Simulated moving-bed chromatographic process for separating and purifying flavone from Chinese yam

Abstract

The present invention discloses simulated moving bed chromatographic process for separating and purifying flavone from Chinese yam. The process includes the following steps: ultrasonically extracting flavone from Chinese yam in alcohol solution; adding hexane into alcohol solution for normal temperature liquid-liquid extraction, filtering and vacuum distilling to obtain coarse Chinese yam flavone extract; purifying the coarse Chinese yam flavone extract in a simulated moving bed; filtering with organic film; eluting with methane-water mixture; dissolving the extracted liquid in alcohol, adding water and cooling to the temperature of -5 deg.c to-12 deg.c to crystallize; filtering, water washing the crystal; stoving to obtain purified Chinese yam flavone product. The present invention has continuous production, high production efficiency and environment friendship.

Description

technical field

[0001] The invention relates to a method for separating and purifying natural medicines, in particular to a method for separating and purifying flavonoids from yam by simulated moving bed chromatography. Background technique

[0002] Yam medicine is a perennial winding herbaceous vine of Dioscoreaceae. Modern medical research shows that yam medicine contains flavonoids, saponins, mucus, choline, starch, sugar, protein, tannin, various amino acids, vitamin C, etc. Its internal components are relatively complex. The current method of extracting yam flavonoids is to soak, filter, and extract to obtain crude products, but to meet the medicinal requirements, it must be further purified. Currently, the commonly used purification method is column chromatography with neutral alumina as a filler. Law. Column chromatography is a commonly used refining method in the pharmaceutical and food industries. The equipment is simple and low in cost. However, although this meth...

Examples

example 1

[0013] Example 1: Separation and purification of Chinese yam flavonoids on a simulated moving bed of Jiangsu Hanbang Technology Co., Ltd. according to the following steps:

[0014] a, get 10kg of 88% ethanol and ultrasonically extract 0.5kg to get the flavonoids in Chinese yam;

[0015] b. Add hexane according to the volume ratio of ethanol and hexane as 4:6, carry out liquid-liquid extraction at room temperature for 3 hours, filter, and evaporate the filtrate to dryness under reduced pressure to obtain the crude extract of Chinese yam flavonoids;

[0016] c. The crude extract of yam flavonoids is made into a feed solution and purified in a simulated moving bed; the crude extract of yam flavonoids is dissolved in methanol, and filtered through a 0.45 μm organic pump filter membrane to obtain a simulated moving bed feed solution with a concentration of 100 mg / ml; The eluent is a mixture of methanol and water, the volume ratio of methanol and water is 4:6;

[0017] d. Dissolve ...

example 2

[0021] Example 2: Separation and purification of Chinese yam flavonoids on a simulated moving bed of Jiangsu Hanbang Technology Co., Ltd. according to the following steps:

[0022] a. Get 17kg of 88% ethanol and ultrasonically extract the flavonoids in 0.8kg of Chinese yam;

[0023] b. Add hexane according to the volume ratio of ethanol and hexane as 4:6, carry out liquid-liquid extraction at room temperature for 4 hours, filter, and evaporate the filtrate to dryness under reduced pressure to obtain the crude extract of Chinese yam flavonoids;

[0024] c. The crude extract of yam flavonoids is made into a feed solution and purified in a simulated moving bed; the crude extract of yam flavonoids is dissolved in methanol, and filtered through a 0.45 μm organic pump membrane to obtain a simulated moving bed feed solution with a concentration of 200 mg / ml; The eluent is a mixture of methanol and water, the volume ratio of methanol and water is 4:6;

[0025] d. Dissolve the extract...

example 3

[0029] Example 3: Separation and purification of Chinese yam flavonoids on a simulated moving bed of Jiangsu Hanbang Technology Co., Ltd. according to the following steps:

[0030] a. Get 24kg of 88% ethanol and ultrasonically extract the flavonoids in 1.2kg of Chinese yam;

[0031] b. Add hexane according to the volume ratio of ethanol and hexane as 4:6, carry out liquid-liquid extraction at room temperature for 5 hours, filter, and evaporate the filtrate to dryness under reduced pressure to obtain the crude extract of Chinese yam flavonoids;

