CN102965409A - Environmental-friendly technology for synchronously extracting sugar and starch nanocrystallines by using enzymatic method - Google Patents
Environmental-friendly technology for synchronously extracting sugar and starch nanocrystallines by using enzymatic method Download PDFInfo
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- CN102965409A CN102965409A CN2012105131490A CN201210513149A CN102965409A CN 102965409 A CN102965409 A CN 102965409A CN 2012105131490 A CN2012105131490 A CN 2012105131490A CN 201210513149 A CN201210513149 A CN 201210513149A CN 102965409 A CN102965409 A CN 102965409A
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Abstract
The invention discloses an environmental-friendly technology for synchronously extracting sugar and starch nanocrystallines by using an enzymatic method. With natural starch as a raw material, starch milk with a certain concentration is prepared, starch particles are enzymatically decomposed by using the enzymatic method, then by means of physical means of ultrasonic waves, high pressure homogenization and the like, the starch particles are further crushed, and finally are enzymatically decomposed for a period of time, a reaction solution is centrifuged, absolute ethyl alcohol is dropwise added in supernate, starch sugar is separated out, and sediments are frozen and dried to obtain the starch nanocrystallines. The starch nanocrystallines prepared by adopting the technology can be used for overcoming the defects of environment pollution, low efficiency and low raw material utilization rate of the traditional acidified starch, and has the advantages of biological degradability and good compatibility, so as to be massively produced.
Description
Technical field
The present invention relates to a kind of ultrasonic wave desmoenzyme that utilizes and process starch granules, enzymolysis is the method for β-amylose and nanometer starch crystal to make starch granules break also, belongs to processing of farm products and nano structural material technical field.
Background technology
Nanotechnology is as a kind of emerge science technology that has the market application potential most, and its potential importance is unquestionable, and some developed countries drop into a large amount of funds and carry out scientific research.At home, many scientific research institutions, institution of higher learning also organize scientific research strength, carry out the research work of nanotechnology, and have obtained certain achievement in research.Starch has wide material sources, biodegradable, physiologically acceptable and characteristics cheaply, and the nanotechnology take starch as raw material will become the study hotspot of the coming years.
Starch is the storaging form of carbohydrate in green plants, extensively is present in the various plants.Because it has short, the advantage such as biological degradability good, density is little of low, renewable cycle of price, become present most study and most possibly become and prepare the raw-material natural polymer of degradable plastics.
Starch is the natural polymer with certain crystalline texture, and amylose starch wherein and amylopectin have formed the hypocrystalline structure of starch granules.It has been generally acknowledged that amylopectin is the main component that forms crystal region in the starch granules, amylose starch has then mainly formed amorphous regions.The unformed area domain structure is more open, can be immersed and swelling by water, after with mineral acid it being carried out mild hydrolysis, amorphous regions wherein can be reacted carbohydrates such as generating glucose, maltose basically, and the crystallizing field that is difficult for being hydrolyzed then generates degree of crystallinity height, nanometer starch crystal that particle diameter is little.
In recent years, the preparation nanometer starch crystal all adopts the mode of acidified starch particle, has made the starch nano crystal grain that output is approximately 0.5% (massfraction) with about 40 days hydrolysis time in the hydrochloric acid catalysis system.The foreign scholar prepares starch nano crystal grain by optimizing acidolysis condition in addition, utilize the sulfuric acid of 3.16mol/L in 40 ℃ of silicon are bathed, to stir 5 days, output increased to 15% (massfraction), and is applied it to and prepares nano composite material among strengthening natural rubber, thermoplastic starch and poly(lactic acid).
By preparation technology's optimization, although the output of the nanometer starch crystal that obviously improves, the high-concentration sulfuric acid that uses in the production process; not only contaminate environment increases production cost, and requires very high to production unit; be unfavorable for large-scale production, limited the further utilization of nanometer starch crystal.
The purpose of this invention is to provide a kind of employing physical method (ultrasonic wave, high-pressure homogeneous etc.) processing starch, behind enzymolysis, obtain respectively sugar (glucose, maltose, maltodextrin etc.) and the efficient biological preparation method of nanocrystalline environmental protection, take native starch as raw material, destroy starch granules through ultrasonic wave, then enzymolysis, the amorphous domain enzymolysis is sugar, crystallizing field is difficult for by enzymolysis, obtain nanocrystallinely, add 4% the sodium hydroxide enzyme that goes out in the hydrolyzed solution, centrifugal, it is the nanocrystalline of 50～800nm that the precipitation lyophilize obtains particle diameter, contain sugar in the supernatant liquor, with dehydrated alcohol with sugar from out, drying obtains finished product.
The present invention has the following advantages: 1. raw material sources are wide, safe, renewable; 2. simple to operate, be fit to scale operation; 3. be applicable to General Instrument equipment, equipment device face is not had corrodibility; 5. can obtain simultaneously nanometer starch crystal and sugar, raw material availability is high; 6. green production, product can relievedly eat.
