CN102040612A - Method for extracting bergamottin from grapefruit peel - Google Patents
Method for extracting bergamottin from grapefruit peel Download PDFInfo
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- CN102040612A CN102040612A CN2010102932178A CN201010293217A CN102040612A CN 102040612 A CN102040612 A CN 102040612A CN 2010102932178 A CN2010102932178 A CN 2010102932178A CN 201010293217 A CN201010293217 A CN 201010293217A CN 102040612 A CN102040612 A CN 102040612A
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- citrus bergamia
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention relates to a method for extracting bergamottin from grapefruit peel. The method comprises the following processes of: dynamically extracting the grapefruit peel by using supercritical CO2 to obtain crude extract, separating the crude extract by using polyamide resin, eluting the crude extract by using deionized water, a 10 to 40 percent ethanol solution and a 60 to 80 percent ethanol solution in turn, collecting high ethanol eluent, re-crystallizing the eluent for 3 to 5 times by using petroleum ether, and drying the crystal under reduced pressure to obtain a product. The method for producing the bergamottin has the advantages of simple process, low carbon, environmental friendliness and safer production.
Description
Technical field:
The present invention relates to the extraction and purification process of Citrus bergamia element, particularly a kind of application supercritical CO
2Technology and polymeric amide isolation technique are extracted the method for purifying Citrus bergamia element.
Background technology:
Shaddock is the mature fruit of Citrus paradisi Macfadyen, originates in southern areas such as China Fujian, Jiangxi, Guangdong, Guangxi.Shaddock delicate fragrance, sour-sweet, Liang Run, nutritious, pharmaceutical use is very high, is that people like one of famous and precious fruit of food, also is the fruit of the medical circle tool dietotherapy benefit of generally acknowledging.
Modern pharmacology is analyzed, and the meat of shaddock and skin all are rich in the dried immature fruit of citron orange, new orange peel and carotene, vitamin B group, vitamins C, mineral substance, carbohydrate and volatilization wet goods.Shaddock ped is similar to other flavonoids, anti-inflammatory action is arranged, and the purer product anti-inflammatory action of shaddock ped mixture is stronger, and modern medicine and pharmacology is discovered, contain compositions such as profuse vitamins C and para-insulin in the shaddock meat, so have hypoglycemic, reducing blood-fat, fat-reducing, skin makeup to support effects such as appearance.Often edible, diseases such as diabetes, arteriosclerosis there is the assisting therapy effect, to obese person's beautifying function of being healthy and strong.
The Citrus bergamia element is a kind of derivative of tonka bean camphor, is present in the shaddock skin.Can be used as perfume base.
Citrus bergamia element (Bergamottin)
Another name: Fructus Citri Sarcodactylis element, bergamottin, Fructus Citri Sarcodactylis booth
Chemical name: 9-[(3-Methyl-2-buten-1-yl) oxy]-7h-furo[3,2-g] [1] benzopyran-7-one
Molecular formula: C
21H
22O
4
Molecular weight: 338.40
Compositional classification: linear furocoumarins class
Physical properties: clear crystal (by sherwood oil or ether-sherwood oil recrystallization).Fusing point 75-80 ℃.Can be dissolved in ethanol, ether, ethyl acetate, acetone equal solvent, water insoluble; Be dissolved in hot caustic solution and make the lactonic ring cracking, meet then cyclization again of acid.Fluorescence is arranged.
The report that extracts the Citrus bergamia element is less.General method normally adopts chromatography or chromatography to extract total coumarins, then with different eluent separation certain compositions wherein.Usually used chromatography comprises silica gel column chromatography and alumina column chromatography, and the acidity of silica gel and alkali alumina can make some tonka bean camphors rotten, so careful when in use.High performance liquid chromatography also generally is used to separate the tonka bean camphor composition in recent years, but is not fine to the few coumarins extraction effect of ester group., further do not segment only with squeezing the juice and extracting the effective constituent of having extracted shatian pomelo as Chinese patent CN1907138 " a kind of Shatian shaddock peel extract and extracting method and application " reported method.
Summary of the invention:
Technology of the present invention is simple, and energy consumption is lower, and solvent toxicity is little, and the dissolvent residual in the product is few, produces safer.
The object of the present invention is achieved like this:
1. supercritical extraction: get fresh shaddock skin chopping, the extractor of packing into, the logical CO that does not contain entrainment agent
2, be adjusted to suitable temperature and pressure and extracted 2～3 hours, the extracting solution decompression resolve filter crude product;
2. polymeric amide separates: above-mentioned crude product is disperseed with 80-90% ethanol, mix sample with polyamide resin, volatilize upper prop, with the ethanolic soln stepwise elution of deionized water and different ratios, collect the height ethanol eluate;
3. crystallization: after above-mentioned elutriant concentrating under reduced pressure is medicinal extract, use sherwood oil recrystallization 3～5 times, drying under reduced pressure, promptly.
The method of said extracted Citrus bergamia element is characterized in that described supercritical extraction condition: extracting temperature is 40～50 ℃, and extraction pressure is 20～35MPa, and resolution temperature is 50～60 ℃, and parsing pressure is 8～10MPa.
The method of said extracted Citrus bergamia element, the ethanol consumption is 5～7 times of amounts of crude product weight when it is characterized in that described dispersion.
The method of said extracted Citrus bergamia element is characterized in that described polymeric amide eluent successively is deionized water, 10～40% ethanolic solns and 60～80% ethanolic solns of 2～3 times of amount column volumes.
The method of said extracted Citrus bergamia element is characterized in that described elution process for using deionized water wash-out impurity earlier, detects the Citrus bergamia element with 10-40% ethanol elution to effluent liquid again, can not detect the Citrus bergamia element with 60-80% ethanol elution to effluent liquid at last.
There is following advantage in the present invention:
1) the supercritical extraction technology is emerging separation and extraction technology, and its advantage is CO
2Toxicological harmless own, security is higher, and at normal temperatures and pressures can be not residual, separates thoroughly;
2) this technology is not because the character of Citrus bergamia element can be brought any disadvantageous effect to subsequent step after therefore extracting, low carbonization without entrainment agent;
3) absorption and the wash-out by polymeric amide can make the furocoumarin(e) class gather soon, can not consume more heat simultaneously.
Further specify the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment.
Embodiment:
Embodiment 1:
Get fresh shaddock skin 10kg (the Citrus bergamia cellulose content 2.1%) extractor of packing into, sealing, CO
2Through cooling liquid in liquefied pot behind the purification utensil.Enter storage tank with high-pressure metering pump with CO
2Send into preheater; be heated to 40 ℃ by preheater; enter extractor by the extractor bottom; with relief valve extractor pressure is controlled to be 20MPa gradually; pressure-stabilisation in the knockout tower is at 8MPa; dynamic extraction 2 hours; emitting after the shutdown and separating out solid 888g is crude product, is scattered in 4.5L 80% ethanol, mixes sample with a small amount of polyamide resin; volatilize; the polyamide resin of last column volume 5L is successively used the 10L deionized water; 10% ethanol; 60% ethanol elution is collected 60% ethanol eluate; concentrating under reduced pressure is to use sherwood oil recrystallization 3 times behind the medicinal extract, and drying under reduced pressure gets finished product 167g (Citrus bergamia cellulose content 98.4%).
Embodiment 2:
Get fresh shaddock skin 10kg (the Citrus bergamia cellulose content 2.2%) extractor of packing into, sealing, CO
2Through cooling liquid in liquefied pot behind the purification utensil.Enter storage tank with high-pressure metering pump with CO
2Send into preheater; be heated to 45 ℃ by preheater; enter extractor by the extractor bottom; with relief valve extractor pressure is controlled to be 35MPa gradually; pressure-stabilisation in the knockout tower is at 9MPa; dynamic extraction 2.5 hours; emitting after the shutdown and separating out solid 910g is crude product, is scattered in 7L 90% ethanol, mixes sample with a small amount of polyamide resin; volatilize; the 15L deionized water is successively used in the polyamide resin absorption of last column volume 5L; 25% ethanol; 75% ethanol elution is collected 75% ethanol eluate; concentrating under reduced pressure is to use sherwood oil recrystallization 4 times behind the medicinal extract, and drying under reduced pressure gets finished product 165g (Citrus bergamia cellulose content 98.6%).
Embodiment 3:
Get fresh shaddock skin 10kg (the Citrus bergamia cellulose content 2.0%) extractor of packing into, sealing, CO
2Through cooling liquid in liquefied pot behind the purification utensil.Enter storage tank with high-pressure metering pump with CO
2Send into preheater; be heated to 40 ℃ by preheater; enter extractor by the extractor bottom; with relief valve extractor pressure is controlled to be 30MPa gradually; pressure-stabilisation in the knockout tower is at 10MPa; dynamic extraction 2 hours; emitting after the shutdown and separating out medicinal extract 918g is crude product, is scattered in 6.4L 85% ethanol, mixes sample with a small amount of polyamide resin; volatilize; the 12L deionized water is successively used in the polyamide resin absorption of last column volume 5L; 40% ethanol; 80% ethanol elution is collected 80% ethanol eluate; concentrating under reduced pressure is to use sherwood oil recrystallization 5 times behind the medicinal extract, and drying under reduced pressure gets finished product 171g (Citrus bergamia cellulose content 99.1%).
Embodiment 4:
Get fresh shaddock skin 10kg (the Citrus bergamia cellulose content 2.2%) extractor of packing into, sealing, CO
2Through cooling liquid in liquefied pot behind the purification utensil.Enter storage tank with high-pressure metering pump with CO
2Send into preheater; be heated to 50 ℃ by preheater; enter extractor by the extractor bottom; with relief valve extractor pressure is controlled to be 35MPa gradually; pressure-stabilisation in the knockout tower is at 9MPa, dynamic extraction 3 hours, and emitting after the shutdown and separating out medicinal extract 879g is crude product; be scattered in 6L 80% ethanol; mix sample with a small amount of polyamide resin, volatilize, the polyamide resin absorption of last column volume 5L; successively use the 10L deionized water; 30% ethanol, 70% ethanol elution is collected 70% ethanol eluate; concentrating under reduced pressure is to use sherwood oil recrystallization 5 times behind the medicinal extract, and drying under reduced pressure gets finished product 185g (Citrus bergamia cellulose content 99.3%).
Claims (5)
1. method of extracting the Citrus bergamia element from the shaddock skin is characterized in that comprising following step:
1. supercritical extraction: get fresh shaddock skin chopping, the extractor of packing into, the logical CO that does not contain entrainment agent
2, be adjusted to suitable temperature and pressure and extracted 2～3 hours, the extracting solution decompression resolve filter crude product;
2. polymeric amide separates: above-mentioned crude product is disperseed with 80-90% ethanol, mix sample with polyamide resin, volatilize upper prop, with the ethanolic soln stepwise elution of deionized water and different ratios, collect the height ethanol eluate;
3. crystallization: after above-mentioned elutriant concentrating under reduced pressure is medicinal extract, use sherwood oil recrystallization 3～5 times, drying under reduced pressure, promptly.
2. according to the method for the described extraction Citrus bergamia of claim 1 element, it is characterized in that described supercritical extraction condition: extracting temperature is 40～50 ℃, and extraction pressure is 20～35MPa, and resolution temperature is 50～60 ℃, and parsing pressure is 8～10MPa.
3. according to the method for the described extraction Citrus bergamia of claim 1 element, the ethanol consumption is 5～7 times of amounts of crude product weight when it is characterized in that described dispersion.
4. according to the method for the described extraction Citrus bergamia of claim 1 element, it is characterized in that described polymeric amide eluent successively is deionized water, 10～40% ethanolic solns and 60～80% ethanolic solns of 2～3 times of amount column volumes.
5. according to the method for the described extraction Citrus bergamia of claim 1 element, it is characterized in that described elution process is for using deionized water wash-out impurity earlier, detect the Citrus bergamia element with 10-40% ethanol elution to effluent liquid again, can not detect the Citrus bergamia element with 60-80% ethanol elution to effluent liquid at last.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010102932178A CN102040612A (en) | 2010-09-27 | 2010-09-27 | Method for extracting bergamottin from grapefruit peel |
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| CN2010102932178A CN102040612A (en) | 2010-09-27 | 2010-09-27 | Method for extracting bergamottin from grapefruit peel |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2014118370A (en) * | 2012-12-14 | 2014-06-30 | Ogawa & Co Ltd | Method of manufacturing polymethoxyflavones |
| CN104173335A (en) * | 2014-08-08 | 2014-12-03 | 浙江大学 | Application of bergamottin in preparation of medicines for preventing and treating diabetes |
| CN106011321A (en) * | 2016-05-16 | 2016-10-12 | 武汉轻工大学 | Method for extracting alcohol-soluble sugar from shaddock peel |
| CN107383040A (en) * | 2017-07-05 | 2017-11-24 | 浙江大学 | A kind of method that bergamot element is isolated and purified from early fragrant shaddock oil vacuole layer |
| CN108185432A (en) * | 2017-12-31 | 2018-06-22 | 西双版纳天恩生物科技开发有限公司 | The preparation method of Flos Rosae Rugosas pollen is lyophilized |
| CN114874199A (en) * | 2022-04-21 | 2022-08-09 | 集美大学 | Method for simultaneously preparing epoxy auraptene and epoxy bergamottin |
-
2010
- 2010-09-27 CN CN2010102932178A patent/CN102040612A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2014118370A (en) * | 2012-12-14 | 2014-06-30 | Ogawa & Co Ltd | Method of manufacturing polymethoxyflavones |
| CN104173335A (en) * | 2014-08-08 | 2014-12-03 | 浙江大学 | Application of bergamottin in preparation of medicines for preventing and treating diabetes |
| CN106011321A (en) * | 2016-05-16 | 2016-10-12 | 武汉轻工大学 | Method for extracting alcohol-soluble sugar from shaddock peel |
| CN106011321B (en) * | 2016-05-16 | 2019-06-14 | 武汉轻工大学 | The method of the molten sugar of alcohol is extracted from pomelo peel |
| CN107383040A (en) * | 2017-07-05 | 2017-11-24 | 浙江大学 | A kind of method that bergamot element is isolated and purified from early fragrant shaddock oil vacuole layer |
| CN108185432A (en) * | 2017-12-31 | 2018-06-22 | 西双版纳天恩生物科技开发有限公司 | The preparation method of Flos Rosae Rugosas pollen is lyophilized |
| CN114874199A (en) * | 2022-04-21 | 2022-08-09 | 集美大学 | Method for simultaneously preparing epoxy auraptene and epoxy bergamottin |
| CN114874199B (en) * | 2022-04-21 | 2024-04-09 | 集美大学 | Method for simultaneously preparing epoxy orange peel oleosin and epoxy bergamotin |
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Application publication date: 20110504 |