CN1179775C - Method for superhigh pressure extracting small molecule component from biomaterial - Google Patents
Method for superhigh pressure extracting small molecule component from biomaterial Download PDFInfo
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Images
Abstract
The present invention provides a superhigh pressure method for extracting middle and small molecule components from biological materials, and relates to a method for extracting the biological materials. The method is mainly used for extracting solids and liquids, particularly middle and small molecule active ingredients of natural products. A mixture of raw material and solvent is pressurized and extracted, loaded in a hermetic high-pressure container, and pressurized at room temperature. When the pressure is boosted to the preset pressure more than 100MPas, the pressure is kept for 3 to 20 minutes; then, the pressure is discharged; finally, the mixture of raw material and solvent is taken out. The mixture of raw material and solvent is firstly loaded in a packaging bag 4. Then, the mixture of raw material and solvent is loaded in the hermetic high-pressure container 1, and a high-pressure medium 6 is led into a high-pressure working chamber of the high-pressure container. The processes of pressure rising, pressure maintenance and pressure discharge are carried out for the high-pressure medium 6, and then the mixture is taken out. The present invention changes the traditional method for extracting middle and small molecule components from biological materials, and has the characteristics of high extraction rate, high speed, etc.
Description
Technical field: the present invention relates to a kind of biomaterial extracting method, mainly is that solid-liquid extracts the particularly extraction of the medium and small molecule functional component of natural products.Biomaterial be meant the integral body of plant natural or artificial culture, animal and microorganism, partly, tissue, portion of tissue or other constituent.Little molecule is meant that the atom number of ingredient is less, the molecule that molecular weight is less.Generally speaking, molecular weight is no more than 10,000.Functional component is meant and can plays the treatment disease, regulate physiological activity, improve health status, promote the effect of growing humans and animals, improves the composition of proterties such as food or feed color.
Functional component kind in the natural products is a lot, belongs to mainly that biology seals, glucoside, organic acid, terpene (comprising diterpene, triterpene) class, quinones, ketone, steroid class, the plain class of phenylpropyl alcohol, resin, volatile oil, compound sugar, carbohydrate (starch, natural gum, cellulose), amino acid, protein, enzyme, tannin, phytochrome, grease, wax, inorganic salts etc.Modal is that a kind of functional component is by multiple different molecular composition.All can change after a lot of functional components are heated, perhaps lose effect, perhaps effect changes, and perhaps loses because of volatilization, perhaps reacts with other composition and becomes other material.
The solubility of these functional components in different solvents is different, generally can be divided into water-soluble, fat-soluble and pure dissolubility.
The chemical constitution of some functional component, the mechanism of action (property of medicine when particularly playing therapeutic action, pharmacological action) are known, and some still is unknown.
Here said super-pressure is meant that pressure surpasses the hydrostatic pressure of 100MPa.
Background technology: (the high monarch of hope compiles " Chinese wild plant exploitation and processing and utilization ", China Light Industry Press, in February, 1997) point out: " the natural products functional component extracts method commonly used to be had: solvent extraction method (comprising infusion process, percolation, decocting method, reflux extraction, continuous backflow extraction method), steam distillation and sublimed method." point out " Natural Medicine Chemistry " (Ministry of Public Health's planning teaching material, Yao Xinsheng chief editor, People's Health Publisher, in June, 1998): " from medicinal material, extract natural functional component solvent method, steam distillation and sublimed method are arranged.The range of application of the two kinds of methods in back is very limited, adopts solvent extraction method under the thumping majority situation." advantage of these methods is that operable solvent species is many, the functional component kind of extraction is many, the recovery rate height, but have the separation and purification difficulty, and the functional component sex change, volatilization loss is serious, and extraction time is long, problems such as complex process.These conventional extracting methods had also had suitable progress in the last few years, enzyme effect technology for example, the broken technology of raw material micro mist etc.But, should, although used these new technologies, fundamentally do not eliminate the drawback of these conventional extracting methods.
