CN101417916A - Glutinous rice scented tea squalene and preparation method thereof - Google Patents
Glutinous rice scented tea squalene and preparation method thereof Download PDFInfo
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- CN101417916A CN101417916A CNA2007101682258A CN200710168225A CN101417916A CN 101417916 A CN101417916 A CN 101417916A CN A2007101682258 A CNA2007101682258 A CN A2007101682258A CN 200710168225 A CN200710168225 A CN 200710168225A CN 101417916 A CN101417916 A CN 101417916A
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Abstract
The invention discloses a glutinous rice scented tea squalene and a preparation method thereof. The method includes the following steps: after drying the leaves of glutinous rice scented tea, then smashing the leaves; digesting the lipophilic substance by an organic solvent and liquid carbon dioxide; removing the organic solvent in the lipophilic substance, thus obtaining the crude extract of glutinous rice scented tea squalene; putting the crude extract of glutinous rice scented tea squalene into alumina or silicon glue layer and using organic solvent to remove such things. The content of the competitive products is more than 90 percent. Tested in a gas phase chromatography method, gas chromatograph-mass spectrum method, infra-red sepectrometry method, nuclear magnetic resonance method, the fingerprint is in correspondence with that of the standard product of the glutinous rice scented tea squalene. The product has the special flavor of squalene and can fully replace the squalene extracted from the liver of sharks in the deep sea. The glutinous rice scented tea squalene competitive products can be used as the standard product of squalene.
Description
Technical field
Glutinous rice scented tea squalene that the present invention relates to from plant leaf, extract and preparation method thereof.
Background technology
The chemical name of squalene (squalene) is: 2,6,10,15,19, and 23-hexamethyl-2,6,14,18,22-20 carbon six alkene.Be the long-chain triterpene compound, belong to height unsaturated hydrocarbons compounds, also claim fish shark alkene, shark alkene, squalene, dog-fish oil element or Oils,glyceridic,cod-liver terpene.Relative density is 0.8584, and fusing point is-75 ℃, the about 330 ℃/normal pressure of boiling point (decomposition), flash-point is 110 ℃, and refractive index is 1.4965 (20 ℃), and viscosity is 0.012Pas, be dissolved in acetone, ethanol, sherwood oil, ethyl acetate, normal hexane, benzene, chloroform and tetracol phenixin, water insoluble.Molecular formula is C
30H
50, relative molecular weight is 410.7, is colourless or little yellow oily liquid.Squalene has stronger biological activity, but enhancing body physiological function, improve immunizing power, can improve the oxygen carrying capacity of human body hemoglobin, enhance metabolism, reducing cholesterol is adjusted fat and proteic ratio, help the ultraviolet injury of opposing, be used for the control of various anoxic diseases, hepatitis, heart trouble and cancer clinically.In addition, squalene can be made lubricant through chemically modified, is used for processor, and better safety and sanitation and thermostability, oxidation-resistance and oilness are arranged.Therefore be widely used in every field such as medicine, beauty treatment, makeup, food and chemical industry.
At present, the squalene main source is abyssal pelagic fishes, based on shark, as phase shark (Centrophores), armour shark (Delatiaslicha), spinule shark (Centrophorusugato), edge kiss Tian Shi shark (Deaniacalea), New Zealand crow shark (Etmopterusbaxteri).In the shark liver oil of different types of deep-sea, the content of squalene has nothing in common with each other, generally between 15～80%.The general technology process of extracting squalene from the shark liver is: raw material is smashed to pieces, saponification, separation, crude product, refining, squalene product.For example from shark liver oil, extract squalene, raw material is directly carried out underpressure distillation or carries out saponification, separate the swallow that obtains reducing pressure again behind the unsaponifiables and heat up in a steamer depickling, then and the sodium Metal 99.5 underpressure distillation, can adopt solvent (ethanol) to handle at last, obtain the squalene highly finished product through underpressure distillation.The alumina layer of employing folding is also arranged, obtain highly purified squalene.
