High-efficiency preparation method for acetyl harpagide reference standard product

A technology of acetyl harpatoside and reference substance, which is applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., to achieve the effects of less solvent consumption, less environmental pollution, and less solvent toxicity

Active Publication Date: 2014-05-21
CHENGDU PUSH BIOLOGICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there are few domestic literature reports on the separation and purification of acetyl harpaside, and it is the first time that high-efficiency preparative liquid chromatography is used for the separation and purification of acetyl harpaside reference substance

Method used

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  • High-efficiency preparation method for acetyl harpagide reference standard product
  • High-efficiency preparation method for acetyl harpagide reference standard product
  • High-efficiency preparation method for acetyl harpagide reference standard product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A high-efficiency preparation method of acetylharpaside reference substance is characterized in that it is carried out according to the following process steps:

[0026] A. Extraction of raw materials: Grind 2kg of herba sinensis into coarse powder, add 20L of ethanol solution with a volume fraction of 40%, reflux extraction for 3 times, each time for 2 hours, combine the extracts, and cool to room temperature;

[0027] B. Macroporous resin enrichment: Weigh 1kg D101 macroporous adsorption resin, fill it with a 10cm diameter glass column to form a resin column, and the volume of the resin bed is about 3L; pass the cooled extract through the activated macropore at a speed of 3BV The adsorption resin column is used for adsorption, and then 9L of water and 6L of ethanol solution with a volume fraction of 40% are used to elute impurities, and then 6L of ethanol solution with a volume fraction of 60% is used to elute the target substance, and the eluate is collected and conce...

Embodiment 2

[0031] A high-efficiency preparation method of acetylharpaside reference substance is characterized in that it is carried out according to the following process steps:

[0032] A. Extraction of raw materials: Grind 5 kg of herba sinensis into coarse powder, add 40 L of ethanol solution with a volume fraction of 45%, reflux extraction for 3 times, each time for 2 hours, combine the extracts, and cool to room temperature;

[0033] B. Macroporous resin enrichment: Weigh 2kg AB-8 macroporous adsorption resin, fill it with a 10cm-diameter glass column to form a resin column, and the volume of the resin bed is about 6L; pass the cooled extract through the activated The macroporous adsorption resin column is adsorbed, and then 18L of water and 12L of ethanol solution with a volume fraction of 40% are used to elute impurities, and then 12L of ethanol solution with a volume fraction of 60% is used to elute the target substance, and the eluate is collected and concentrated to About 1.2L...

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Abstract

The invention discloses a high-efficiency preparation method for an acetyl harpagide reference standard product and belongs to the technical field of Chinese medicine modernization. The method comprises the following process steps of: A, extracting raw materials, namely performing refluxing extraction for 3 times by using 40 to 60 percent ethanol and 2 hours each time; B, enriching by using macroporous resin, namely removing impurities by using water and ethanol and eluting the target substance by using the ethanol; C, performing high-efficiency preparation and liquid phase separation, wherein the mobile phase is a 20 to 30 volume percent methanol solution and the detection wavelength is 210 nm; and D, recovering products, namely eluting by using the ethanol, concentrating and drying to obtain acetyl harpagide reference standard product with the purity of over 99 percent. The method is simple and quick, low in solvent consumption, high in yield and economic and environment-friendly, and has high economic value and academic value.

Description

Technical field [0001] The present invention involves a preparation method of a Chinese medicine chemical control product, which is a modern technology field of traditional Chinese medicine. Specifically, the invention involves a method of rapidly separating acetyl Haboside control from Chinese medicine muscles and bone grass. Background technique [0002] Ajugae Herba (Ajugae Herba), which is a genus of Labiaatae ( Ajuga L.) Plant muscles and bones ( Ajuga decumbens Thunb.) The dry whole grass, also known as the golden sore grass, the gallbladder, the bitter grass, and the scattered blood grass.The taste is bitter, cold, and returns to the lung meridian.It has the effect of clearing heat and detoxifying, cooling blood and swelling.It is used for sore throat, blood hemoptysis, and swelling and pain.The newly collected variety for the 2010 version of "China Pharmacopoeia". [0003] Acetyl Haboside (8-O-AceTylharpagide), molecular formula is C 17 H 26 O 11 , Structural formula as f...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/04C07H1/08
Inventor 夏柯文焕松郭建华刘丁
Owner CHENGDU PUSH BIOLOGICAL TECH
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