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Extraction method and use method of naringin

An extraction method and naringin technology are applied in the application and preparation field of naringin, which can solve the problems of low target substance content, complicated operation and high cost, and achieve the effects of high degreasing efficiency, simple operation and low cost.

Active Publication Date: 2015-08-05
CHINA TOBACCO HUNAN INDAL CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The extraction method is complex in operation, long in cycle and high in cost, and the key is column chromatographic separation
Although water extraction has advantages, it is cumbersome to concentrate it into an extract, because the extract has poor fluidity and viscosity, and when the material is transferred, it will adhere to the container wall and column chromatography is difficult. It is difficult to control the moisture in the extract. The water content has an important impact on the subsequent solvent elution and separation effect, and affects the stability of the subsequent column chromatography separation process; the extract is first precipitated with alcohol to obtain a crude product and then column chromatography separation can alleviate this problem to a certain extent, but Bringing an increase in the alcohol precipitation process and the subsequent process of evaporation and recovery of ethanol
The separation process of column chromatography is complicated, the solvent elution time is long, the consumption of organic solvent is high, and there are many factors affected; in order to obtain a better separation effect, the content of the target substance in the eluent is extremely low, and finally a large amount of organic solvent needs to be concentrated and evaporated to recover , so the costly
And even if the column chromatography separation process is adopted, the patent still needs to take further multiple ethanol recrystallizations to achieve the ideal purification effect
[0005] The key technology in CN1431216A is to put the initial product extract on the chromatographic column, and the separation of the chromatographic column has a good effect, making subsequent recrystallization and purification possible; but the column chromatographic separation process is complicated, the solvent elution time is long, and the organic solvent consumption is high. There are many factors affecting the process; in order to achieve a better separation effect, the content of the target substance in the eluent is extremely low, and finally a large amount of organic solvent needs to be concentrated and evaporated to recover, so the cost is high
And even if the column chromatography separation process is adopted, the patent still needs to take further multiple ethanol recrystallizations to achieve the ideal purification effect

Method used

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  • Extraction method and use method of naringin
  • Extraction method and use method of naringin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] ① Wash the white spongy mesocarp obtained after peeling off the yellow exocarp of the mature fresh pomelo peel, dry, crush and sieve to 30 mesh;

[0030] ② Reflux degreasing with petroleum ether, filter, and dry the filter residue at 40°C;

[0031] ③Add 60% ethanol to the filter residue, the volume of the added ethanol is 15 times of the quality of the degreased pomelo peel filter residue, heat and stir at 60°C, and reflux for 1.5h;

[0032] ④ suction filtration, collecting the filtrate, concentrating the filtrate under reduced pressure to 1 / 3 of the original volume of the filtrate, to obtain crude naringin;

[0033] ⑤ Add a small amount of water to the crude naringin, dissolve it at 60°C, cool it at 4°C for 24 hours, remove the supernatant, filter and collect the precipitate;

[0034] ⑥Under the same conditions, repeated recrystallization twice to obtain naringin, the purity of naringin was 81.2%. Experimentally measured the prepared naringin 1 See attached for HNMR...

Embodiment 2

[0036] ① Wash the white spongy mesocarp obtained after peeling off the yellow exocarp of mature fresh pomelo peel, dry, crush and sieve to 30 mesh;

[0037] ② Reflux degreasing with petroleum ether, filter, and dry the filter residue at 40°C;

[0038]③Add 70% ethanol to the filter residue, the volume of the added ethanol is 20 times of the quality of the degreased pomelo peel filter residue, heat and stir at 60°C, and reflux for 2h;

[0039] ④ suction filtration, collecting the filtrate, concentrating the filtrate under reduced pressure to 1 / 3 of the original volume of the filtrate, to obtain crude naringin;

[0040] ⑤ Add a small amount of water to the crude naringin, dissolve it at 60°C, cool it at 4°C for 24 hours, remove the supernatant, filter and collect the precipitate;

[0041] ⑥Under the same conditions, repeated recrystallization twice to obtain naringin, the purity of naringin was 83.7%.

Embodiment 3

[0043] ① Wash the white spongy mesocarp obtained after peeling off the yellow exocarp of the mature fresh pomelo peel, dry, crush and sieve to 30 mesh;

[0044] ② Reflux degreasing with petroleum ether, filter, and dry the filter residue at 40°C;

[0045] ③Add 80% ethanol to the filter residue, the volume of the added ethanol is 25 times of the quality of the degreased pomelo peel filter residue, heat and stir at 60°C, and reflux for 2.5h;

[0046] ④ suction filtration, collecting the filtrate, concentrating the filtrate under reduced pressure to 1 / 3 of the original volume of the filtrate, to obtain crude naringin;

[0047] ⑤ Add a small amount of water to the crude naringin, dissolve it at 60°C, cool it at 4°C for 24 hours, remove the supernatant, filter and collect the precipitate;

[0048] ⑥Under the same conditions, repeat the recrystallization twice to obtain naringin, the purity of naringin is 85.6%.

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Abstract

The invention discloses an extraction method and a use method of naringin. The extraction method comprises stripping yellow outer pericarp of shaddock peel as a raw material to obtain white spongy shaddock peel, carrying out crushing and sieving to obtain shaddock peel powder, carrying out degreasing by an alkane solvent such as petroleum ether with weak polarity, carrying out filtration, drying the filter residue, adding ethanol into the filter residue, carrying out reflux extraction, carrying out pumping filtration, collecting the filtrate, carrying out reduced pressure condensation and carrying out recrystallization to obtain naringin. The extraction method has simple processes and a low cost. The naringin added into cigarette cut tobacco so that cigarette fragrant characteristics are improved and cigarette sensory quality is improved.

Description

【Technical field】 [0001] The invention relates to the field of application and preparation of naringin, in particular to a method for extracting naringin and its application method in cigarettes. 【Background technique】 [0002] Grapefruit is the ripe fruit of pomelo, a Rutaceae plant. Grapefruit is fragrant, sweet and sour, cool, rich in nutrition, and has high medicinal value. It is one of the fruits that people like to eat, and it is also recognized by the medical field as the most therapeutic fruit. Pomelo peel is rich in a large amount of naringin, for example, more than 50% of naringin in grapefruit is distributed in the peel. Naringin is a dihydroflavonoid compound with various biological activities, such as anti-oxidation, anti-mutation, anti-tumor, antibacterial, improving microcirculation, reducing the fragility of capillaries, etc. It is widely used in the fields of medicine, food and cosmetics Has a wide range of applications. [0003] The patent document of pub...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/07C07H1/08A24B15/40
CPCA24B15/403C07H1/08C07H17/07
Inventor 杨华武黎艳玲尹双凤吕浩铭
Owner CHINA TOBACCO HUNAN INDAL CORP
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