Squalene removes and is present in inside and outside the animal body, also is distributed widely in the plant materials.All there is squalene in parts such as root, blade, stem, skin and seed many plants, as seed, the seed of olive, Amaranthus seed, Grosvenor Momordica seed, the tail alpine ash (Eucalyptus urophylla S.T.Blake * E.grandis W.Hill ex Mainden) of Salvia japonica Thunb., tobacco leaf, pteridophyte, algae and bryophyte, part babassu.Wherein with sweet oil, plam oil, Grosvenor Momordica seed and Amaranthus seed oil content for the highest.As squalene content is up to 1.16% in the sweet oil of collecting in Spain autumn, squalene content reaches 5～8% in the seed oil of Amaranthus, and Grosvenor Momordica kind benevolence content is about 20%, and the timber content of tail alpine ash is about 0.79%.The extraction of squalene mainly is to use organic solvent extraction in the plant materials, removes the impurity of slightly carrying, and through purifying, obtains the squalene product.The organic solvent that uses is from hanging down the polarity sherwood oil to strong polar ethanol, the mode of extracting has cold soaking stain diacolation, refluxing extraction, Soxhlet extraction, microwave extraction and supersound extraction rope, and the method for removing impurity has the chemical reagent precipitator method, silica gel chromatography and molecular distillation method.
The deep-sea shark is precious watching for animals, and its growth and breeding potential are all lower, along with over-drastic is fished for, the possibility of disappearance in imminent danger are arranged, and lays in lessly from the plant resources of finding to contain squalene, and development and use acquire a certain degree of difficulty.And the application of squalene more and more widely, and market demand is increasing, and limited squalene resource can not satisfy the demand in market, is the key work that current urgency is expected solution so seek the new squalene resource that is simple and easy to obtain.
At present, domestic and international research person is seeking to prepare squalene with the synthetic method, even attempts adopting microbe fermentation method to obtain squalene, and these two kinds of approach still are in the laboratory preliminary study stage, also have bigger difference with practical application.So urgent need provides the preparation method of the squalene that a kind of cost is low, easy to operate, yield is high.
Summary of the invention
Glutinous rice scented tea (Teucrium manghuaense) is a kind of per nnial herb of southern china growth, plantation that can be a large amount of in Yunnan and Hainan, and the blade of can gathering the whole year, and reproduction speed is fast, plants under general fruit tree, and is with low cost.The present invention furthers investigate glutinous rice scented tea, finds to contain in its cured leaf sheet 0.2% the squalene of having an appointment.The invention provides and a kind ofly extract squalene from the glutinous rice scented tea blade, the method cost is low, easy to operate, yield is high, and the glutinous rice scented tea resource obtains more or less freelyly, has high promotional value.
The invention provides the preparation method of a kind of glutinous rice scented tea squalene that from the glutinous rice scented tea blade, extracts and glutinous rice scented tea squalene.
Glutinous rice scented tea squalene and preparation method thereof, the preparation method comprises the following steps:
(1), raw material is prepared: with the bright leaf crushed after being dried of glutinous rice scented tea, make powder, powder is generally at 10～80 orders;
(2), extract: make from the glutinous rice scented tea leaf with chemical organic solvent extraction method or super critical extraction and extract the crude extract that contains squalene the powder, its volume ratio V
Solvent/ V
The leaf powderBe 2～50:1;
(3), concentrate: remove the organic solvent in the lipid-soluble substance, promptly make the crude extract of glutinous rice scented tea squalene;
(4), purifying: with the crude extract peroxidation aluminium or the silica gel column chromatography of glutinous rice scented tea squalene, use the organic solvent wash-out, collect colourless elutriant part;
(5), reconcentration: the colourless elutriant that will collect is removed organic solvent with distillation under vacuum, and vacuum degree control is at 200～350mbar, and bath temperature is controlled at 35 ℃-55 ℃, promptly makes the glutinous rice scented tea squalene elaboration.
