CN102965409B - 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
- Publication number
- CN102965409B CN102965409B CN201210513149.0A CN201210513149A CN102965409B CN 102965409 B CN102965409 B CN 102965409B CN 201210513149 A CN201210513149 A CN 201210513149A CN 102965409 B CN102965409 B CN 102965409B
- Authority
- CN
- China
- Prior art keywords
- starch
- enzyme
- nanocrystallines
- sugar
- minutes
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
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
Art
The present invention relates to one and utilize ultrasonic wave desmoenzyme process starch granules, starch granules is broken and enzymolysis is the method for β-amylose and nanometer starch crystal, belong to processing of farm products and nano structural material technical field.
Background technology
Nanotechnology is as a kind of emerge science technology most with market application potential, 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 achieve certain achievement in research.Starch has the feature of wide material sources, biodegradable, physiologically acceptable and low cost, is that the nanotechnology of raw material will become the study hotspot of the coming years with starch.
Starch is the storaging form of carbohydrate in green plants, is extensively present in various plant.Because it has price low, renewable cycle short, the advantage such as biological degradability good, density is little, become current 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 define the semicrystalline structure of starch granules.It has been generally acknowledged that amylopectin is the main component forming crystal region in starch granules, amylose starch then mainly defines amorphous regions.Amorphous regions structure comparison is loose, can to immerse by water and swelling, after carrying out mild hydrolysis with mineral acid to it, amorphous regions wherein substantially can be reacted and be generated the carbohydrate such as glucose, maltose, and the crystallizing field be not easily hydrolyzed then generates the nanometer starch crystal that degree of crystallinity is high, particle diameter is little.
In recent years, prepare the mode that nanometer starch crystal all adopts acidified starch particle, in hydrochloric acid catalysis system, obtained with the hydrolysis time of about 40 days the starch nano crystal grain that output is approximately 0.5% (massfraction).In addition foreign scholar prepares starch nano crystal grain by optimizing acidolysis condition, the sulfuric acid of 3.16mol/L is utilized to stir 5 days in 40 DEG C of silicon baths, by output increased to 15% (massfraction), and apply it to strengthen among natural rubber, thermoplastic starch and poly(lactic acid) and prepare nano composite material.
By the optimization of preparation technology, although the output of the nanometer starch crystal significantly improved, the high-concentration sulfuric acid used in production process; not only contaminate environment, increases production cost, and requires very high to production unit; be unfavorable for large-scale production, limit the further utilization of nanometer starch crystal.
The object of this invention is to provide a kind of employing physical method (ultrasonic wave, high-pressure homogeneous etc.) process starch, sugar (glucose is obtained respectively after enzymolysis, maltose, maltodextrin etc.) and the nanocrystalline efficient biological preparation method of environmental protection, take native starch as raw material, through ultrasonic destruction starch granules, then enzymolysis, amorphous domain enzymolysis is sugar, crystallizing field is not easily by enzymolysis, obtain nanocrystalline, the sodium hydroxide adding 4% in hydrolyzed solution goes out enzyme, centrifugal, it is the nanocrystalline of 50 ~ 800nm that pellet frozen drying obtains particle diameter, containing sugar in supernatant liquor, with dehydrated alcohol, sugar is separated, drying obtains finished product.
The present invention has the following advantages: 1. raw material sources are wide, safe, renewable; 2. simple to operate, be applicable to scale operation; 3. be applicable to General Instrument equipment, corrodibility is not had to equipment device face; 5. can obtain nanometer starch crystal and sugar, raw material availability is high simultaneously; 6. green production, product can relievedly eat.
Embodiment
The present invention is achieved like this, and preparation process method is:
(1) buffer preparation: preparation pH is the buffered soln of 4.2, stand-by.
(2) saccharifying enzyme pre-treatment: the activity first measuring saccharifying enzyme, then heats Glucoamylase Solution, makes it to activate, stand-by.
(3) prepare starch milk: added in damping fluid by 10% ~ 20% concentration by starch, and the saccharifying enzyme handled well is added wherein by the enzyme amount of 15 ~ 55U/g starch, stir.
