Catharanthus roseus total alkaloids separation method in Catharanthus roseus extract

Abstract

The invention discloses a method for separating total alkaloid from traditional Chinese medicine, in particular a method for separating total alkaloid from an extracting solution of the traditional Chinese medicine, namely Catharanthus roseus, and belongs to the field of traditional Chinese medicines. The method comprises the following technical proposal: taking the extracting solution of the Catharanthus roseus; adjusting the pH value of the extracting solution to between 1 and 7; filtering the extracting solution; taking and adding the filtrate to a cation exchange resin column; rinsing the filtrate and removing the impurities; eluting the filtrate with 0.5 to 15 percent acid liquor; checking eluent until no alkaloid exists; collecting the eluent; adding alkali to the eluent for neutralization; performing desalting treatment on the mixed solution; and performing concentrated drying to obtain the Catharanthus roseus total alkaloid. The method overcomes the defects of low extracting rate, large using level of organic solvent, complicated process, inability of large-scale production, and the like in the prior art and can efficiently separate high purity of the Catharanthus roseus total alkaloid from the extracting solution of the Catharanthus roseus.

Description

technical field

[0001] The invention relates to the extraction and separation of effective components of traditional Chinese medicine, in particular to a method for extracting and separating total alkaloids of periwinkle from traditional Chinese medicine periwinkle extract, which belongs to the field of traditional Chinese medicine. Background technique

[0002] Alkaloids are a large class of basic nitrogen-containing compounds that widely exist in nature, are active ingredients of many Chinese herbal medicines, and are an important class of substances in nature. Periwinkle is the whole plant of Catharanthus roseus (L.) G.Don, a plant of the family Apocynaceae, also known as Ririxin, Yanlaihong, etc. In addition, there is a variant of this plant, Catharanthus roseus (L.) G .Donvar.albus (Sweet) G.Don, yellow periwinkle G.roseus (L.) G.Don var.flvus (Tsiang) Metcalr, also equally used as medicine. Periwinkle is a commonly used folk Chinese herbal medicine. It is cool in natu...

Examples

Embodiment 1

[0034] Take 1000g of periwinkle decoction pieces, add water and decoct twice, 10 times the amount each time, decoct for 2 hours, combine the decoction liquid, centrifuge, adjust pH=3, centrifuge, and the supernatant is passed through cation exchange at 4 times the column volume / hour Resin (001×7, hydrogen type, diameter-to-height ratio 1:8), washed with water until the effluent is colorless, then eluted with 15% hydrochloric acid solution, the elution rate is 2 times the column volume / hour, until the alkaloid test is negative (The effluent was added dropwise with 10% silicotungstic acid without precipitation), the eluate was collected, neutralized with sodium hydroxide to neutral, desalted, and the filtrate was concentrated and dried to obtain the total alkaloids of Vinca japonica.

Embodiment 2

[0036] Get periwinkle decoction pieces 1000g, add the acidic water of pH=5 to infiltrate, combine the infiltrate and add water and dilute to 10000ml, centrifuge, adjust pH=1, centrifuge, supernatant passes through cation exchange resin (Doulex 50, sodium type, diameter-to-height ratio 1:5), wash with water until the effluent is colorless, then elute with 5% hydrochloric acid solution, the elution rate is 4 times the column volume / hour, after elution is 2 times the column volume, soak for 5 hours , and then eluted until the alkaloid test was negative (10% silicotungstic acid was added dropwise to the effluent without precipitation), the eluate was collected, neutralized to neutral with calcium hydroxide, desalinated, the filtrate was concentrated and dried to obtain the total organism of periwinkle alkali.

Embodiment 3

[0038] Take 5 kg of periwinkle 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 the supernatant to 2 times the column volume / hour, pass through the upper cation exchange resin (001×10, sodium type, diameter-to-height ratio 1:7), wash with water until the effluent is colorless, and then wash with 1% hydrochloric acid solution (containing 1% sodium chloride) Elution, the elution rate is 5 times the column volume / hour, until the alkaloid test is negative (10% silicotungstic acid is added dropwise to the effluent without precipitation), the eluate is collected, neutralized to neutral with sodium hydroxide, and desalted , the filtrate was concentrated and dried to obtain the total alkaloids of vinca.

technical field

[0001] The invention relates to the extraction and separation of effective components of traditional Chinese medicine, in particular to a method for extracting and separating total alkaloids of periwinkle from traditional Chinese medicine periwinkle extract, which belongs to the field of traditional Chinese medicine. Background technique

[0002] Alkaloids are a large class of basic nitrogen-containing compounds that widely exist in nature, are active ingredients of many Chinese herbal medicines, and are an important class of substances in nature. Periwinkle is the whole plant of Catharanthus roseus (L.) G.Don, a plant of the family Apocynaceae, also known as Ririxin, Yanlaihong, etc. In addition, there is a variant of this plant, Catharanthus roseus (L.) G .Donvar.albus (Sweet) G.Don, yellow periwinkle G.roseus (L.) G.Don var.flvus (Tsiang) Metcalr, also equally used as medicine. Periwinkle is a commonly used folk Chinese herbal medicine. It is cool in natu...

Examples

Embodiment 1

[0034] Take 1000g of periwinkle decoction pieces, add water and decoct twice, 10 times the amount each time, decoct for 2 hours, combine the decoction liquid, centrifuge, adjust pH=3, centrifuge, and the supernatant is passed through cation exchange at 4 times the column volume / hour Resin (001×7, hydrogen type, diameter-to-height ratio 1:8), washed with water until the effluent is colorless, then eluted with 15% hydrochloric acid solution, the elution rate is 2 times the column volume / hour, until the alkaloid test is negative (The effluent was added dropwise with 10% silicotungstic acid without precipitation), the eluate was collected, neutralized with sodium hydroxide to neutral, desalted, and the filtrate was concentrated and dried to obtain the total alkaloids of Vinca japonica.

Embodiment 2

[0036] Get periwinkle decoction pieces 1000g, add the acidic water of pH=5 to infiltrate, combine the infiltrate and add water and dilute to 10000ml, centrifuge, adjust pH=1, centrifuge, supernatant passes through cation exchange resin (Doulex 50, sodium type, diameter-to-height ratio 1:5), wash with water until the effluent is colorless, then elute with 5% hydrochloric acid solution, the elution rate is 4 times the column volume / hour, after elution is 2 times the column volume, soak for 5 hours , and then eluted until the alkaloid test was negative (10% silicotungstic acid was added dropwise to the effluent without precipitation), the eluate was collected, neutralized to neutral with calcium hydroxide, desalinated, the filtrate was concentrated and dried to obtain the total organism of periwinkle alkali.

Embodiment 3

[0038] Take 5 kg of periwinkle 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 the supernatant to 2 times the column volume / hour, pass through the upper cation exchange resin (001×10, sodium type, diameter-to-height ratio 1:7), wash with water until the effluent is colorless, and then wash with 1% hydrochloric acid solution (containing 1% sodium chloride) Elution, the elution rate is 5 times the column volume / hour, until the alkaloid test is negative (10% silicotungstic acid is added dropwise to the effluent without precipitation), the eluate is collected, neutralized to neutral with sodium hydroxide, and desalted , the filtrate was concentrated and dried to obtain the total alkaloids of vinca.