Preparation method of isodon excisoides total diterpenoid extractive

Abstract

The invention relates to a preparation method of an isodon excisoides total diterpenoid extractive, which is capable of effectively solving the problem of extracting total diterpenoid from isodon excisoides with high quality and high extraction rate. The preparation method disclosed by the invention comprises the following steps of crushing isodon excisoides, decocting by adding water, filtering water decoction, and cooling to form sampling solution; after immersing macroreticular resin by using ethanol, dynamically cleaning resin by using ethanol, washing till alcohol smell does not exist, immersing by using hydrochloric acid, washing again till the macroreticular resin is neutral, then, immersing by using NaOH solution, dynamically cleaning resin, washing till the macroreticular resin is neutral, after dynamically eluting ethanol, packing the macroreticular resin in a column through a wet method, and dynamically absorbing the sampling solution through a resin column; and eluting the sample column by using water after absorbing, eluting through ethanol again, collecting ethanol eluent, decompressing and recycling the solvent, and evaporating, thereby obtaining the isodon excisoides total diterpenoid extractive. The preparation method disclosed by the invention is simple, easy to operate and use, steady, reliable, high in product yield, good in quality, simple, practical and free from pollution; research basis is provided for researching isodon amethystoides diterpenoid anti-tumour candidate drugs.

Description

Technical field

[0001] The invention relates to a preparation method of the total diterpene extract of the pseudo-fragrant tea and the macroporous adsorption resin, and belongs to the field of medicine. Background technique

[0002] The coriander genus plants have shown obvious anti-tumor effects. Since 1976, the diterpenoids in this genus have become the focus of domestic and foreign scholars seeking new anti-tumor lead compounds. In recent years, with the discovery of new diterpenoids from coriander, a large number of cytotoxic diterpenoids from coriander have been reported. Currently, as anti-tumor candidate compounds, Rubescensine A and Calyx coriander A have been reported. , Big-leaf scented tea vegetable enanthus, etc., related products of three sisters slices (Xinle scented tea vegetable), Rubescens syrup, slices (Didophyllum vulgaris), Anti-inflammatory and gallbladder slices (including Xihuangcao), etc. In addition, there are reports showing that the diterpenoids of fra...

Examples

Embodiment 1

[0020] In specific implementation, the present invention is realized by the following steps:

[0021] (1) Preparation of sample solution: crush 1kg of dry medicinal materials of the scented tea vegetable, add water to decocting twice, decocting for 1 hour each time, add 12L of water for the first time, and add 8L of water for the second time. Combine the two decoctions, filter, and let stand and cool to room temperature to obtain 10L of supernatant, which is the sample liquid;

[0022] (2) Pretreatment of the resin: The method is to soak the D101 macroporous adsorption resin with 95% ethanol by volume for 24 hours, then wet pack the column, and dynamically clean the resin with 95% ethanol by volume. The amount of ethanol added It is 5 times the volume of the resin, and then washed with water until there is no alcohol smell, and then soaked in hydrochloric acid with a volume concentration of 5% for 6 hours to dynamically clean the resin. The amount of hydrochloric acid added is 3 ti...

Embodiment 2

[0026] The present invention is realized by the following steps:

[0027] (1) Preparation of sample solution: crush 1kg of dry medicinal materials of the scented tea vegetable, add water to decocting twice, decocting for 1 hour each time, add 12L of water for the first time, and add 8L of water for the second time. Combine the two decoctions, filter, and let stand and cool to room temperature to obtain 10L of supernatant, which is the sample liquid;

[0028] (2) Pretreatment of the resin: The method is that the HP20 macroporous adsorption resin is soaked in ethanol with a volume concentration of 95% for 24 hours, then the column is wet-packed, and the resin is dynamically cleaned with ethanol with a volume concentration of 95%. The amount of ethanol added It is 5 times the volume of the resin, and then washed with water until there is no alcohol smell, and then soaked in hydrochloric acid with a volume concentration of 5% for 6 hours to dynamically clean the resin. The amount of hy...