Emerging supercritical CO
2Extracting process has solved a series of problems of said extracted method, and very outstanding advantage is arranged aspect separation and purification, becomes the important method that functional component extracts in the natural products." supercritical fluid technique-principle and application " (Zhu Ziqiang writes, Chemical Industry Press, in March, 2000) pointed out; " CO
2Has lipophilic behavior.It has been generally acknowledged that supercritical CO
2Can extract the light fraction in essential oil, fat, alcohol, aldehyde, ketone, the cured and resin selectively ... sugared, many salt are insoluble to supercritical CO basically
2Water such as alkaloid, polysaccharide, steroid, terpene, glucoside or pure soluble substance are at CO
2In solubility very low, therefore it is very difficult to use this technology to extract.Alkaloid, nicotine, caffeine sometimes with other compound, in conjunction with forming salt, cause the extraction difficulty as citric acid, chlorogenic acid etc. ".In addition, supercritical CO
2Extract and also have problems such as apparatus expensive, operating cost height.
Technology contents: the objective of the invention is to overcome deficiency and shortcoming that existing extracting method exists, provide a kind of fast, the superhigh pressure extracting method of medium and small minute subconstiuent of biomaterial that recovery rate is high.
Above-mentioned purpose of the present invention is achieved in that accompanying drawings is as follows:
The superhigh pressure extracting method of medium and small minute subconstiuent of biomaterial is the mixture pressurised extraction that adopts raw material and solvent, the mixture of raw material and solvent is contained in the high-pressure bottle 1 of sealing, and at room temperature to its pressurization, carried out pressurize 3～20 minutes during predetermined pressure more than pressure is elevated to 100Mpa, the mixture of raw material and solvent is taken out in release then at last.
The mixture of raw material and solvent can be contained in earlier in the packaging bag 4, then in the high-pressure bottle 1 that reinstalls sealing, transmission medium 6 be introduced in the high-pressure working chamber of high-pressure bottles, to transmission medium 6 boost, pressurize, release, take out mixture then.
Can carry out one or more times boosting of carrying out of the mixture in the container or transmission medium 6, pressurize, stress-relief process.
Can in the high-pressure bottle working chamber, add physical action device 8, this device can boost preceding, when boosting, during pressurize, during release, after the release or have an effect in the whole high pressure extraction process, also can before high pressure extraction or after extracting, have an effect.
Said solvent can be water, lipid, alcohols or other organic solvent, in raw material and solvent mixture, can add chemistry or biological products.
In the high pressure extraction process, can with heat or lower the temperature and carry out simultaneously.
The present invention has the following advantages:
1. therefore all liq can select only solvent for use according to the character of extract as the transmission medium of super-pressure.Solvent can be water, lipid, alcohols or other organic solvent.Possess conventional extraction and can use the advantage of multiple solvent, do not have supercritical CO
2Extraction can only be extracted the shortcoming of liposoluble constituent.
2. super-pressure processing is generally all carried out at ambient temperature, and so long as not special heating or cooling, variations in temperature generally is no more than 5 ℃.Do not have leaching process such as hot dipping is got, distillation to be heated, functional component destroys, the shortcoming of loss, and is very favourable to extracting temperature sensitivity composition and volatile component.Sometimes in order to improve certain performance of extraction, as improving extract yield, changing the composition of extract etc., also can super-pressure and heat (intensification or lower the temperature) synergy.
3. in theory, the solubility of material in solvent raises along with pressure and increases.It is more than the 100MPa that super-pressure extracts the pressure that uses, conventional (atmospheric pressure) and the supercritical CO of extracting
2High many of the pressure of extraction when (pressure is below 10MPa).When therefore super-pressure extracted, what the solubility of active ingredient in solvent will be high was many, and it is also just much higher to extract yield.
