Method for separating cytospaz total alkaloid from traditional Chinese medicine extract liquid

Abstract

The invention discloses a method for separating total alkaloid from traditional Chinese medicine, in particular a method for separating belladonna total alkaloid from traditional Chinese medicine extract, which belongs to the field of traditional Chinese medicines. The method comprises the following technical proposal that the traditional Chinese medicine extract is taken and filtered; the pH value of the traditional Chinese medicine extract is adjusted to be between 1 and 7; filtrate is added to a cation exchange resin column, eluted with water to remove impurities and then eluted by use of 0.5 to 15 percent acid liquid; and eluent is collected, added with alkali for neutralization and desalted so as to prepare belladonna total alkaloid. The method overcomes the deficiency that the prior art is low in extraction ratio, large in the amount of organic solvents, complex in process, incapable of mass production, and the like, and can efficiently separate high-purity belladonna total alkaloid from traditional Chinese medicine extract.

Description

technical field

[0001] The invention relates to a method for extracting and separating active ingredients of traditional Chinese medicines, in particular to a method for extracting and separating total alkaloids of hyoscyamine from traditional Chinese medicine extracts, which belongs to the field of traditional Chinese medicines. Background technique

[0002] Traditional Chinese medicine alkaloids are an important class of substances existing in nature, and more than 700 species have been isolated so far. They are the largest class of active ingredients in traditional Chinese medicine with definite curative effects and a wide range of uses, especially for cancer, liver disease, cardiovascular and cerebrovascular diseases, and rheumatism. etc. have unique curative effects, such as ephedrine in ephedra for relieving asthma, reserpine in Rauwolfia for lowering blood pressure, galantamine in lycoris for sequelae of poliomyelitis, and the Morphine is a famous analgesic; quinine i...

Examples

Embodiment 1

[0040] Take 1000g of Yangjinhua slices, add water and decoct twice, 10 times the amount each time, decoct for 2 hours, combine the decoction liquid, centrifuge, adjust the pH=3, centrifuge, and the supernatant passes through the cation at 4 times the column volume / hour Exchange resin (001×7, hydrogen type, diameter-to-height ratio 1:8), wash with water until the effluent is colorless, add 3% hydrochloric acid for elution, and the elution rate is 2 times the column volume / hour, collect the eluent, until The alkaloid test was negative (the effluent was added dropwise with 10% silicotungstic acid without precipitation), neutralized to neutral with sodium hydroxide, desalinated, and the filtrate was concentrated and dried to obtain the total alkaloids of Datura japonica.

Embodiment 2

[0042] Get 1000g of Teng Gong Teng decoction pieces, add acidic water with pH=5 for percolation, combine the percolation solution and add water to dilute to 10000ml, centrifuge, adjust pH=1, centrifuge, supernatant passes through cation exchange resin (AmberliteIR- -120, hydrogen type, diameter-to-height ratio 1:6), washed with water until the effluent was colorless, then eluted with 0.5% hydrochloric acid solution, the elution rate was 4 times the column volume / hour, after elution was 2 times the column volume, soaked for 5 hours, then eluted until the alkaloid test was negative (the effluent was added dropwise with 10% silicotungstic acid without precipitation), collected this part of the eluate, neutralized to neutral with calcium hydroxide, desalinated, and the filtrate was concentrated and dried to obtain Ding Gongteng total alkaloids.

Embodiment 3

[0044] Take 5 kg of yangjinhua decoction pieces, add 70% ethanol to ultrasonically extract twice, add 5 times the amount each time, ultrasonically for 0.5 hours, combine the extracts, centrifuge, recover ethanol, add water to 5000ml, adjust pH = 2, centrifuge, and supernatant Pass through the upper cation exchange resin (001×10, sodium type, diameter-to-height ratio 1:7) at 2 times the column volume / hour, wash with water until the effluent is colorless, and then use 6% sulfuric acid solution (containing 1mol / L of CaCl 2 ) elution, the elution rate is 5 times column volume / hour, collect the eluate until the alkaloid test is negative (the effluent is added dropwise with 10% silicotungstic acid without precipitation), and neutralized to neutral with sodium hydroxide, Desalting, the filtrate was concentrated and dried to obtain the total alkaloids of Dajinhua.

technical field

[0001] The invention relates to a method for extracting and separating active ingredients of traditional Chinese medicines, in particular to a method for extracting and separating total alkaloids of hyoscyamine from traditional Chinese medicine extracts, which belongs to the field of traditional Chinese medicines. Background technique

[0002] Traditional Chinese medicine alkaloids are an important class of substances existing in nature, and more than 700 species have been isolated so far. They are the largest class of active ingredients in traditional Chinese medicine with definite curative effects and a wide range of uses, especially for cancer, liver disease, cardiovascular and cerebrovascular diseases, and rheumatism. etc. have unique curative effects, such as ephedrine in ephedra for relieving asthma, reserpine in Rauwolfia for lowering blood pressure, galantamine in lycoris for sequelae of poliomyelitis, and the Morphine is a famous analgesic; quinine i...

Examples

Embodiment 1

[0040] Take 1000g of Yangjinhua slices, add water and decoct twice, 10 times the amount each time, decoct for 2 hours, combine the decoction liquid, centrifuge, adjust the pH=3, centrifuge, and the supernatant passes through the cation at 4 times the column volume / hour Exchange resin (001×7, hydrogen type, diameter-to-height ratio 1:8), wash with water until the effluent is colorless, add 3% hydrochloric acid for elution, and the elution rate is 2 times the column volume / hour, collect the eluent, until The alkaloid test was negative (the effluent was added dropwise with 10% silicotungstic acid without precipitation), neutralized to neutral with sodium hydroxide, desalinated, and the filtrate was concentrated and dried to obtain the total alkaloids of Datura japonica.

Embodiment 2

[0042] Get 1000g of Teng Gong Teng decoction pieces, add acidic water with pH=5 for percolation, combine the percolation solution and add water to dilute to 10000ml, centrifuge, adjust pH=1, centrifuge, supernatant passes through cation exchange resin (AmberliteIR- -120, hydrogen type, diameter-to-height ratio 1:6), washed with water until the effluent was colorless, then eluted with 0.5% hydrochloric acid solution, the elution rate was 4 times the column volume / hour, after elution was 2 times the column volume, soaked for 5 hours, then eluted until the alkaloid test was negative (the effluent was added dropwise with 10% silicotungstic acid without precipitation), collected this part of the eluate, neutralized to neutral with calcium hydroxide, desalinated, and the filtrate was concentrated and dried to obtain Ding Gongteng total alkaloids.

Embodiment 3

[0044] Take 5 kg of yangjinhua decoction pieces, add 70% ethanol to ultrasonically extract twice, add 5 times the amount each time, ultrasonically for 0.5 hours, combine the extracts, centrifuge, recover ethanol, add water to 5000ml, adjust pH = 2, centrifuge, and supernatant Pass through the upper cation exchange resin (001×10, sodium type, diameter-to-height ratio 1:7) at 2 times the column volume / hour, wash with water until the effluent is colorless, and then use 6% sulfuric acid solution (containing 1mol / L of CaCl 2 ) elution, the elution rate is 5 times column volume / hour, collect the eluate until the alkaloid test is negative (the effluent is added dropwise with 10% silicotungstic acid without precipitation), and neutralized to neutral with sodium hydroxide, Desalting, the filtrate was concentrated and dried to obtain the total alkaloids of Dajinhua.

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