Embodiment 3

[0032] The present invention is realized by the following steps:

[0033] (1) Preparation of sample solution: crush 1kg of dry medicinal materials of the scented tea vegetable, add water to decocting twice, decocting for 1 hour each time, add 12L of water for the first time, and add 8L of water for the second time. Combine the two decoctions, filter, and let stand and cool to room temperature to obtain 10L of supernatant, which is the sample liquid;

[0034] (2) Pretreatment of the resin: The method is to soak the AB8 macroporous adsorption resin with 95% ethanol by volume for 24 hours, then wet-pack the column, and dynamically clean the resin with 95% ethanol by volume. The amount of ethanol added It is 5 times the volume of the resin, and then washed with water until there is no alcohol smell, and then soaked in hydrochloric acid with a volume concentration of 5% for 6 hours to dynamically clean the resin. The amount of hydrochloric acid added is 3 times the volume of the resin, ...

Technical field

[0001] The invention relates to a preparation method of the total diterpene extract of the pseudo-fragrant tea and the macroporous adsorption resin, and belongs to the field of medicine. Background technique

[0002] The coriander genus plants have shown obvious anti-tumor effects. Since 1976, the diterpenoids in this genus have become the focus of domestic and foreign scholars seeking new anti-tumor lead compounds. In recent years, with the discovery of new diterpenoids from coriander, a large number of cytotoxic diterpenoids from coriander have been reported. Currently, as anti-tumor candidate compounds, Rubescensine A and Calyx coriander A have been reported. , Big-leaf scented tea vegetable enanthus, etc., related products of three sisters slices (Xinle scented tea vegetable), Rubescens syrup, slices (Didophyllum vulgaris), Anti-inflammatory and gallbladder slices (including Xihuangcao), etc. In addition, there are reports showing that the diterpenoids of fra...

Examples

Embodiment 1

[0020] In specific implementation, the present invention is realized by the following steps:

[0021] (1) Preparation of sample solution: crush 1kg of dry medicinal materials of the scented tea vegetable, add water to decocting twice, decocting for 1 hour each time, add 12L of water for the first time, and add 8L of water for the second time. Combine the two decoctions, filter, and let stand and cool to room temperature to obtain 10L of supernatant, which is the sample liquid;

[0022] (2) Pretreatment of the resin: The method is to soak the D101 macroporous adsorption resin with 95% ethanol by volume for 24 hours, then wet pack the column, and dynamically clean the resin with 95% ethanol by volume. The amount of ethanol added It is 5 times the volume of the resin, and then washed with water until there is no alcohol smell, and then soaked in hydrochloric acid with a volume concentration of 5% for 6 hours to dynamically clean the resin. The amount of hydrochloric acid added is 3 ti...

Embodiment 2

[0026] The present invention is realized by the following steps:

[0027] (1) Preparation of sample solution: crush 1kg of dry medicinal materials of the scented tea vegetable, add water to decocting twice, decocting for 1 hour each time, add 12L of water for the first time, and add 8L of water for the second time. Combine the two decoctions, filter, and let stand and cool to room temperature to obtain 10L of supernatant, which is the sample liquid;

[0028] (2) Pretreatment of the resin: The method is that the HP20 macroporous adsorption resin is soaked in ethanol with a volume concentration of 95% for 24 hours, then the column is wet-packed, and the resin is dynamically cleaned with ethanol with a volume concentration of 95%. The amount of ethanol added It is 5 times the volume of the resin, and then washed with water until there is no alcohol smell, and then soaked in hydrochloric acid with a volume concentration of 5% for 6 hours to dynamically clean the resin. The amount of hy...

Embodiment 3

[0032] The present invention is realized by the following steps:

[0033] (1) Preparation of sample solution: crush 1kg of dry medicinal materials of the scented tea vegetable, add water to decocting twice, decocting for 1 hour each time, add 12L of water for the first time, and add 8L of water for the second time. Combine the two decoctions, filter, and let stand and cool to room temperature to obtain 10L of supernatant, which is the sample liquid;

[0034] (2) Pretreatment of the resin: The method is to soak the AB8 macroporous adsorption resin with 95% ethanol by volume for 24 hours, then wet-pack the column, and dynamically clean the resin with 95% ethanol by volume. The amount of ethanol added It is 5 times the volume of the resin, and then washed with water until there is no alcohol smell, and then soaked in hydrochloric acid with a volume concentration of 5% for 6 hours to dynamically clean the resin. The amount of hydrochloric acid added is 3 times the volume of the resin, ...

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