4. under the super-pressure effect, cell membrane is destroyed, and intracellular functional component enters solvent easily; Simultaneously, solvent also enters biological cell inside easily.So greatly shortened extraction time.Conventional dipping and enzyme degraded generally need one day to several days, or longer.Supercritical CO
2The extraction time of extraction generally arrives several hrs one.Super-pressure extracts and generally only to need 5-10 minute, the longest can be above 30 minutes yet.
5. be subjected to the super-pressure effect, sex change will take place in macromolecular substances such as protein, starch, resin glue, bring convenience for separation, the purifying of solution;
6. versatility is good.Transmission medium can be the liquid identical with solvent, also can be different liquid.The running parameter of extra-high tension unit is easy to adjust and accurately control, and can guarantee that in high-pressure working chamber pressure everywhere is identical.This has not only guaranteed the in full accord of extraction conditions, and an extra-high tension unit need not be made any change and just can use multiple solvent, the multiple efficacies composition in the leaching plurality of raw materials.
7. super-pressure can act on synergy with other physics (as ultrasonic wave, mechanical agitation, electric pulse), chemistry (carrying agent, cosolvent, precipitating reagent as use) and biology (as the enzyme degraded), extract performance (as improving the yield of extract) to improve, change the constituent (as making certain become fractional precipitation) of extract, or change the proterties (as making certain functional component lose or connect certain group) of extract.
8. pollutant effulent is few.Therefore solubility of substances height under the ultra-high pressure condition can reduce solvent load significantly, thereby reduce emission.This is especially favourable with an organic solvent the time.
9. energy-conservation.When super-pressure extracts, be not catabiotic in the dwell time.The compressibility of liquid is very little, heating rising temperature and supercritical CO when the also conventional heat of the energy that consumes in the process of boosting is extracted
2During extraction CO
2Gas compresses and liquefies little many of the energy that consumed.
Description of drawings:
Fig. 1 carries out the schematic diagram of super-pressure extraction element in packaging bag to the mixture splendid attire of raw material and solvent by transmission medium;
Fig. 2 directly carries out the schematic diagram of super-pressure extraction element to the mixture of raw material and solvent;
Fig. 3 directly carries out the schematic diagram of super-pressure extraction element to the mixture of raw material and solvent by the piston pressurization;
Fig. 4 installs the schematic diagram that the physical action device carries out the super-pressure extraction element additional in Fig. 1.
1. high-pressure bottles, 2. end caps, 3. connecting pipes, 4. packaging bags, 5. mixtures, 6. transmission media, 7. pistons, 8. physical action devices among the figure
The specific embodiment: further specify particular content of the present invention and embodiment below in conjunction with accompanying drawing.
The present invention applies super-pressure (pressure is more than the 100MPa) by the mixture to raw material and solvent, and the functional component in the biomaterial is dissolved in the solvent.
The solvent that uses can be water, fat, alcohol (aqueous solution that comprises alcohol) or organic solvent (as benzinum, chloroform, acetone).What can extract is little molecule functional component.
These little molecule functional components belong to that biology seals, the light fraction in glucoside, organic acid, terpene (comprising diterpene, triterpene) class, alcohols, furans, quinones, ketone (comprising flavones) class, steroid class, phenols, the plain class of phenylpropyl alcohol, vitamins, volatile oil, resin and the wax, compound sugar, phytochrome, grease etc.Modal is that a kind of functional component is by multiple different molecular composition.
The processing step that super-pressure extracts is consulted Fig. 1 and is: the also sealing in packaging bag 4 of mixture 5 splendid attires of raw material and solvent.Packaging bag can be used soft material, and for example plastic sheeting is made; Also can use hard material, for example metal, glass are made.Requirement to packaging bag 4 is a good airproof performance, is subjected to super-pressure to do the time spent phenomenon of osmosis does not take place.Whole packing is put into high-pressure bottle 1, use end cap 2 sealed high-pressure vessels 1 then.By connecting pipe 3 transmission medium 6 is introduced in the high-pressure working chamber of high-pressure bottle 1 and end cap 2 compositions.By pump or pressurize to transmission medium by booster again, make the pressure in the high-pressure working chamber be elevated to predetermined value, this pressure is called operating pressure.The process of rising pressure is called boosts.Keep operating pressure certain hour length, this process is called pressurize.Keep the time span of operating pressure to be called the dwell time.Dwell time makes the pressure in the high-pressure working chamber reduce to zero after reaching predetermined value, and this process is called release.Take off end cap 2 backs and in high-pressure bottle 1, take out whole packing.Then by the mixture 5 that takes out raw material and solvent in the packaging bag 4.The high pressure extraction process finishes.