[0032] c. The crude extract of yam flavonoids is made into a feed solution and purified in a simulated moving bed; the crude extract of yam flavonoids is dissolved in methanol, and filtered through a 0.45 μm organic pump membrane to obtain a simulated moving bed feed solution with a concentration of 300 mg / ml; The eluent is a mixture of methanol and water, the volume ratio of methanol and water is 4:6;

[0033] d. Dissolve the extract...

technical field

[0001] The invention relates to a method for separating and purifying natural medicines, in particular to a method for separating and purifying flavonoids from yam by simulated moving bed chromatography. Background technique

[0002] Yam medicine is a perennial winding herbaceous vine of Dioscoreaceae. Modern medical research shows that yam medicine contains flavonoids, saponins, mucus, choline, starch, sugar, protein, tannin, various amino acids, vitamin C, etc. Its internal components are relatively complex. The current method of extracting yam flavonoids is to soak, filter, and extract to obtain crude products, but to meet the medicinal requirements, it must be further purified. Currently, the commonly used purification method is column chromatography with neutral alumina as a filler. Law. Column chromatography is a commonly used refining method in the pharmaceutical and food industries. The equipment is simple and low in cost. However, although this meth...

Examples

example 1

[0013] Example 1: Separation and purification of Chinese yam flavonoids on a simulated moving bed of Jiangsu Hanbang Technology Co., Ltd. according to the following steps:

[0014] a, get 10kg of 88% ethanol and ultrasonically extract 0.5kg to get the flavonoids in Chinese yam;

[0015] b. Add hexane according to the volume ratio of ethanol and hexane as 4:6, carry out liquid-liquid extraction at room temperature for 3 hours, filter, and evaporate the filtrate to dryness under reduced pressure to obtain the crude extract of Chinese yam flavonoids;

[0016] c. The crude extract of yam flavonoids is made into a feed solution and purified in a simulated moving bed; the crude extract of yam flavonoids is dissolved in methanol, and filtered through a 0.45 μm organic pump filter membrane to obtain a simulated moving bed feed solution with a concentration of 100 mg / ml; The eluent is a mixture of methanol and water, the volume ratio of methanol and water is 4:6;

[0017] d. Dissolve ...

example 2

[0021] Example 2: Separation and purification of Chinese yam flavonoids on a simulated moving bed of Jiangsu Hanbang Technology Co., Ltd. according to the following steps:

[0022] a. Get 17kg of 88% ethanol and ultrasonically extract the flavonoids in 0.8kg of Chinese yam;

[0023] b. Add hexane according to the volume ratio of ethanol and hexane as 4:6, carry out liquid-liquid extraction at room temperature for 4 hours, filter, and evaporate the filtrate to dryness under reduced pressure to obtain the crude extract of Chinese yam flavonoids;

[0024] c. The crude extract of yam flavonoids is made into a feed solution and purified in a simulated moving bed; the crude extract of yam flavonoids is dissolved in methanol, and filtered through a 0.45 μm organic pump membrane to obtain a simulated moving bed feed solution with a concentration of 200 mg / ml; The eluent is a mixture of methanol and water, the volume ratio of methanol and water is 4:6;

[0025] d. Dissolve the extract...

example 3

[0029] Example 3: Separation and purification of Chinese yam flavonoids on a simulated moving bed of Jiangsu Hanbang Technology Co., Ltd. according to the following steps:

[0030] a. Get 24kg of 88% ethanol and ultrasonically extract the flavonoids in 1.2kg of Chinese yam;

[0031] b. Add hexane according to the volume ratio of ethanol and hexane as 4:6, carry out liquid-liquid extraction at room temperature for 5 hours, filter, and evaporate the filtrate to dryness under reduced pressure to obtain the crude extract of Chinese yam flavonoids;

[0032] c. The crude extract of yam flavonoids is made into a feed solution and purified in a simulated moving bed; the crude extract of yam flavonoids is dissolved in methanol, and filtered through a 0.45 μm organic pump membrane to obtain a simulated moving bed feed solution with a concentration of 300 mg / ml; The eluent is a mixture of methanol and water, the volume ratio of methanol and water is 4:6;

[0033] d. Dissolve the extract...