CN102198231A - Method for extracting ceramide-rich lipid from byproducts of agriculture and forestry by supercritical extraction technology - Google Patents
Method for extracting ceramide-rich lipid from byproducts of agriculture and forestry by supercritical extraction technology Download PDFInfo
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- CN102198231A CN102198231A CN201110085912XA CN201110085912A CN102198231A CN 102198231 A CN102198231 A CN 102198231A CN 201110085912X A CN201110085912X A CN 201110085912XA CN 201110085912 A CN201110085912 A CN 201110085912A CN 102198231 A CN102198231 A CN 102198231A
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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
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- 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 ceramide-rich lipid by adopting a green supercritical extraction technology and taking cheap byproducts of agriculture and forestry raw materials, and the method has unlimited market potential and values of ecological and environment friendliness. During the operation of supercritical extraction equipment, temperature is controlled to 60 to 100 DEG C, pressure is controlled to 10 to 30 MPa, and time is controlled to 1 to 3 hours; during the operation, 10-20% methanol and ethanol as entrainers are added, and then extract liquid is obtained, and is rotated and evaporated to dryness to obtain the ceramide-rich active lipid; and after alkali treatment, ceramide is separated by high-efficiency liquid chromatography. The method disclosed by the invention belongs to a green technology, has the advantages of high extraction yield, simplified separation steps and low cost, and simultaneously can be used for obtaining ceramide lipid in different contents.
Description
Technical field
The present invention relates to field that agriculture and forestry by-product is carried out the green preparation of reactive compound by supercritical extraction technique, especially about extracting the method that is rich in the ceramide lipid in the agriculture and forestry by-product.
Background technology
Agriculture and forestry by-product can be used as regenerated organic-biological resource, is used for the different compound products of human's demand, helps to alleviate the world resource crisis, solves the raw material problem of following organic products.
Ceramide has been studied determines that its characteristic effect is its moisture holding capacity, results to contain hydrophilic radical in the ceramide structure, and water is had affinity interaction preferably, is described as " king of moisturizing ", is 16 times of hyaluronic acid moisture-keeping efficacy.Especially the old dry skin effective percentage of preserving moisture is reached 80%.
Ceramide combines the ceramide glycolipid (cerabroside) that forms with sugar and is distributed widely in the animal and plant body, and particularly in central nervous system, liver, spleen and the hemocyte, it forms the cell membrane of animal and plant tissue.As the receptor of membrane antigen and virus, antibacterial and toxin thereof, they are at cell recognition, and cell binds, and regulates cellular immunization, and aspects such as decision blood group play a very important role.To the research of ceramide and ceramide glycolipid, caused that people pay attention to widely in recent years.The various countries scholar constantly separates from biology and obtains this compounds, and has synthesized a large amount of analog, finds that it has effects such as antitumor, antiviral, anti-liver poison, immunological enhancement.
The United Nations Industrial Development Organization is referred to as a kind of resource of underusing to Testa oryzae.At present in the Japanese market containing Testa oryzae ceramide mass fraction at powder-type more than 0.3% and aqueous type goods, as the important source material of beauty food.Before centuries, it is found that wine brewing craftsman's hands Bai Youxi again, secret is exactly one of the raw material of making wine Testa oryzae.Contain the bioactive molecule of clock more than 30 in the Testa oryzae, as ceramide, γ-An Jidingsuan, vitamin A, vitamin E, nicotinic acid etc.Developed at present abroad the multiple use of Testa oryzae, as rice bran nutrients, Testa oryzae trophic fiber, rice bran protein, these are that the health product and the skin care item impetus of raw material is powerful with the Testa oryzae.
Supercritical is a supercritical fluid, be a kind of not only on-gaseous between gas-liquid but also the states of matter of non-liquid state, this material can only could exist when its temperature and pressure postcritical, the density of supercritical fluid is bigger, similar with liquid, and its viscosity approaches gas, so supercritical fluid is a kind of very good extractant.Supercritical fluid is contacted with material to be separated, it is extracted the composition of polarity size, boiling point height and molecular weight size selectively successively.Certainly, the resulting extract of corresponding each pressure limit can not be single, but the blending constituent that can controlled condition obtains optimal proportion, method by decompression, intensification makes supercritical fluid become common gases then, be extracted material and then separate out fully or substantially, separate the purpose of purifying thereby reach.