Also can consult Fig. 2: by pump or pass through booster again,, directly send into high-pressure working chamber by connecting pipe (3) the mixture 5 of raw material and solvent as transmission medium.Boost then, pressurize and release.
Also can end cap 2 be replaced by piston 7, consult Fig. 3: the piston motion realizes boosting by making, pressurize and release.
Consult Fig. 4: can add device 8 in the high-pressure working chamber, be called the synergy of super-pressure and physical method this moment to raw material and solvent deposits yields physical action.The physical action device can be a supersonic generator, electric pulse generator, mechanical stirring device, heater, the device of cooling device or other form.These devices can when boosting, in the dwell time, during release, after the release, or be had an effect in the whole high pressure extraction process before boosting.
These physical action devices also can not be attached on the high-pressure installation, before high pressure extraction, or have an effect after the high pressure extraction, are called pre-treatment and post processing this moment.
Can add chemicals or biological products in the mixture of raw material and solvent.The chemicals or the biological products that add can be a kind of, also can be multiple.They can be respectively or play jointly carry, effects such as altogether molten, inhibition, precipitation, reaction, improve the high pressure extraction performance or change the molecular structure of extract.
Example one
Transmission medium: kerosene and transformer oil mixture;
Solvent: water;
Raw material: tealeaves
Packing material: plastic sheeting
Operating pressure: 350MPa; Dwell time: 5 minutes; Pressure rising time, 20 seconds; The release time, 1 second;
Temperature: room temperature;
Functional component: theophylline.
Effect: identical with 95 ℃ of hot-water soaks 15 minutes, fragrance is denseer.
Example two
Transmission medium: kerosene and transformer oil mixture;
Solvent: liquor;
Raw material: matrimony vine
Packing material: plastic sheeting
Operating pressure: 400MPa; Dwell time: 5 minutes; Pressure rising time, 20 seconds; The release time, 1 second;
Temperature: room temperature;
Functional component: LBP-X.
Effect: with identical room temperature soaking in Chinese liquor 15 days.
Example three
Transmission medium: kerosene and transformer oil mixture;
Solvent: soybean oil;
Raw material: pimiento
Packing material: plastic sheeting
Operating pressure: 5000MPa; Dwell time: 10 minutes; Pressure rising time, 20 seconds; The release time, 1 second;
Temperature: room temperature;
Functional component: capsicum red pigment;
Effect: identical with fried 15 minutes of soya-bean oil.
Claims (6)
1. the superhigh pressure extracting method of medium and small minute subconstiuent of biomaterial, it is the mixture pressurised extraction that adopts raw material and solvent, it is characterized in that the mixture with raw material and solvent is contained in the high-pressure bottle of sealing (1), and at room temperature to its pressurization, carried out pressurize 3～20 minutes during predetermined pressure more than pressure is elevated to 100Mpa, the mixture of raw material and solvent is taken out in release then at last.
2. the superhigh pressure extracting method of medium and small minute subconstiuent of biomaterial according to claim 1, it is characterized in that and the mixture of raw material and solvent can be contained in earlier in the packaging bag (4), and then in the high-pressure bottle (1) of the sealing of packing into, transmission medium (6) is introduced in the high-pressure working chamber of high-pressure bottle, to transmission medium (6) boost, pressurize, release, take out mixture then.
