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Extracting and purifying method of queretagetin

A purification method, tagetin technology, applied in the direction of organic chemistry, can solve the problems of large amount of solvent, long cycle, low yield, etc., and achieve the effect of shortening the extraction time, short time, and large amount of preparation

Inactive Publication Date: 2015-01-07
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As mentioned above, existing methods for purifying tagetes have shortcomings such as low yield, long period, large amount of solvent, and low yield.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Crush chamomile through a 20-mesh sieve, weigh 3kg, add 24g of pectinase, mix evenly, enzymatically hydrolyze for 2 days, add 24L of 70% ethanol solution to the raw material for enzymatic hydrolysis and suspend for 50min, and carry out negative pressure cavitation for suspension Liquid extraction once to obtain the extract, concentrated, added to a polyamide resin column, the impurities were first eluted with 4BV of 20% ethanol, and then the active ingredients were eluted with 6BV of 75% ethanol. The collected active ingredients were concentrated under reduced pressure and dried to obtain a crude product. Mix n-hexane, ethyl acetate, methanol, and water in a volume ratio of 4:2.5:2.5:2. After layering, take the upper phase as the stationary phase and the lower phase as the mobile phase. Adjust the rotation speed to 850rpm. Control the flow rate at 2ml / min, remove the phase to dissolve the crude product, and inject the sample through the injection valve. The ultraviolet d...

Embodiment 2

[0018] Crush chamomile through a 20-mesh sieve, weigh 3kg, add 18g of amylase and mix evenly, enzymatically hydrolyze for 1 day, add 30L of 75% ethanol solution to the enzymolyzed material and suspend for 45min, and carry out negative pressure cavitation to suspend the solid-liquid Extracted twice to obtain the extract, concentrated, added to a polyamide resin column, first eluted impurities with 3BV 30% ethanol, then eluted active ingredients with 5BV 75% ethanol, collected active ingredients concentrated under reduced pressure, and dried to obtain a crude product. Mix n-hexane, ethyl acetate, methanol, and water in a volume ratio of 5:3:3:5. After layering, take the upper phase as the stationary phase and the lower phase as the mobile phase. Adjust the rotation speed to 800rpm. Pump the lower phase Control the flow rate at 2ml / min, remove the phase to dissolve the crude product, and inject the sample through the injection valve. The ultraviolet detection wavelength is 254nm, ...

Embodiment 3

[0020] Crush chamomile through a 20-mesh sieve, weigh 3kg, add 24g of cellulase, mix evenly, enzymatically hydrolyze for 2 days, add 15L of 80% ethanol solution to the enzymatic hydrolyzed raw material and suspend for 50min, and carry out negative pressure cavitation for suspension Liquid extraction twice to obtain the extract, concentrated, added to a polyamide resin column, the impurities were first eluted with 4BV of 35% ethanol, and then the active ingredients were eluted with 5BV of 80% ethanol, the collected active ingredients were concentrated under reduced pressure and dried to obtain a crude product. Mix n-hexane, ethyl acetate, methanol, and water in a volume ratio of 6:1:1:4. After layering, take the upper phase as the stationary phase, and the lower phase as the mobile phase. Adjust the speed to 950rpm. Pump the lower phase Control the flow rate at 3ml / min, remove the phase to dissolve the crude product, inject the sample through the injection valve, and detect the ...

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Abstract

The invention discloses an extracting and purifying method of queretagetin. The extracting and purifying method comprises the following steps: crushing matricaria recutita, adding biological enzyme to perform enzymolysis to obtain an enzymolysis raw material; after adding a 65-80% alcohol liquid which is 5-10 times the amount of the enzymolysis raw material to mix with the enzymolysis raw material, performing negative-pressure cavitation, suspension and solid-liquid extraction to obtain an extracting liquid; concentrating the extracting liquid, adsorbing by a polyamide resin column, performing alcohol-water elution, collecting eluant, concentrating and drying the eluant to obtain a crude product; separating and purifying the crude product by high-speed counter-current chromatography, taking n-hexane-ethyl acetate-methanol-water as a solvent system, detecting the crude product by an ultraviolet detector, collecting a fraction and recycling reagents, and drying the collected fraction and the recycled reagents to obtain queretagetin. The extracting and purifying method of the queretagetin disclosed by the invention is simple to operate and high in efficiency; and moreover, the queretagetin is high in product purity and suitable for industrial preparation.

Description

technical field [0001] The invention belongs to the technical field of extracting natural substances, and relates to a method for extracting and purifying tagetes. Background technique [0002] Chamomile is mainly produced in my country Xinjiang north and west. Born in the valley wilderness, field edge. Beijing with Shanghai The garden is cultivated for viewing. Europe , Asia There are also distributions in the north and west. Matricariae tastes slightly bitter, sweet and fragrant, improves eyesight, relieves liver fire, treats insomnia, lowers blood pressure, can enhance vitality and refresh oneself; enhances memory, lowers blood pressure. cholesterol ;Expelling phlegm and relieving cough, can effectively relieve bronchitis and asthma, relieve headaches, migraines or muscular pain caused by colds, neutralize stomach acid , Soothing nerves is helpful; it can eliminate muscle soreness caused by colds, calm the spirit, relieve emotions, improve sleep quality, an...

Claims

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Application Information

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IPC IPC(8): C07D311/30C07D311/40
CPCC07D311/30C07D311/40
Inventor 刘东锋杨成东
Owner NANJING ZELANG MEDICAL TECH
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