CN101704868B - Method for preparing naringin - Google Patents
Method for preparing naringin Download PDFInfo
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- CN101704868B CN101704868B CN2009102328024A CN200910232802A CN101704868B CN 101704868 B CN101704868 B CN 101704868B CN 2009102328024 A CN2009102328024 A CN 2009102328024A CN 200910232802 A CN200910232802 A CN 200910232802A CN 101704868 B CN101704868 B CN 101704868B
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Abstract
The invention relates to a method for preparing naringin, which is simple in operation, light in pollution and low in equipment investment, and comprises the following process steps of: taking coarse powder of pummelo peel, adding water of which the volume is 8 to 12 times the weight of the coarse powder of pummelo peel into the coarse powder, soaking at the temperature of between 30 and 80 DEG C for 8 to 24h, performing filter pressing, taking filtrate, adding CaCl3 into the filtrate, uniformly stirring the filtrate added with CaCl3, standing the mixture overnight, filtering, taking the filtrate, adding strong ammonia water into the filtrate to adjust the pH to between 7 and 8, adsorbing the filtrate added with strong ammonia water with a macroporous adsorption resin column, eluting with water to remove impurities, eluting with 50 to 90 percent ethanol, collecting the eluate of which the volume is 3 to 8 times that of the column, reclaiming the ethanol at reduced pressure, concentrating the eluate, and refrigerating the eluate to separate out crystal. The naringin prepared by the method is high in purity and easy to realize industrial enlargement.
Description
Technical field
The present invention relates to a kind of preparation method of naringin, especially a kind of method of from plant, extracting naringin.
Background technology
Naringin (Naringin), different name: naringin, naringin etc., molecular formula: C27H32O14, molecular weight: 580.541, CAS accession number: 10236-47-2, structural formula is following:
Naringin is a kind of natural compounds, has anti-inflammatory, antitumor, the anti-ageing multiple physiologically active of waiting for a long time, and extensively is present in the Rutaceae various plants.
Pummelo Peel is prematurity or the outer pericarp of maturescent drying of rutaceae Huazhou shaddock Citrus grandis Tomentosa or shaddock Citrus grandis (L.) Osbeck.Having looses trembles with fear eliminating dampness, sharp gas, effects such as dissolving phlegm.Wherein contain a large amount of naringins.
In the prior art, the extraction separation of naringin mainly adopts organic solvent method etc., but the content of the naringin that these extraction processes obtain is low, and is seriously polluted in the production process, and unfavorable big production operation.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method who is beneficial to big production operation, naringin that product purity is high.
For solving the problems of the technologies described above, the present invention adopts following technical proposal:
Get the Pummelo Peel meal, add the water that its weight 8-12 doubly measures volume, 30-80 ℃ of temperature soaked 8-24 hour, and filtrating is got in press filtration, added CaCl
2, stirring, placement is spent the night, and filters; Get filtrating, add strong aqua and regulate pH7-8, through macroporous adsorptive resins absorption, water elution removal of impurities; The 50-90% ethanol elution is collected the elutriant that 3-8 doubly measures column volume, and decompression recycling ethanol also concentrates refrigeration; Separate out crystallization, fractional crystallization adds the absolute ethyl alcohol recrystallization, separates, washs, is drying to obtain.
The condition optimization that temperature is soaked is: add the water of 10 times of amounts of medicinal material weight volume, 60 ℃ of temperature were soaked 12 hours.
The model of macroporous adsorbent resin is one or more among AB-8, H-103, D-101, DA-201, the DS-401.
The alcohol concn of wash-out macroporous adsorptive resins is preferably 75%.
The amount of collecting the macroporous adsorptive resins elutriant is preferably 5 times of amount column volumes.
Adopt technique scheme to prepare naringin, easy and simple to handle, pollute less, equipment drops into for a short time, is beneficial to big production operation.
To combine embodiment that the present invention is done further elaboration below, but the scope that the present invention requires to protect is not limited to following embodiment.
Embodiment
Embodiment 1
Get Pummelo Peel meal 10Kg, add the water of 8 times of amounts of its weight volume, 30 ℃ of temperature were soaked 8 hours, and filtrating is got in press filtration, adds CaCl
2, stirring, placement is spent the night, and filters, and gets filtrating; Add strong aqua and regulate pH7-8, through macroporous adsorptive resins absorption, the water elution removal of impurities, 50% ethanol elution is collected 3 times of elutriants of measuring column volumes; Decompression recycling ethanol also concentrates, and refrigeration is separated out crystallization, fractional crystallization; Add the absolute ethyl alcohol recrystallization, separate, wash, be drying to obtain naringin 88.2g, detect through HPLC, purity is 98.2%.
Embodiment 2
Get Pummelo Peel meal 10Kg, add the water of 12 times of amounts of its weight volume, 80 ℃ of temperature were soaked 24 hours, and filtrating is got in press filtration, adds CaCl
2, stirring, placement is spent the night, and filters, and gets filtrating; Add strong aqua and regulate pH7-8, through macroporous adsorptive resins absorption, the water elution removal of impurities, 90% ethanol elution is collected 8 times of elutriants of measuring column volumes; Decompression recycling ethanol also concentrates, and refrigeration is separated out crystallization, fractional crystallization; Add the absolute ethyl alcohol recrystallization, separate, wash, be drying to obtain naringin 103.9g, detect through HPLC, purity is 98.1%.