Summary of the invention
The present invention is achieved like this, and the preparation process method is:
(1) buffer preparation: preparation pH is 4.2 buffered soln, and is stand-by;
(2) saccharifying enzyme pre-treatment: at first measure the activity of saccharifying enzyme, then heat Glucoamylase Solution, make it to activate, stand-by;
(3) preparation starch milk: starch is added in the damping fluid by 10%～20% concentration, and the enzyme amount of the saccharifying enzyme of handling well by 15～55 U/g starch added wherein, stir;
(4) saccharification enzyme digestion reaction: with the starch milk enzyme mixation that stirs in 50～65 ℃ of stirred in water bath 5～10 hours, different amylorrhexis asynchronism(-nization)s.In the reaction process, with microscopic examination starch granules pattern;
(5) ultrasonication: when crackle appears in microscopically observation starch granules, use the ultrasonication reaction solution, power setting was processed 20～40 minutes at 150～250W, 1～2 second intermittent time, ultrasonication 1～2 second;
(6) amylorrhexis reaction: regulate pH value to 6.5, by 70～90U/g starch adding amylase, be adjusted to simultaneously 55～65 ℃ of enzyme optimum temperutures in the mentioned solution, stirred in water bath 5～10 hours, and with microscope tracing observation starch granules pattern;
(7) high-pressure homogeneous processing: when starch granules break fully until with microscopic examination less than starch granules and when breaking lamella, with high pressure homogenizer processing reaction liquid 30～60 minutes, left standstill 1.5～2 hours;
(8) separate: at first with emulsion under 8000～10000r/min rotating speed centrifugal 10～20 minutes, the precipitation that obtains namely is that particle diameter is the nanometer starch crystal of 50～800nm after lyophilize is processed, take out supernatant liquor, add ethanol in supernatant liquor, the precipitation of separating out is β-amylose (glucose, maltose, maltodextrin etc.) after drying.
Can produce green natural, energy-efficient according to this step, the nanometer starch crystal that is fit to suitability for industrialized production, this preparation method has improved raw material availability greatly, do not use highly corrosive high toxicity pharmaceutical chemicals, the nanometer starch crystal of producing can be used in food, more can be applied to the slowly-releasing of medicine, also can be used for field of new.
Be described further below in conjunction with the invention of example to the nanocrystalline green technology of a kind of ultrasonic wave desmoenzyme simultaneous extraction sugar and starch, but the present invention is not limited only to these examples.
Embodiment 1
Take by weighing the 100g waxy corn starch, be placed on 1000mLpH and be in the buffered soln of Sodium phosphate dibasic-citric acid of 4.6, add the good saccharifying enzyme 1500U of pre-treatment, it is to stir 8 hours in 60 ℃ of water-baths that above-mentioned mixed solution is placed on temperature, observe starch granules every half an hour with 400 power microscopes during this time, perform record.Then ultrasonication, the condition of setting is: power 160w, 1.5 seconds intermittent times, in 2 seconds treatment times, processed 20 minutes.In solution, add α-amylase 8000U afterwards, under identical pH, uniform temp, stirred 8 hours, take out reaction solution, high-pressure homogeneous 20 minutes, leave standstill half an hour, under the 8000r/min rotating speed centrifugal 20 minutes, get supernatant liquor, add dehydrated alcohol in the 1:1 ratio in supernatant liquor, can find out has Precipitation, is sugar (glucose, maltose, maltodextrin etc.).Get precipitation, obtain the nanometer starch crystal that particle diameter is 50～300nm after the lyophilize.
Embodiment 2
Take by weighing the 100g pea starch, placing 1000mLpH is 4.8 citric acid-sodium citrate buffer, add and activate completely saccharifying enzyme 2000U, be placed on after mixing in 55 ℃ of water-baths, speed with 100r/min stirred 10 hours, used the microscopic examination starch granules every 40 minutes in the enzymolysis process, record, contrast.Then process with ultrasonic generator, it is 200W that power is set, and 1 second intermittent time, in 2 seconds treatment times, processes 30 minutes.Take out reaction solution, regulate pH to 6.0, add α-amylase 10000U, under uniform temp, stirred 15 hours, high-pressure homogeneous 30 minutes afterwards, left standstill under the 10000r/min rotating speed centrifugal 20 minutes 40 minutes.In supernatant liquor, add dehydrated alcohol in the 1:1.5 ratio, Precipitation is arranged, obtain the β-amyloses such as glucose, maltose, maltodextrin behind the filtration drying.Add acetone in precipitation, obtaining particle diameter in dry 3 hours in air dry oven is 200～800nm nanometer starch crystal.