(4) saccharification enzyme digestion reaction: by the starch milk enzyme mixation that stirs 50 ~ 65 DEG C of stirred in water bath 5 ~ 10 hours, the different amylorrhexis time is different.In reaction process, with microscopic examination starch granules pattern.
(5) ultrasonication: when crackle appears in basis of microscopic observation starch granules, uses ultrasonication reaction solution, and power setting, at 150 ~ 250W, processes 20 ~ 40 minutes, 1 ~ 2 second intermittent time, ultrasonication 1 ~ 2 second.
(6) amylorrhexis reaction: adjust ph to 6.5, adds amylase by 70 ~ 90U/g starch in above-mentioned solution, is adjusted to enzyme optimum temperuture 55 ~ 65 DEG C simultaneously, stirred in water bath 5 ~ 10 hours, and with microscope tracing observation starch granules pattern.
(7) high-pressure homogeneous process: when starch granules break completely until with microscopic examination less than starch granules and break lamella time, with high pressure homogenizer processing reaction liquid 30 ~ 60 minutes, leave standstill 1.5 ~ 2 hours.
(8) be separated: first by emulsion under 8000 ~ 10000r/min rotating speed centrifugal 10 ~ 20 minutes, the nanometer starch crystal of the precipitation obtained namely to be particle diameter after lyophilize process be 50 ~ 800nm, take out supernatant liquor, in supernatant liquor, add ethanol, the precipitation of precipitation is β-amylose (glucose, maltose, maltodextrin etc.) after drying.
Green natural, energy-efficient can be produced according to this step, be applicable to the nanometer starch crystal of suitability for industrialized production, this preparation method substantially increases raw material availability, do not use highly corrosive high toxicity pharmaceutical chemicals, the nanometer starch crystal produced can be applied 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 a kind of nanocrystalline method of ultrasonic wave desmoenzyme simultaneous extraction sugar and starch, but the present invention is not limited only to these examples.
Embodiment 1
Take 100g waxy corn starch, being placed on 1000mLpH is in the buffered soln of Sodium phosphate dibasic-citric acid of 4.6, add the saccharifying enzyme 1500U that pre-treatment is good, above-mentioned mixed solution being placed on temperature is stir 8 hours in 60 DEG C of water-baths, period observes starch granules every half an hour with 400 power microscopes, performs record.Then ultrasonication, setting model is: power 160w, 1.5 seconds intermittent times, 2 seconds treatment times, processes 20 minutes.Backward solution in add α-amylase 8000U, stir 8 hours under identical pH, uniform temp, take out reaction solution, high-pressure homogeneous 20 minutes, leave standstill half an hour, under 8000r/min rotating speed centrifugal 20 minutes, get supernatant liquor, in supernatant liquor, add dehydrated alcohol in 1:1 ratio, can find out there is Precipitation, be sugar (glucose, maltose, maltodextrin etc.).Get precipitation, after lyophilize, obtain the nanometer starch crystal that particle diameter is 50 ~ 300nm.
Embodiment 2
Take 100g pea starch, be placed in the citric acid-sodium citrate buffer that 1000mLpH is 4.8, add and activate saccharifying enzyme 2000U completely, be placed in 55 DEG C of water-baths after mixing, 10 hours are stirred with the speed of 100r/min, microscopic examination starch granules was used every 40 minutes, record, contrast in enzymolysis process.Then use ultrasonic generator process, arranging power is 200W, 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, stir 15 hours at the same temperature, high-pressure homogeneous 30 minutes afterwards, leave standstill 40 minutes, under 10000r/min rotating speed centrifugal 20 minutes.In supernatant liquor, add dehydrated alcohol in 1:1.5 ratio, have Precipitation, after filtration drying, obtain the β-amyloses such as glucose, maltose, maltodextrin.In precipitation, add acetone, in air dry oven, drying obtains particle diameter for 3 hours is 200 ~ 800nm nanometer starch crystal.