Embodiment 3
Get Pummelo Peel meal 10Kg, add the water of 10 times of amounts of its weight volume, 60 ℃ of temperature were soaked 12 hours, and filtrating is got in press filtration, adds CaCl
2, stirring, placement is spent the night, and filters, and gets filtrating; Add strong aqua and regulate pH7-8, through the absorption of D101 macroporous adsorptive resins, the water elution removal of impurities, 75% ethanol elution is collected 5 times of elutriants of measuring column volumes; Decompression recycling ethanol also concentrates, and refrigeration is separated out crystallization, fractional crystallization; Add the absolute ethyl alcohol recrystallization, separate, wash, be drying to obtain naringin 118.9g, detect through HPLC, purity is 99.2%.
Embodiment 4
Get Pummelo Peel meal 10Kg, add the water of 10 times of amounts of its weight volume, 60 ℃ of temperature were soaked 12 hours, and filtrating is got in press filtration, adds CaCl
2, stirring, placement is spent the night, and filters, and gets filtrating; Add strong aqua and regulate pH7-8, through the absorption of DA-201 macroporous adsorptive resins, the water elution removal of impurities, 75% ethanol elution is collected 5 times of elutriants of measuring column volumes; Decompression recycling ethanol also concentrates, and refrigeration is separated out crystallization, fractional crystallization; Add the absolute ethyl alcohol recrystallization, separate, wash, be drying to obtain naringin 101.2g, detect through HPLC, purity is 99.0%.
Embodiment 5
Get Pummelo Peel meal 10Kg, add the water of 10 times of amounts of its weight volume, 60 ℃ of temperature were soaked 12 hours, and filtrating is got in press filtration, adds CaCl
2, stirring, placement is spent the night, and filters, and gets filtrating; Add strong aqua and regulate pH7-8, through the absorption of DS-401 macroporous adsorptive resins, the water elution removal of impurities, 75% ethanol elution is collected 5 times of elutriants of measuring column volumes; Decompression recycling ethanol also concentrates, and refrigeration is separated out crystallization, fractional crystallization; Add the absolute ethyl alcohol recrystallization, separate, wash, be drying to obtain naringin 103.7g, detect through HPLC, purity is 98.7%.
Claims (5)
1. the preparation method of a naringin is characterized in that described method comprises the following steps: to get the Pummelo Peel meal, adds the water that its weight 8-12 doubly measures volume, and 30-80 ℃ of temperature soaked 8-24 hour, and filtrating is got in press filtration, adds CaCl
2, stirring, placement is spent the night, and filters; Get filtrating, add strong aqua and regulate pH7-8, through macroporous adsorptive resins absorption, water elution removal of impurities; The 50-90% ethanol elution is collected the elutriant that 3-8 doubly measures column volume, and decompression recycling ethanol also concentrates refrigeration; Separate out crystallization, fractional crystallization adds the absolute ethyl alcohol recrystallization, separates, washs, is drying to obtain.
2. according to the preparation method of the said naringin of claim 1, it is characterized in that the condition that said temperature is soaked is: add the water of 10 times of amounts of medicinal material weight volume, 60 ℃ of temperature were soaked 12 hours.
3. according to the preparation method of the said naringin of claim 1, the model that it is characterized in that said macroporous adsorbent resin is one or more among AB-8, H-103, D-101, DA-201, the DS-401.
4. according to the preparation method of the said naringin of claim 1, the alcohol concn that it is characterized in that said wash-out macroporous adsorptive resins is 75%.
5. according to the preparation method of the said naringin of claim 1, the amount that it is characterized in that said collection macroporous adsorptive resins elutriant is 5 times of amount column volumes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102328024A CN101704868B (en) | 2009-10-20 | 2009-10-20 | Method for preparing naringin |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009102328024A CN101704868B (en) | 2009-10-20 | 2009-10-20 | Method for preparing naringin |
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| CN101704868A CN101704868A (en) | 2010-05-12 |
| CN101704868B true CN101704868B (en) | 2012-07-04 |
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| CN2009102328024A Expired - Fee Related CN101704868B (en) | 2009-10-20 | 2009-10-20 | Method for preparing naringin |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106946958B (en) * | 2017-03-21 | 2019-04-19 | 李潇 | Purposes of the biochemical extraction process and its extract of aurantiin in treatment dermatitis |
| CN108129532A (en) * | 2018-02-05 | 2018-06-08 | 广东药科大学 | A kind of method that aurantiin is prepared based on Exocarpium Citri Grandis |
| CN110713508A (en) * | 2018-07-13 | 2020-01-21 | 重庆市畜牧科学院 | Method for extracting naringin from citrus pulp |
| CN109970828B (en) * | 2019-04-25 | 2022-03-11 | 天然润宝健康产业有限公司 | Method for extracting naringin from exocarpium citri rubrum |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1431216A (en) * | 2003-01-21 | 2003-07-23 | 中山大学 | Method for extracting naringin |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1431216A (en) * | 2003-01-21 | 2003-07-23 | 中山大学 | Method for extracting naringin |
Non-Patent Citations (3)
| Title |
|---|
| 闻永举等.D101型大孔吸附树脂对柚皮中柚皮苷的富集研究.《中国现代中药》.2008,第10卷(第8期),第32-34页. * |
| 闻永举等.柚皮中柚皮苷提取工艺研究.《江苏农业科学》.2008,(第4期),第257-258页. * |
| 韦英杰等.化橘红中黄酮成分提取工艺的研究.《时珍国医国药》.2004,第15卷(第7期),第407-408页. * |
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