the traditional crude baicalin extraction can be extracted by water extraction and acid precipitation, such as Zhai Baotong et al [Zhai Baotong, Wang Ying. Research on the extraction process of baicalin. , 4(23):91-93] that is, the method of water extraction and acid precipitation is adopted, and the content of baicalin in the obtaine...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/07C07H1/06
Inventor 贾继明宋剑孟作环马振嗣
Owner HEBEI YILING MEDICINE INST