Embodiment 3
100g Starch rice is placed in the buffered soln that 1000mLpH is the Sodium phosphate dibasic-citric acid of 4.0, add mensuration enzyme to live and the saccharifying enzyme 2000U activated, mixing and being placed on temperature is stir 10 hours in the water-bath of 50 DEG C, and every 30 minutes patterns with microscopic examination starch granules, can find out that the slight crack of size inequality appears in starch particle surface, make a record.Use ultrasonication starch granules, utilize hyperacoustic cavatition, make starch granules broken further, the setting model of ultrasonic generator is: power 180W, 1 second intermittent time, in 2 seconds treatment times, processes 30 minutes.Process terminates rear regulator solution pH to neutral, raise water-bath temperature to 65 DEG C, α-amylase 10000U (dissimilar α-amylase is added in solution, quality is different), continue stirring 15 hours, use microscope tracing observation, can obviously see that starch granules diminishes, until disappear.Now with high pressure homogenizer process 30 minutes, leave standstill 1 hour, under 10000r/min rotating speed centrifugal 15 minutes.Get supernatant liquor, add dehydrated alcohol in the ratio of 1:1, now have Precipitation, filtration drying obtains sugar (glucose, maltose, maltodextrin etc.), quick taking-up precipitation, be placed in plate, obtaining particle diameter through lyophilize is 100 ~ 800nm nanometer starch crystal.
Physical method obtains the β-amylose such as nanometer starch crystal and glucose, maltose, maltodextrin in conjunction with biological enzyme, simple to operate, is easy to produce, high to raw material availability.Compare traditional preparation technology, this process low-carbon environmental protection, low production cost, the basis that the progress for nanosecond science and technology is from now on established.
Claims (3)
1. the method that ultrasonic wave desmoenzyme simultaneous extraction sugar and starch is nanocrystalline, is characterized in that, preparation process method is:
1) buffer preparation: preparation pH is the buffered soln of 4.2, stand-by;
2) saccharifying enzyme pre-treatment: the activity first measuring saccharifying enzyme, then heats Glucoamylase Solution, makes it to activate, stand-by;
3) prepare starch milk: added in damping fluid by 10% ~ 20% concentration by starch, and the saccharifying enzyme handled well is added wherein by the enzyme amount of 15 ~ 55U/g starch, stir;
4) saccharification enzyme digestion reaction: by the starch milk enzyme mixation that stirs 50 ~ 65 DEG C of stirred in water bath 5 ~ 10 hours, in reaction process, with microscopic examination starch granules pattern;
5) ultrasonication: when crackle appears in basis of microscopic observation starch granules, uses ultrasonication reaction solution, and power setting, at 150 ~ 250W, processes 20 ~ 40 minutes, 1 ~ 2 second intermittent time, ultrasonication 1 ~ 2 second;
6) amylorrhexis reaction: adjust ph to 6.5, adds α-amylase by 70 ~ 90U/g starch in above-mentioned solution, is adjusted to enzyme optimum temperuture 55 ~ 65 DEG C simultaneously, stirred in water bath 5 ~ 10 hours, and with microscope tracing observation starch granules pattern;
7) high-pressure homogeneous process: when starch granules break completely until with microscopic examination less than starch granules and break lamella time, with high pressure homogenizer processing reaction liquid 30 ~ 60 minutes, leave standstill 1.5 ~ 2 hours, obtain emulsion;
8) be separated: first by emulsion under 8000 ~ 10000r/min rotating speed centrifugal 10 ~ 20 minutes, the precipitation obtained is after lyophilize process, the nanometer starch crystal of to be namely particle diameter be 50 ~ 800nm, take out supernatant liquor, in supernatant liquor, add ethanol, the precipitation of precipitation is β-amylose after drying.
2. the method that a kind of ultrasonic wave desmoenzyme simultaneous extraction sugar and starch according to claim 1 is nanocrystalline, it is characterized in that, starch used is the mixture of a kind of in waxy corn starch, common corn starch, yam starch, sweet potato starch, pea starch, wheat starch, green starch, Starch rice or two kinds.
