Separation and purification method of three iridoid components in radix scrophulariae

A technology for the separation and purification of iridoids, applied in chemical instruments and methods, organic chemistry, preparation of sugar derivatives, etc., can solve the problems of irreversible adsorption, time-consuming, laborious, and environmental pollution, and achieve no loss of samples and reduce The effect of high cost and recovery rate

Inactive Publication Date: 2018-08-24
SOUTHWEST UNIVERSITY
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Problems solved by technology

[0003] In summary, the problems in the prior art are: Traditional separation methods such as ordinary chromatographic column method and recrystallization to separate ef

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  • Separation and purification method of three iridoid components in radix scrophulariae

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[0029] Example 1

[0030]The ratio of solid to liquid: 1:10, 1:15, 1:20, 1:25, 1:30 respectively; the experimental results show that with the increase of the ratio of solid to liquid, the extraction rate of iridoids also gradually When the ratio of solid to liquid reaches 1:20, the extraction rate reaches the highest value, the ratio of solid to liquid continues to increase, and the extraction rate shows a downward trend. It may be because, with the increase of the solid-liquid ratio, the contact area between the solution and the Scrophulariaceae powder becomes larger, which is conducive to the enzymatic hydrolysis reaction; but when the solid-liquid ratio is too large, the cellulase in the reaction system will be reduced. concentration, and the catalytic activity of cellulase [9] , thereby reducing the extraction rate of iridoid components. Therefore, the material-liquid ratio of 1:20 was taken as the central level, and the subsequent orthogonal experiment optimization was ...

Example Embodiment

[0031] Example 2

[0032] Solution pH: 3, 3.5, 4, 4.5, 5, respectively. The experimental results showed that when the pH was between 3 and 3.5, the extraction rate of iridoids gradually increased and reached the maximum value at pH 3.5; when the pH exceeded 3.5, the extraction rate decreased significantly. This is because pH is an important factor affecting the enzymatic hydrolysis efficiency. When the cellulase is at a suitable pH, the enzymatic activity is the highest and the enzymatic hydrolysis reaction efficiency is the highest. When the pH exceeds 3.5, the enzymatic activity decreases and the enzymatic hydrolysis efficiency is reduced. also gradually decreased. Therefore, the solvent pH 3.5 was taken as the central level, and the subsequent orthogonal experiment optimization was carried out.

Example Embodiment

[0033] Example 3

[0034] Extraction time: Select the extraction time as 0.5h, 1h, 1.5h, 2h, 2.5h, respectively. The experimental results show that the extraction rate of iridoids in the extraction time of 0.5 to 2 hours is in a gradually increasing trend. This is because in the initial stage of extraction, the enzyme concentration is high and the enzyme activity is large, which can quickly The cell wall of ginseng was enzymatically hydrolyzed, and the iridoids were dissolved out, so that the extraction rate gradually increased; but when the extraction time was longer than 2h, the extraction rate of iridoids began to gradually decrease. Therefore, the extraction time 2h was taken as the center level, and the subsequent orthogonal experiment optimization was carried out.

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Abstract

The invention belongs to the technical field of separation and purification of radix scrophulariae iridoid compounds and discloses a separation and purification method of three iridoid components in radix scrophulariae. The separation and purification method comprises the following steps: weighing 10kg of the radix scrophularia; adding purified water which is 15 times of the radix scrophularia; adjusting the pH (Potential of Hydrogen) value to 3.5; carrying out crude separation; refluxing and extracting for 2h at the temperature of 60 DEG C; filtering and collecting filtrate; extracting filtrate from filtering dreg according to the above method; combining the filtrate of the two times; evaporating on a rotary evaporator to obtain extract, wherein the yield of the extract is about 31.5 percent; purifying by high-speed counter-current chromatography. The separation and purification method disclosed by the invention has the characteristics of great separation amount, no sample loss, highrecovery rate, mild separation environment, solvent saving and the like and is widely applied to preparation, separation and purification of chemical substances in the fields including biology, medicines, environment protection and the like.

Description

technical field [0001] The invention belongs to the technical field of separation and purification of iridoid compounds from Scrophulariaceae, in particular to a method for separation and purification of three iridoid components in Scrophulariaceae. Background technique [0002] At present, the existing technologies commonly used in the industry are as follows: Scrophulariaceae is the dried root of Scrophulariaceae Scrophulariaceae. Traditional Chinese medicine believes that Scrophulariaceae is sweet, bitter, and salty, and its nature is slightly cold. It has the effects of nourishing yin and cooling blood, purging fire and detoxifying, etc. Restless sleep at night, spontaneous night sweats, sore throat embolism, is a commonly used traditional Chinese medicine in clinic. Modern medicine shows that Scrophulariaceae contains glycosides, alkaloids and other ingredients, which have anti-inflammatory, anti-tumor, and liver-protecting effects. In the prior art, traditional separ...

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Application Information

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IPC IPC(8): C07H1/08C07H17/04
CPCC07H1/08C07H17/04
Inventor 陈章宝刘娇娇
Owner SOUTHWEST UNIVERSITY
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