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Method for preparing naringin or hesperidin

A technology for hesperidin and naringin, which is applied in the field of preparation of naringin or hesperidin, can solve the problem of large solvent consumption, large and long loss in the operation process, reflux time of several hours to ten hours, and immersion The extraction time is at least half an hour, and it can take more than ten hours to achieve the effect of simple post-processing concentration, remarkable advancement, and simple purification.

Inactive Publication Date: 2010-05-12
THIRD INST OF OCEANOGRAPHY STATE OCEANIC ADMINISTATION
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  • Abstract
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Problems solved by technology

The solid-liquid ratio of organic solvent reflux or leaching at normal pressure is generally 1:10-20, the solvent consumption is large, the concentration and recovery process is large, the operation process loss is also large, and it takes a long time, and the reflux time is several hours to more than ten Hours, the extraction time is at least half an hour, and the longest is more than ten hours

Method used

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  • Method for preparing naringin or hesperidin

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preparation example Construction

[0018] A kind of preparation method of naringin or hesperidin of the present invention, such as figure 1 As shown, the fruits or peels and pomace containing naringin or hesperidin are dried, pulverized, and sieved respectively, and the crushed and sieved extraction materials 3 are respectively loaded into a high-pressure extraction machine with a heating jacket 1. In the still 2; set the extraction pressure and extraction temperature, the heating jacket 1 starts to heat up, open the check valve 4, and use the high-pressure solvent pump 5 to pump the extraction solvent in the solvent tank 6 into the high-pressure extraction still 2. Open the electric valve 7 below the high-pressure extraction kettle 2, and collect the extract in the extract collection bottle 8. At the end of the extraction, open the electric valve 10 above the nitrogen bottle 9, and use the nitrogen in the nitrogen bottle 9 to blow out all the extract in the high-pressure extraction kettle 2 into the extract co...

Embodiment 1

[0021] Put 4.5 grams of pulverized pomelo peel powder into the extraction kettle, set the extraction pressure to 50 bar, the extraction temperature to 60°C, statically extract with absolute ethanol for 10 minutes, and extract continuously for 5 times. Combine the extracts, concentrate the extracts to one-fifth of the original volume in a vacuum concentrator, filter the insoluble matter with filter paper, adjust the pH of the filtered clear liquid to about 5 with acetic acid, cool and crystallize in a refrigerator, and filter the crystals to obtain Crude naringin. The crude naringin is recrystallized twice with 95% ethanol to obtain naringin with a purity greater than 91%.

Embodiment 2

[0023] Put 6 grams of pulverized pomelo peel powder into the extraction kettle, set the extraction pressure to 50 bar, the extraction temperature to 75° C., statically extract with 95% ethanol aqueous solution for 10 minutes, and extract continuously for 3 times. Combine the extracts, concentrate the extracts to one-fifth of the original volume in a decompression concentrator, remove insolubles by filtering through a 0.45 μ filter membrane, adjust the pH of the filtered clear liquid to about 5 with 10% hydrochloric acid solution, and place Cool and crystallize in the refrigerator, and filter the crystals to obtain crude naringin. Crude naringin is finely ground, washed with ethyl acetate until colorless, and recrystallized twice with 95% ethanol to obtain naringin with a purity greater than 93%.

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Abstract

The invention relates to a method for preparing naringin or hesperidin, which comprises the following operating steps of: 1) drying and crushing fruits, fruit peels and fruit residues containing the naringin or the hesperidin, and respectively filling the crushed materials into an extraction kettle of a pressure solvent extraction device; 2) selecting an extraction solvent, setting an extraction pressure, an extraction temperature, an extraction static time and an extraction frequency, extracting with the pressure solvent extraction device, and collecting the extract liquor; and 3) concentrating the extract liquor in vacuum, centrifugating the extract liquor or filtering the extract liquor to remove insoluble substances, adjusting pH of the clear liquid, cooling the clear liquid to crystallize or precipitate, recrystallizing the coarse crystals, drying the coarse crystals, or re-dissolving the precipitate for re-precipitation, and obtaining a pure product of the naringin or the hesperidin. Compared with the conventional solvent extraction method, ultrasonic-assisted extraction method and microwave-assisted extraction method, the preparation method has the advantages of high speed, capability of repeatedly extracting, safety, high efficiency, and simple post treatment such as concentration and purification.

Description

technical field [0001] The invention relates to a method for preparing naringin or hesperidin, in particular to a method for extracting and preparing naringin or hesperidin from fruits of Rutaceae plants by using a pressure solvent extraction technique. Background technique [0002] Naringin (naringin) (C 27 h 32 o 14 ·8H 20 ), mainly exist in pomelo (CitruSgrandis), grapefruit (CitruSradisi), huyou, lime (CitruSaurantium), citrus aurantium, citrus aurantium, tangerine and the peels and fruits of these plant varieties, hesperidin (hesperidin) (C 28 h 34 o 15 ), mainly found in the peels and fruits of trifoliate oranges, oranges, tangerines, oranges, citrons, lemons and these plant varieties. In the food industry, naringin can be used as a natural pigment, flavor improver and bittering agent. Both naringin and hesperidin can be used as a new sweetener dihydrochalcone with high sweetness, non-toxicity and low energy. raw materials. In the pharmaceutical industry, narin...

Claims

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Application Information

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IPC IPC(8): C07H17/07C07H1/08
CPCY02P20/544Y02P20/54
Inventor 许晨许建中唐旭沈国林晓峰宁方刚
Owner THIRD INST OF OCEANOGRAPHY STATE OCEANIC ADMINISTATION
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