3. the method that a kind of ultrasonic wave desmoenzyme simultaneous extraction sugar and starch according to claim 1 is nanocrystalline, it is characterized in that, damping fluid is Lin acid hydrogen Er Na – citrate buffer solution, Ning Meng Suan – sodium citrate buffer solution, Yi Suan – sodium acetate buffer or phosphate buffered saline buffer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210513149.0A CN102965409B (en) | 2012-12-05 | 2012-12-05 | Environmental-friendly technology for synchronously extracting sugar and starch nanocrystallines by using enzymatic method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210513149.0A CN102965409B (en) | 2012-12-05 | 2012-12-05 | Environmental-friendly technology for synchronously extracting sugar and starch nanocrystallines by using enzymatic method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102965409A CN102965409A (en) | 2013-03-13 |
| CN102965409B true CN102965409B (en) | 2015-05-20 |
Family
ID=47795845
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210513149.0A Active CN102965409B (en) | 2012-12-05 | 2012-12-05 | Environmental-friendly technology for synchronously extracting sugar and starch nanocrystallines by using enzymatic method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102965409B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103435705B (en) * | 2013-08-14 | 2015-07-08 | 江南大学 | Method for preparing starch nanocrystal |
| 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 |
Citations (1)
| 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 |
-
2012
- 2012-12-05 CN CN201210513149.0A patent/CN102965409B/en active Active
Patent Citations (1)
| 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 |
|---|
| Preparation of nano-sized starch particles by complex formation with n-butanol;Jong-Yea Kim et al;《Carbohydrate Polymers》;20091231;第76卷;20091231 * |
| 大米纳米淀粉的超生法制备及载药性研究;胡爱军等;《粮食与饲料工业》;20111231(第8期);全文 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102965409A (en) | 2013-03-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Shen et al. | Succinic acid production from duckweed (Landoltia punctata) hydrolysate by batch fermentation of Actinobacillus succinogenes GXAS137 | |
| CN102433367B (en) | Preparation method of microporous starch having high specific surface area | |
| CN102965409B (en) | Environmental-friendly technology for synchronously extracting sugar and starch nanocrystallines by using enzymatic method | |
| CN103060400B (en) | Porous starch and joint preparation method for liquid glucose used for fermentation thereof | |
| CN106832435B (en) | A kind of processing method of lotus seed starch-lipid complex nano particle | |
| CA2710504A1 (en) | Process for producing saccharide | |
| CN105218248A (en) | A kind of preparation method of biological and ecological methods to prevent plant disease, pests, and erosion active liquid seaweed fertilizer | |
| CN104630311A (en) | Method for synchronously producing straw nano-cellulose and bacterial cellulose by using sweet sorghum | |
| CN102321704A (en) | Method for treating starchy raw material and method for preparing citric acid | |
| CN108095129B (en) | Method for preparing water-soluble dietary fibers of bran through fermentation | |
| CN103833862A (en) | Oxidized glutinous rice starch as well as preparation method and application thereof | |
| CN105348397B (en) | A kind of method that chemical bond enzyme process efficiently prepares thermostable type slow-digestion starch | |
| CN102234672A (en) | Enzymolysis method for starchy material and method for preparing citric acid | |
| CN103436573A (en) | Production method of biocatalytic efficient agricultural chitosan oligosaccharide | |
| CN105385748A (en) | Preparation method for fermentative production of marine peptides streptozotocin by using sea cucumber leftovers | |
| Zhang et al. | Bacterial cellulose synthesized with apple pomace enhanced by ionic liquid pretreatment | |
| CN106755179B (en) | A kind of culture medium suitable for bacteria cellulose fermentation | |
| Herawati et al. | Effect of autoclaving-cooling treatments on chemical characteristic and structure of tacca (Tacca leontopetaloides) starch | |
| CN109971798A (en) | A method of producing high concentration lactic acid | |
| CN102876757B (en) | Technique for preparing (FOs) feruloyl oligosaccharides by adopting two-period-type combined regulation fermentation technology | |
| CN104673767A (en) | Method for producing feruloyl esterase | |
| CN103343151B (en) | Preparation method of liquid medium for bacterial cellulose film | |
| CN113845600B (en) | Preparation method of high-amylose mung bean resistant starch | |
| Ylitervo | Production of ethanol and biomass from orange peel waste by Mucor indicus | |
| CN104450832A (en) | Technology for enzymatic efficient deacetylation and chitin degradation by using Thermophilic Bacillus |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |