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Method for separating hesperidin, neohesperidin, naringin and synephrine from immature bitter oranges

A technology of neohesperidin and hesperidin, applied in the fields of naringin and synephrine, neohesperidin, and extraction of hesperidin, which can solve the problems of low yield, complicated operation, and high cost

Active Publication Date: 2020-10-20
HUNAN HUACHENG BIOTECH
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  • Abstract
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Problems solved by technology

[0007] CN104230871A discloses a method for separating polymethoxylated flavonoids, hesperidin and synephrine in Fructus Aurantium, specifically using Fructus Fructus Fructus as raw material, through ethanol extraction, resin adsorption, ethanol and ammonia water respectively eluting, concentrating and drying and other steps to obtain the synephrine product with a content of more than 28% and a yield of more than 50% and the hesperidin product with a content of more than 93% and a yield of more than 70%; this method can only obtain synephrine and hesperidin, and the yield The yield is not high, and the purity of the obtained synephrine is very low
[0008] CN105481920A discloses a method for extracting hesperidin, neohesperidin and synephrine. Specifically, aurantium citrus and citrus peel are used as raw materials, extracted by ethanol aqueous solution, enzymatically hydrolyzed with pectinase, and the filter residue is extracted with alkali to adjust acidity. Recrystallize and dry to obtain a hesperidin sample with a content of 98% and a yield of 8.8%; A neohesperidin sample with a yield of more than 5.3%; the filtrate is acid-adjusted and then adsorbed by a macroporous adsorption resin column and a cationic column, eluted with ammonia water, recrystallized, and dried to obtain hesperidin with a content of 98% and a yield of more than 2.1%. Flynn product; this method cannot obtain naringin, requires the use of biological agents, complicated operation, and low yield
[0009] CN106220698A discloses a method for isolating high-purity hesperidin, neohesperidin, naringin and synephrine from Fructus Aurantii, comprising the following steps in turn: (1) enzymatic hydrolysis, (2) extraction, (3) Membrane separation, (4) separation of synephrine, (5) separation of naringin, (6) separation of neohesperidin, (7) separation of hesperidin; this method requires the use of biological agents and more complex Nanofiltration membrane equipment, the cost is high, and the yield of synephrine is less than 90%

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  • Method for separating hesperidin, neohesperidin, naringin and synephrine from immature bitter oranges

Examples

Experimental program
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Embodiment 1

[0044] (1) Heating extraction: take 100 kg of Fructus Aurantii, crush, pass through a 20-mesh sieve, add 3000L of water in 3 times, stir and extract for 1 hour at 85℃ each time, cool, pass through a fine filter membrane, collect the extract and extract separately Slag

[0045] (2) Separation of hesperidin: The extract residue obtained in step (1) was extracted with 1500L sodium hydroxide solution with a concentration of 0.5wt% at 30°C for 1.5h, centrifuged and filtered, the filtrate was adjusted to pH value with hydrochloric acid 2. After standing for crystallization at room temperature, the precipitated crystals are filtered under reduced pressure and vacuum dried to obtain 5.56 kg of hesperidin product with a purity of 99.32wt% and an extraction rate of 98.09%;

[0046] (3) Separation of neohesperidin: pass the extract obtained in step (1) through D101 macroporous adsorption resin, and collect the effluent for later use; the macroporous adsorption resin is desorbed with 2BV ethan...

Embodiment 2

[0050] (1) Heating extraction: take 200kg of Citrus aurantium, crush, pass through a 30-mesh sieve, add 8000L water in 4 times, stir and extract at 90℃ for 1.5h each time, cool, pass through a fine filter membrane, collect the extract and Extract residue

[0051] (2) Separation of hesperidin: the extract residue obtained in step (1) was extracted with a 4000L potassium hydroxide solution with a concentration of 1.0 wt% at 35°C for 2.5 hours, centrifuged and filtered, and the filtrate was adjusted to pH value with hydrochloric acid 4. After standing for crystallization at room temperature, the precipitated crystals are filtered under reduced pressure and vacuum dried to obtain 11.17kg of hesperidin product with a purity of 99.08wt% and an extraction rate of 98.29%;

[0052] (3) Separation of new hesperidin: pass the extract obtained in step (1) through D101 macroporous adsorption resin, and collect the effluent for later use; the macroporous adsorption resin is desorbed with 2.5BV o...

Embodiment 3

[0056] (1) Heating extraction: Take 300kg of Fructus Aurantii, crush, pass through 40 mesh sieve, add 12000L of water in 4 times, stir and extract 2h each time at 92℃, cool, pass through fine filter membrane, collect extract and extract separately Slag

[0057] (2) Separation of hesperidin: The extract residue obtained in step (1) was stirred and extracted with 7500L saturated lime aqueous solution at 45°C for 4h, centrifuged and filtered, the filtrate was adjusted to pH 6 with hydrochloric acid, and then left to stand at room temperature for crystallization , The precipitated crystals were filtered under reduced pressure and vacuum dried to obtain 16.52 kg of hesperidin product with a purity of 99.54wt% and an extraction rate of 97.36%;

[0058] (3) Separation of neohesperidin: pass the extract obtained in step (1) through D101 macroporous adsorption resin, and collect the effluent for use; the macroporous adsorption resin is desorbed with 3BV 75% ethanol by volume to obtain desor...

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Abstract

The invention discloses a method for separating hesperidin, neohesperidin, naringin and synephrine from immature bitter oranges. The method comprises the following steps: (1) heating and leaching; (2)separation of hesperidin; (3) separation of neohesperidin; (4) separation of naringin; and (5) separation of synephrine. The four products obtained by the method disclosed by the invention have highpurity and extraction rate. The content of the hesperidin is up to 99.54% at most, and the extraction rate is 98.29%; the content of the neohesperidin is up to 99.68% at most, and the extraction rateis 97.98%; the content of the naringin is up to 97.17% at most, and the extraction rate is 95.91%; and the content of the synephrine is up to 92.33% at most, and the extraction rate is 97.26%. On thepremise of guaranteeing the extraction rate and the product content, the method achieves comprehensive utilization of the immature bitter oranges, and increases the additional value of the immature bitter oranges; and the method is simple and feasible in process operation, the adopted solvent is low in cost, non-toxic and harmless, and the method has low requirement for production equipment and issuitable for industrial production.

Description

Technical field [0001] The present invention relates to a method for extracting active ingredients from Fructus Aurantii, in particular to a method for extracting hesperidin, neohesperidin, naringin and synephrine from Fructus Aurantii. Background technique [0002] Citrus aurantium is the dried young fruit of the rutaceae plant Citrus aurantium L. and its cultivars or sweet orange (Citrussinensis Osbeck). It is spherical or hemispherical, with hard texture, delicate smell, sour and slightly bitter. From Sichuan, Hunan, Hubei, Jiangxi and other places, it has the effects of dispelling qi and accumulating, resolving phlegm and dispelling pimple. Its main active ingredients include flavonoids (hesperidin, neohesperidin, naringin, etc.) and biological Alkali (synephrine, N-methyltyramine, etc.). [0003] Hesperidin has the structure of dihydroflavonoid oxygen glycosides, which plays an important role in maintaining osmotic pressure, enhancing capillary toughness, shortening bleeding ...

Claims

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Application Information

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IPC IPC(8): C07H1/08C07H17/07C07H15/203C07C213/10C07C215/60
CPCC07C213/10C07H1/08C07H15/203C07H17/07C07C215/60
Inventor 魏来李伟黄华学
Owner HUNAN HUACHENG BIOTECH
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