3. the superhigh pressure extracting method of medium and small minute subconstiuent of biomaterial according to claim 1 and 2 is characterized in that can carrying out one or more times boosting of carrying out of the mixture in the container or transmission medium (6), pressurize, stress-relief process.
4. the superhigh pressure extracting method of medium and small minute subconstiuent of biomaterial according to claim 1 and 2, it is characterized in that in the high-pressure bottle working chamber, to add physical action device (8), this device can boost preceding, when boosting, during pressurize, during release, after the release or have an effect in the whole high pressure extraction process, also can before high pressure extraction or after extracting, have an effect.
5. the superhigh pressure extracting method of medium and small minute subconstiuent of biomaterial according to claim 1 and 2, it is characterized in that said solvent can be water, lipid, alcohols or other organic solvent, in raw material and solvent mixture, can add chemistry or biological products.
6. the superhigh pressure extracting method of medium and small minute subconstiuent of biomaterial according to claim 1 and 2 is characterized in that in the high pressure extraction process, can with heat or lower the temperature and carry out simultaneously.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021445907A CN1179775C (en) | 2001-12-30 | 2002-11-08 | Method for superhigh pressure extracting small molecule component from biomaterial |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN01138981.8 | 2001-12-30 | ||
| CN01138981 | 2001-12-30 | ||
| CN011389818 | 2001-12-30 | ||
| CNB021445907A CN1179775C (en) | 2001-12-30 | 2002-11-08 | Method for superhigh pressure extracting small molecule component from biomaterial |
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| CN1419947A CN1419947A (en) | 2003-05-28 |
| CN1179775C true CN1179775C (en) | 2004-12-15 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB021445907A Expired - Fee Related CN1179775C (en) | 2001-12-30 | 2002-11-08 | Method for superhigh pressure extracting small molecule component from biomaterial |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102441291A (en) * | 2011-12-01 | 2012-05-09 | 吉林省包装工程研究中心 | New method for extracting or purifying effective component of traditional Chinese medicine |
| CN104447925B (en) * | 2014-11-26 | 2016-10-26 | 湖北省农业科学院农产品加工与核农技术研究所 | A kind of method of cordycepin in hyperpressure extraction Cordyceps militaris rice medium |
| CN104694348A (en) * | 2015-03-19 | 2015-06-10 | 沈阳伊人宝生化制品有限公司 | Peruvian ginseng health wine |
| CN104921997B (en) * | 2015-06-23 | 2017-12-08 | 山东省分析测试中心 | The whitening of a kind of peony ultrahigh-pressure extraction method and its preparation, anti-oxidant Essence |
| CN105363241A (en) * | 2015-12-07 | 2016-03-02 | 江苏知原药业有限公司 | ultra-high pressure extraction apparatus for traditional Chinese medicines |
| CN108185430A (en) * | 2017-05-20 | 2018-06-22 | 郑毅男 | A kind of Fresh edible soybean effervesce piece preparation method |
| CN107929512B (en) * | 2017-11-23 | 2020-05-08 | 健民药业集团股份有限公司 | Method for preparing bone strengthening Longmu granules by adopting ultrahigh pressure extraction |
| CN108096073B (en) * | 2017-12-27 | 2020-12-25 | 北京昱美源科贸有限公司 | Production process and application of traditional Chinese medicine oil prepared from Umbelliferae medicinal materials of Umbelliferae |
| CN109289245A (en) * | 2018-11-08 | 2019-02-01 | 飞潮（无锡）过滤技术有限公司 | A kind of 700Mpa continous way high hydrostatic pressure extraction separator |
| CN110743193B (en) * | 2019-10-31 | 2021-06-22 | 南通科鑫超临界设备有限公司 | Ultrasonic-simulated high-speed separation supercritical extraction process |
| CN111423935B (en) * | 2020-04-22 | 2024-02-20 | 郑州市美宴食品有限公司 | Preparation method of sesame oil rich in medium-chain fatty acid, tocopherol and phytosterol |
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2002
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| CN1419947A (en) | 2003-05-28 |
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