Chemical organic solvent extraction method of described usefulness or supercritical extraction method can extract it from the glutinous rice scented tea blade; Described chemical organic solvent extraction method: be selected from ethanol, acetone, sherwood oil, chloroform, ethyl acetate, tetracol phenixin, benzene, normal hexane, the ether one or more; Described supercritical extraction method: select carbonic acid gas, ethanol is as entrainment agent.
The glutinous rice scented tea squalene that the present invention makes has the peculiar fragrance of squalene standard substance, and squalene content can substitute the squalene that extracts fully greater than 90% in the elaboration from the shark liver of deep-sea, and can use as the squalene standard substance.The glutinous rice scented tea squalene Products Development has huge social and economic benefit.
Description of drawings
Fig. 1 is the gas-chromatography collection of illustrative plates of glutinous rice scented tea squalene crude extract;
Fig. 2 is the gas-chromatography collection of illustrative plates of glutinous rice scented tea squalene elaboration;
Fig. 3 is the infared spectrum of squalene reference substance;
Fig. 4 is the infared spectrum of glutinous rice scented tea squalene elaboration;
Fig. 5 is the proton nmr spectra of glutinous rice scented tea squalene elaboration;
Fig. 6 is the carbon-13 nmr spectra of glutinous rice scented tea squalene elaboration.
Embodiment
Below in conjunction with embodiment the present invention is described.
The extracting method of glutinous rice scented tea squalene is very simple, it can be extracted from the glutinous rice scented tea blade with conventional chemical organic solvent extraction method or supercritical extraction method.Described chemical organic solvent is selected from one or more in ethanol, acetone, sherwood oil, chloroform, ethyl acetate, tetracol phenixin, benzene, normal hexane, the ether, and supercutical fluid is selected carbonic acid gas, and ethanol is as entrainment agent.The technology of extracting can adopt percolation, reflux extraction, soxhlet extraction, microwave extraction method, ultrasonic extraction and supercritical extraction method etc.
The invention provides the preparation method of a kind of glutinous rice scented tea squalene that from the glutinous rice scented tea blade, extracts and glutinous rice scented tea squalene.
Glutinous rice scented tea squalene and preparation method thereof, the preparation method comprises the following steps:
(1), raw material is prepared: with the bright leaf crushed after being dried of glutinous rice scented tea, make powder, powder is generally at 10～80 orders;
(2), extract: make from the bright leaf of glutinous rice scented tea with chemical organic solvent extraction method or super critical extraction and extract the crude extract that contains squalene the powder, its volume ratio V
Solvent/ V
The leaf powderBe 2～50:1;
(3), concentrate: remove the organic solvent in the lipid-soluble substance, promptly make the crude extract of glutinous rice scented tea squalene;
(4), purifying: with the crude extract peroxidation aluminium or the silica gel column chromatography of glutinous rice scented tea squalene, use the organic solvent wash-out, collect colourless elutriant part;
(5), reconcentration: the colourless elutriant that will collect is removed organic solvent with distillation under vacuum, and vacuum degree control is at 200～350mbar, and bath temperature is controlled at 35 ℃～55 ℃, promptly makes the glutinous rice scented tea squalene elaboration.
Chemical organic solvent extraction method of described usefulness or supercritical extraction method can extract it from the glutinous rice scented tea blade; Described chemical organic solvent extraction method: be selected from ethanol, acetone, sherwood oil, chloroform, ethyl acetate, tetracol phenixin, benzene, normal hexane, the ether one or more; Described supercritical extraction method: select carbonic acid gas, ethanol is as entrainment agent.
Embodiment 1:
Getting dried glutinous rice scented tea blade 100g pulverizes, adopt apparatus,Soxhlet's, use acetone to make extraction agent, carry out heating in water bath according to a conventional method and extract, temperature is controlled at 75 ℃～85 ℃, is back to that the solvent color is an oyster in the extractor, about general 12h, extraction finishes, and acetone is removed in underpressure distillation, gets the glutinous rice scented tea squalene crude extract.(45 * 600mm), the aluminum oxide consumption is 5～7 times of dry back sample, uses the sherwood oil wash-out with alumina chromatographic column on the crude extract, collect the colourless part of elutriant, remove sherwood oil with distillation under vacuum, promptly get glutinous rice scented tea squalene 0.21g, contain squalene 93.5% after testing.
Example 2:
Get dried glutinous rice scented tea blade 100g and pulverize, adopt microwave device, use acetone to make extraction agent, from the glutinous rice scented tea powder, extract the crude extract that contains squalene, extraction conditions: volume ratio V
Solvent/ V
The leaf powderBe 2:1, temperature is 80 ℃, intermittent backflow 30min, filtering and collecting filter liquid, residue repetitive operation 3 times.Extraction finishes, and acetone is removed in underpressure distillation (vacuum degree control is at 200～250mbar, and bath temperature is controlled at 50 ℃～55 ℃), gets the glutinous rice scented tea squalene crude extract.(45 * 600mm), the aluminum oxide consumption is 5～7 times of dry back sample, uses the sherwood oil wash-out with alumina chromatographic column on the crude extract, collect the colourless part of elutriant, remove sherwood oil with distillation under vacuum, promptly get glutinous rice scented tea squalene 0.182g, contain squalene 92.1% after testing.
Example 3:
Get dried glutinous rice scented tea blade 100g and pulverize, adopt ultrasonoscope, use acetone to make extraction agent, from the glutinous rice scented tea powder, extract the crude extract that contains squalene, extraction conditions: volume ratio V
Solvent/ V
The leaf powderBe 5:1,70 ℃ of temperature, hold-time 1h, filtering and collecting filter liquid, residue repetitive operation 3 times.Extraction finishes, and underpressure distillation removes (vacuum degree control is at 200～250mbar, and bath temperature is controlled at 50 ℃～55 ℃) and removes acetone, gets the glutinous rice scented tea squalene crude extract.(45 * 600mm), the silica gel consumption is 5～7 times of dry back sample, uses the sherwood oil wash-out with silica gel column chromatography on the crude extract, collect the colourless part of elutriant, remove sherwood oil with distillation under vacuum, promptly get glutinous rice scented tea squalene 0.175g, contain squalene 91.7% after testing.
Example 4:
Getting dried glutinous rice scented tea blade 100g pulverizes, adopt apparatus,Soxhlet's, use ether to make extraction agent, carry out heating in water bath according to a conventional method and extract, be back to that the solvent color is an oyster in the extractor, about general 12h, extraction finishes, ether is removed in underpressure distillation (vacuum degree control is at 300～350mbar, and bath temperature is controlled at 35 ℃～40 ℃), gets the glutinous rice scented tea squalene crude extract.(45 * 600mm), the aluminum oxide consumption is 5～7 times of dry back sample, uses the sherwood oil wash-out with alumina chromatographic column on the crude extract, collect the colourless part of elutriant, remove sherwood oil with distillation under vacuum, promptly get glutinous rice scented tea squalene 0.195g, contain squalene about 91.0% after testing.
Example 5:
Get dried glutinous rice scented tea blade 100g and pulverize, adopt the supercritical fluid extraction instrument, use liquid carbon dioxide to make extraction agent, the ethanol of leaf powder 15% is done entrainment agent, 45 ℃ of temperature, and pressure 40MPa extracts 3h, obtains the glutinous rice scented tea squalene crude extract.(45 * 600mm), the aluminum oxide consumption is 2～4 times of dry back sample, uses the sherwood oil wash-out with alumina chromatographic column on the crude extract, collect the colourless part of elutriant, remove sherwood oil with distillation under vacuum, promptly get glutinous rice scented tea squalene 0.175g, contain squalene about 90.0% after testing.
Example 6:
Getting dried glutinous rice scented tea blade 100g pulverizes, adopt apparatus,Soxhlet's, use acetone+ether (9:1) to make extraction agent, carrying out heating in water bath according to a conventional method extracts, temperature is controlled at 70 ℃～80 ℃ and is back to that the solvent color is an oyster in the extractor, and about general 12h, extraction finishes, organic solvent is removed in underpressure distillation, gets the glutinous rice scented tea squalene crude extract.(45 * 600mm), the aluminum oxide consumption is 5～7 times of dry back sample, uses the sherwood oil wash-out with alumina chromatographic column on the crude extract, collect the colourless part of elutriant, remove sherwood oil with distillation under vacuum, promptly get glutinous rice scented tea squalene 0.207g, contain squalene about 91.8% after testing.
Claims (2)
1, glutinous rice scented tea squalene and preparation method thereof is characterized in that: the preparation method comprises the following steps:
(1), raw material is prepared: with the bright leaf crushed after being dried of glutinous rice scented tea, make powder, powder is generally at 10～80 orders;
(2), extract: make from the glutinous rice scented tea leaf with chemical organic solvent extraction method or super critical extraction and extract the crude extract that contains squalene the powder, its volume ratio V
Solvent/ V
The leaf powderBe 2～50:1;
(3), concentrate: remove the organic solvent in the lipid-soluble substance, promptly make the crude extract of glutinous rice scented tea squalene;
(4), purifying: with the crude extract peroxidation aluminium or the silica gel column chromatography of glutinous rice scented tea squalene, use the organic solvent wash-out, collect colourless elutriant part;
(5), reconcentration: the colourless elutriant that will collect is removed organic solvent with distillation under vacuum, and vacuum degree control is at 200～350mbar, and bath temperature is controlled at 35 ℃～55 ℃, promptly makes the glutinous rice scented tea squalene elaboration.
2, glutinous rice scented tea squalene according to claim 1 and preparation method thereof is characterized in that: it can be extracted from the glutinous rice scented tea blade with chemical organic solvent extraction method or supercritical extraction method; Described chemical organic solvent extraction method: be selected from ethanol, acetone, sherwood oil, chloroform, ethyl acetate, tetracol phenixin, benzene, normal hexane, the ether one or more; Described supercritical extraction method: select carbonic acid gas, ethanol is as entrainment agent.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102028060A (en) * | 2010-11-02 | 2011-04-27 | 浙江大学 | Method for preparing extract of oil soluble tea |
| CN102161611A (en) * | 2011-03-11 | 2011-08-24 | 中国烟草总公司广东省公司 | Method for preparing squalene based on tobacco as raw material |
| CN105067715A (en) * | 2015-08-13 | 2015-11-18 | 苏州优谱德精密仪器科技有限公司 | Method for detecting complicated organic chemical raw materials |
| CN110128238A (en) * | 2019-06-05 | 2019-08-16 | 武汉工程大学 | A method of entrainment extracts and overcritical isolates and purifies squalene from Grain Production of Amaranthus seed |
-
2007
- 2007-10-26 CN CNA2007101682258A patent/CN101417916A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102028060A (en) * | 2010-11-02 | 2011-04-27 | 浙江大学 | Method for preparing extract of oil soluble tea |
| CN102161611A (en) * | 2011-03-11 | 2011-08-24 | 中国烟草总公司广东省公司 | Method for preparing squalene based on tobacco as raw material |
| CN102161611B (en) * | 2011-03-11 | 2013-08-07 | 中国烟草总公司广东省公司 | Method for preparing squalene based on tobacco as raw material |
| CN105067715A (en) * | 2015-08-13 | 2015-11-18 | 苏州优谱德精密仪器科技有限公司 | Method for detecting complicated organic chemical raw materials |
| CN110128238A (en) * | 2019-06-05 | 2019-08-16 | 武汉工程大学 | A method of entrainment extracts and overcritical isolates and purifies squalene from Grain Production of Amaranthus seed |
| CN110128238B (en) * | 2019-06-05 | 2021-10-15 | 武汉工程大学 | Method for extracting squalene from amaranthus hypochondriacus seeds in entrainment mode and separating and purifying squalene in supercritical mode |
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Application publication date: 20090429 |