It is that raw material is produced and is rich in the ceramide lipid from agriculture and forestry by-product that prior art adopts solvent method more, and it is lower to have an extraction ratio, complex steps, and impure height in the lipid of ceramide, solvent recovery needs power consumption, shortcomings such as parting material contaminated environment.This patent is a raw material with the agriculture and forestry by-product of recycling cheapness, adopts green supercritical extraction technique to extract and is rich in the ceramide lipid, has great market potential and ecological, environmental protective and is worth.
Summary of the invention
The object of the invention provides a kind of green method that is rich in the ceramide lipid that extracts in the agriculture and forestry by-product, effectively prepares the ceramide lipid.
Concrete technical scheme of the present invention is as follows:
The present invention is that a kind of supercritical extraction technique extracts the method that is rich in the ceramide lipid in the agriculture and forestry by-product, with the agriculture and forestry by-product is raw material, adopt green supercritical extraction technique to extract and be rich in the active lipid of ceramide in the agriculture and forestry by-product, preparation process is as follows:
1), with the garbage drying of agriculture and forestry by-product Testa oryzae, Testa Tritici, corn processed, pulverizing the order number is less than 1mm, the agriculture and forestry by-product that takes by weighing processing places supercritical extraction equipment to extract still, still is extracted in sealing, logical CO
2, control temperature, pressure;
2), in service at supercritical extraction equipment, control temperature at 60～100 ° of C, pressure is controlled at 10～30MPa, the time was controlled at 1～3 hour, during add entrainer;
3) obtain extract, then, the rotation evaporate to dryness must be rich in the active lipid 1 of ceramide;
4), the lipid 1 that will be rich in ceramide joins 0.1～0.5mol/L sodium methoxide solution, be rich in the lipid 1 of ceramide: the sodium methoxide solution weight ratio is 1: 80～150, stir 5～24h at normal temperatures, after alkali treatment is finished, reactant liquor is rotated evaporate to dryness, be rich in the lipid 2 of ceramide after the acquisition alkali treatment;
5), get the lipid that is rich in ceramide 2 after the above-mentioned alkali treatment, separate the lipid 3 that obtains ceramide through high performance liquid chromatography, be NMR, ESI-MS, analyze its structure.
The active lipid of ceramide of the present invention comprises: ceramide, sugar are sewed ceramide, sugar and are sewed steroid, sugar and sew phospholipid, sugar and sew one or more of glyceride.
The alkali that the present invention relates to alkali treatment comprises sodium hydroxide, potassium hydroxide.
The alkali that the present invention relates to alkali treatment is Feldalat NM.
Entrainer of the present invention comprises enzyme or a kind of and two or more alcohols.
Entrainer of the present invention is 10～20% methanol, ethanol.
Agricultural byproducts of the present invention comprise agricultural processing wastes such as Testa oryzae, Testa Tritici, corn, fruit and vegerable.
The present invention relates to entrainer and comprise a kind of and two or more alcohols, the best is an ethanol.
The alkali that the present invention relates to alkali treatment comprises sodium hydroxide, potassium hydroxide and Feldalat NM, is good with Feldalat NM.
Beneficial effect of the present invention is as follows:
1, supercritical extraction can and mainly be CO at lower temperature
2Extract under gas shrouds, prevented the oxidation and the loss of heat-sensitive substance effectively, kept effective ingredient in the extract;
2, extraction unites two into one with separating, as the CO of saturated solute
2When fluid enters separator, because the decline or the variation of temperature of pressure, make CO
2Separate rapidly with extract, not only Cui Qu efficient height but also energy consumption is less, has improved production efficiency;
3, CO
2Gas price is cheap, the purity height, and extraction ratio improves, and has simplified separating step.And can repetitive cycling use aborning, thereby whole technique has reduced cost effectively;
4, avoid using chlorinated solvents, the alcohols entrainer of use is easily removed, and can be recycled;
5, technology is simple grasps easily, and the speed of extraction is fast, belongs to the environmental friendliness technology;
6, obtain the ceramide lipid of different content simultaneously.
The specific embodiment
Embodiment 1
The 1st step: with the garbage drying of Testa oryzae processing, pulverizing the order number is less than 1mm, and the agriculture and forestry by-product that takes by weighing processing places supercritical extraction equipment to extract still, and still is extracted in sealing, logical CO
2, control temperature, pressure;
The 2nd step: in service at supercritical extraction equipment, 60～100 ° of C of control temperature, pressure is controlled at 10～30MPa, and the time was controlled at 1～3 hour; The methanol, the ethanol that add entrainer 10～20% during this time;
The 3rd step: obtain extract then, the rotation evaporate to dryness must be rich in the active lipid 1 of ceramide;
The 4th step: the lipid 1 that will be rich in ceramide joins 0.1～0.5mol/L sodium methoxide solution, be rich in the lipid 1 of ceramide: the sodium methoxide solution weight ratio is 1: 80～150, stir 5～24h at normal temperatures, after alkali treatment is finished, reactant liquor is rotated evaporate to dryness, be rich in the lipid 2 of ceramide after the acquisition alkali treatment;
The 5th step: get the lipid that is rich in ceramide 2 after the above-mentioned alkali treatment, separate the lipid 3 that obtains ceramide, be NMR, ESI-MS, analyze its structure through high performance liquid chromatography.
Embodiment 2
Preparation process and method according to embodiment 1.
The Testa Tritici that 100 grams were handled, powder particle diameter place supercritical extraction equipment to extract still less than 1mm, and still is extracted in sealing, logical CO
2, the control temperature, pressure, in service at supercritical extraction equipment, control temperature 60 ° of C, pressure is controlled at 20MPa, the time was controlled at 2 hours, during add the methanol of 10% entrainer, obtain extract then, CO
2Separate rapidly with extract, rotate evaporate to dryness again, must be rich in the active lipid 1 of ceramide, the lipid 1 that is rich in ceramide is joined 0.35mol/L sodium methoxide solution 100mL, stir 10h at normal temperatures, after alkali treatment is finished, reactant liquor is rotated evaporate to dryness, obtain to be rich in the lipid 2 of ceramide, be rich in the lipid 3 of the lipid 2 of ceramide through the isolating ceramide of high performance liquid chromatography, be NMR, ESI-MS, analyze its structure, ceramide extraction ratio 95%.
Embodiment 3
Preparation process and method according to embodiment 1.
The corn processed garbage that 100 grams were handled, powder particle diameter place supercritical extraction equipment to extract still less than 1mm, and still is extracted in sealing, logical CO
2, control temperature, pressure.In service at supercritical extraction equipment, 100 ° of C of control temperature, pressure is controlled at 25MPa, and the time was controlled at 1.5 hours; The ethanol that adds 10% entrainer during this time obtains extract, CO then
2Separate rapidly with extract, rotate evaporate to dryness again, must be rich in the active lipid 1 of ceramide, the lipid 1 that is rich in ceramide is joined 0.4mol/L potassium hydroxide solution 100mL, stir 15h at normal temperatures, after alkali treatment is finished, reactant liquor is rotated evaporate to dryness, obtain to be rich in the lipid 2 of ceramide, be rich in the lipid 3 of the lipid 2 of ceramide through the isolating ceramide of high performance liquid chromatography, be NMR, ESI-MS, analyze its structure, ceramide extraction ratio 93%.
Project is subsidized: state natural sciences fund 30870553; The International Technology collaborative project 2010DFA34370 of country.
Claims (6)
1. a supercritical extraction technique extracts the method that is rich in the ceramide lipid in the agriculture and forestry by-product, it is characterized in that: be raw material with the agriculture and forestry by-product, adopt green supercritical extraction technique to extract and be rich in the active lipid of ceramide in the agriculture and forestry by-product, preparation process is as follows:
1), with the garbage drying of agriculture and forestry by-product Testa oryzae, Testa Tritici, corn processed, pulverizing the order number is less than 1mm, the agriculture and forestry by-product that takes by weighing processing places supercritical extraction equipment to extract still, still is extracted in sealing, logical CO
2, control temperature, pressure;
2), in service at supercritical extraction equipment, control temperature at 60～100 ° of C, pressure is controlled at 10～30MPa, the time was controlled at 1～3 hour, during add entrainer;
3) obtain extract, then, the rotation evaporate to dryness must be rich in the active lipid 1 of ceramide;
4), the lipid 1 that will be rich in ceramide joins 0.1～0.5mol/L sodium methoxide solution, be rich in the lipid 1 of ceramide: the sodium methoxide solution weight ratio is 1: 80～150, stir 5～24h at normal temperatures, after alkali treatment is finished, reactant liquor is rotated evaporate to dryness, be rich in the lipid 2 of ceramide after the acquisition alkali treatment;
5), get the lipid that is rich in ceramide 2 after the above-mentioned alkali treatment, separate the lipid 3 that obtains ceramide through high performance liquid chromatography, be NMR, ESI-MS, analyze its structure.