Embodiment 3
It is the buffered soln of Sodium phosphate dibasic-citric acid of 4.0 that the 100g Starch rice is placed 1000mLpH, add and measure the saccharifying enzyme 2000U that enzyme is lived and activated, mixing and being placed on temperature is to stir 10 hours in 50 ℃ the water-bath, and every 30 minutes patterns with the microscopic examination starch granules, can find out that the uneven slight crack of size appears in starch particle surface, makes a record.Use the ultrasonication starch granules, utilize hyperacoustic cavatition, make starch granules further broken, the condition that arranges of ultrasonic generator is: power 180W, 1 second intermittent time, in 2 seconds treatment times, processed 30 minutes.Regulator solution pH was to neutral after processing finished, and rising water-bath temperature to 65 ℃ adds the dissimilar α-amylase of α-amylase 10000U(in solution, quality is different), continue to stir 15 hours, use the microscope tracing observation, can see obviously that starch granules diminishes, until disappear.Process 30 minute with high pressure homogenizer this moment, left standstill under the 10000r/min rotating speed centrifugal 15 minutes 1 hour.Get supernatant liquor, the ratio adding dehydrated alcohol in 1:1 has Precipitation this moment, filtration drying obtains sugar (glucose, maltose, maltodextrin etc.), take out fast precipitation, place plate, obtaining particle diameter through lyophilize is 100～800nm nanometer starch crystal.
Physical method makes the β-amyloses such as nanometer starch crystal and glucose, maltose, maltodextrin in conjunction with biological enzyme, simple to operate, is easy to produce, and is high to raw material availability.Compare traditional preparation technology, this process low-carbon environmental protection, low production cost, the basis of establishing for the from now on progress of nanosecond science and technology.
Claims (6)
1. nanocrystalline green technology of ultrasonic wave desmoenzyme simultaneous extraction sugar and starch, it is characterized in that: adopt the ative starch breast behind enzymolysis, ultrasonication, then through amylase enzymolysis, high-pressure homogeneous afterwards, enzymolysis for some time again, isolate at last supernatant liquor and precipitation, separate out sugar in the supernatant liquor with dehydrated alcohol, precipitation is dry behind lyophilize or washing with acetone, obtains nanometer starch crystal.
2. according to claim 1 method is characterized in that: used starch comprises waxy corn starch (waxy corn starch), conventional corn starch, yam starch, sweet potato starch, pea starch, wheat starch, green starch, Starch rice etc. (comprise both and both above mixture).
3. according to claim 1,2 method, it is characterized in that: damping fluid can be the Lin acid hydrogen Er Na – citrate buffer solution that can prepare the enzyme optimal pH, Ning Meng Suan – sodium citrate buffer solution, Yi Suan – sodium acetate buffer, phosphate buffered saline buffer etc.
4. according to claim 1,2,3 method, it is characterized in that: the manufacturer of saccharifying enzyme is different, production technique is different, its activity is also different, adopt the enzyme of 15～55 U/g starch to participate in reaction.
5. according to claim 1,2,3,4 method, it is characterized in that: the ultrasonication condition is that power setting was processed 20～40 minutes at 150～250W, 1～2 second intermittent time, ultrasonication 1～2 second.
6. according to claim 1,2,3,4,5 method, it is characterized in that: the production technique of α-amylase is different, the source is different, its activity is not quite similar, and add α-amylase by 70～90U/g starch.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103435705A (en) * | 2013-08-14 | 2013-12-11 | 江南大学 | Method for preparing starch nanocrystal |
| CN107446059A (en) * | 2016-05-31 | 2017-12-08 | 齐鲁工业大学 | A kind of short tube shape nanometer starch crystal and preparation method thereof |
| CN109260491A (en) * | 2018-08-13 | 2019-01-25 | 安徽启威生物科技有限公司 | A kind of preparation method of nano-starch eliminating smell agent |
| CN111019983A (en) * | 2019-12-27 | 2020-04-17 | 齐齐哈尔大学 | Preparation method of corn starch nanocrystal |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR100873015B1 (en) * | 2007-08-17 | 2008-12-09 | 고려대학교 산학협력단 | Methods for preparing nano-sized starch particle |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100873015B1 (en) * | 2007-08-17 | 2008-12-09 | 고려대학교 산학협력단 | Methods for preparing nano-sized starch particle |
Non-Patent Citations (2)
| Title |
|---|
| JONG-YEA KIM ET AL: "Preparation of nano-sized starch particles by complex formation with n-butanol", 《CARBOHYDRATE POLYMERS》, vol. 76, 31 December 2009 (2009-12-31), pages 20091231 * |
| 胡爱军等: "大米纳米淀粉的超生法制备及载药性研究", 《粮食与饲料工业》, no. 8, 31 December 2011 (2011-12-31) * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103435705A (en) * | 2013-08-14 | 2013-12-11 | 江南大学 | Method for preparing starch nanocrystal |
| CN103435705B (en) * | 2013-08-14 | 2015-07-08 | 江南大学 | Method for preparing starch nanocrystal |
| CN107446059A (en) * | 2016-05-31 | 2017-12-08 | 齐鲁工业大学 | A kind of short tube shape nanometer starch crystal and preparation method thereof |
| CN107446059B (en) * | 2016-05-31 | 2019-10-11 | 齐鲁工业大学 | A kind of short tube shape nanometer starch crystal and preparation method thereof |
| CN109260491A (en) * | 2018-08-13 | 2019-01-25 | 安徽启威生物科技有限公司 | A kind of preparation method of nano-starch eliminating smell agent |
| CN111019983A (en) * | 2019-12-27 | 2020-04-17 | 齐齐哈尔大学 | Preparation method of corn starch nanocrystal |
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