2. supercritical extraction technique according to claim 1 extracts the method that is rich in the ceramide lipid in the agriculture and forestry by-product, it is characterized in that the active lipid of ceramide comprises: ceramide, sugar are sewed ceramide, sugar and are sewed steroid, sugar and sew phospholipid, sugar and sew one or more of glyceride.
3. supercritical extraction technique according to claim 1 extracts the method that is rich in the ceramide lipid in the agriculture and forestry by-product, and it is characterized in that: the alkali that relates to alkali treatment comprises sodium hydroxide, potassium hydroxide.
4. supercritical extraction technique according to claim 1 extracts the method that is rich in the ceramide lipid in the agriculture and forestry by-product, and it is characterized in that: the alkali that relates to alkali treatment is Feldalat NM.
5. supercritical extraction technique according to claim 1 extracts the method that is rich in the ceramide lipid in the agriculture and forestry by-product, and it is characterized in that: described entrainer comprises a kind of and two or more alcohols.
6. supercritical extraction technique according to claim 1 extracts the method that is rich in the ceramide lipid in the agriculture and forestry by-product, and it is characterized in that: described entrainer is 10～20% methanol, ethanol.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103755583A (en) * | 2014-01-27 | 2014-04-30 | 广州市娇兰化妆品有限公司 | Method for extracting and separating ceramide in konjac flying powder |
| CN104151244A (en) * | 2014-08-19 | 2014-11-19 | 南京农业大学 | Rice bran spirolactam-type compound and preparation method and application thereof |
| CN105218604A (en) * | 2015-10-19 | 2016-01-06 | 浙江大学 | Subcritical abstraction obtains the method for natural glycolipid |
| CN105403633A (en) * | 2015-10-28 | 2016-03-16 | 广州中大南沙科技创新产业园有限公司 | Method for determining content of ceramide in konjak |
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| CN101301067A (en) * | 2008-06-06 | 2008-11-12 | 浙江大学 | Method for synthetically extracting active matters in rice bran with separation technique |
| CN101591262A (en) * | 2009-06-09 | 2009-12-02 | 浙江大学 | Extract the method for the ceramide amphoteric lipid in the agriculture and forestry by-product |
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| CN101591262A (en) * | 2009-06-09 | 2009-12-02 | 浙江大学 | Extract the method for the ceramide amphoteric lipid in the agriculture and forestry by-product |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103755583A (en) * | 2014-01-27 | 2014-04-30 | 广州市娇兰化妆品有限公司 | Method for extracting and separating ceramide in konjac flying powder |
| CN103755583B (en) * | 2014-01-27 | 2015-07-01 | 广州市娇兰化妆品有限公司 | Method for extracting and separating ceramide in konjac flying powder |
| CN104151244A (en) * | 2014-08-19 | 2014-11-19 | 南京农业大学 | Rice bran spirolactam-type compound and preparation method and application thereof |
| CN104151244B (en) * | 2014-08-19 | 2016-08-17 | 南京农业大学 | A kind of rice bran spiral lactam analog compound and its preparation method and application |
| CN105218604A (en) * | 2015-10-19 | 2016-01-06 | 浙江大学 | Subcritical abstraction obtains the method for natural glycolipid |
| CN105218604B (en) * | 2015-10-19 | 2018-06-29 | 浙江大学 | The method that subcritical abstraction obtains natural glycolipid |
| CN105403633A (en) * | 2015-10-28 | 2016-03-16 | 广州中大南沙科技创新产业园有限公司 | Method for determining content of ceramide in konjak |
| CN105403633B (en) * | 2015-10-28 | 2018-05-11 | 广州中大南沙科技创新产业园有限公司 | Ceramide content assay method in konjaku |
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Application publication date: 20110928 |