CN105199116A - Starch nanoparticle sedimentation preparation method through treatment of starch water solution by adopting ultrasonic wave - Google Patents
Starch nanoparticle sedimentation preparation method through treatment of starch water solution by adopting ultrasonic wave Download PDFInfo
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- CN105199116A CN105199116A CN201510689780.XA CN201510689780A CN105199116A CN 105199116 A CN105199116 A CN 105199116A CN 201510689780 A CN201510689780 A CN 201510689780A CN 105199116 A CN105199116 A CN 105199116A
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Abstract
The invention relates to a starch nanoparticle sedimentation preparation method through treatment of starch water solution by adopting ultrasonic waves and belongs to the technical field of nano materials. The production efficiency of the prior art is lower, the production cost is higher and the product quality is not high. The starch nanoparticle sedimentation preparation method through treatment of starch water solution by adopting ultrasonic waves is characterized in that the method comprises the steps of dispersing starch in water and performing gelatinization at 60 to 100 DEG C to obtain starch water solution, wherein the starch concentration is 1 to 8g/100mL; treating the obtained starch water solution for 1 to 60min by using 100 to 600W ultrasonic waves generated by an ultrasonic generator to obtain low-viscosity starch water solution; dropping the obtained low-viscosity starch water solution in ethanol in ultrasonic oscillation, wherein the volume ratio of the starch water solution to the used ethanol is 1:(2-10), and continuously performing ultrasonic oscillation for 3 to 10min after dropping to complete sedimentation to obtain starch nanoparticle suspension; performing centrifugal separation to the obtained starch nanoparticle suspension, removing supernatant, washing sediments with ethanol, and then performing freeze-drying to obtain starch nanoparticles. The starch nanoparticle sedimentation preparation method through treatment of starch water solution by adopting ultrasonic waves is used for preparing various starch nanoparticles.
Description
Technical field
The present invention relates to a kind of starch nanometer granule particle sedimentation method adopting ultrasonication amidin, in advance ultrasonication is carried out to amidin, then through nanometer sedimentation, finally obtain starch nanometer granule, belong to technical field of nano material.
Technical background
Starch is the natural high molecular substance of occurring in nature rich reserves.Native starch is also referred to as ative starch, and it exists in the form of granules, and because crop varieties is different, the particle diameter of starch granules is between 2 ~ 100 μm.Carry out processing to ative starch and can obtain starch nanometer granule, so-called starch nanometer granule refers to that size is less than the starch molecule aggregate of 1000nm.Because starch has cheap and easy to get, nontoxic, the feature such as degradable, good biocompatibility, starch nanometer granule has very wide application prospect in a lot of fields, if as pharmaceutical carrier embedding medicinal, protein, nucleic acid, gene etc.; Use in emulsion as stablizer; As the composition being easy in microcapsule embedded food volatilize; Enhancing as matrix material is equal.
In existing starch nanometer granule preparation method, nanometer settling process is relevant with the present invention.Nanometer settling process is joined in non-solvent by starch solution, or joined in this starch solution by non-solvent, contacted with starch solution by non-solvent, makes starch molecule separate out at solvent/non-solvent interface and form particle.The shortcoming of the method is, obtain the starch nanometer granule compared with small particle size, the starch solution of high dilution and a large amount of non-solvents must be used, the concentration of such as amidin needs low to 1g/100mL, the volume of non-solvent need be 20 times of starch solution volume, therefore, production efficiency is lower, and production cost is higher; In addition, the excessive velocities that solvent and non-solvent exchange, the starch nanometer granule size distribution obtained is wider, and quality product is not high.
Summary of the invention
The object of the invention is to the deficiency overcoming existing nanometer settling process, say from method itself starch concentration improved starch solution, and then enhance productivity, reduce non-solvent consumption, and then reduce production cost; Obtain the less starch nanometer granule of particle diameter from product, and reduce particle size distribution range, thus improve the quality of products.For this reason, we have invented a kind of starch nanometer granule particle sedimentation method adopting ultrasonication amidin.
The starch nanometer granule particle sedimentation method of the employing ultrasonication amidin of the present invention is characterized in that:
(1) by starch dispersion in water, and gelatinization at 60 ~ 100 DEG C of temperature, obtain amidin, starch concentration is 1 ~ 8g/100mL;
(2) the ultrasonication 1 ~ 60min of the 100 ~ 600W produced with ultrasonic generator by gained amidin, obtains the low-viscosity starch aqueous solution;
(3) the gained low-viscosity starch aqueous solution is added drop-wise in the ethanol be in sonic oscillation, the volume ratio of amidin and ethanol used is 1:2 ~ 10, drip rear continuation sonic oscillation 3 ~ 10min, complete sedimentation, obtain starch nanometer granule suspension;
(4) by the centrifugation of gained starch nanometer granule suspension, removing supernatant liquor, throw out alcohol wash postlyophilization, obtains starch nanometer granule.
Its technique effect of the present invention is:
Adopt ultrasonication amidin, present invention obtains the starch nanometer granule less than prior art particle diameter, as waxy corn starch median size reaches 80.86nm, and narrow particle size distribution, as shown in Figure 1 and Figure 2, therefore quality product is improved.Meanwhile, the concentration of amidin significantly improves, and as brought up to 8g/100mL of the present invention from the 1g/100mL of prior art is the highest, this makes the production efficiency of the method for the present invention significantly improve; And the significantly minimizing of non-solvent consumption, as being minimumly reduced to 2 times from 20 times of prior art, this makes the production cost of the method for the present invention obviously reduce.
Accompanying drawing explanation
Fig. 1 adopts and the W-Gum nano particle diameter distribution plan not adopting ultrasonication amidin finally to obtain, and in figure, curve 1, curve 2 are adopt and the W-Gum nano particle diameter distribution curve not adopting ultrasonication amidin finally to obtain respectively.Fig. 2 adopts and the potato starch nano particle diameter distribution plan not adopting ultrasonication amidin finally to obtain, and this figure is simultaneously as Figure of abstract; In figure, curve 1, curve 2 are adopt and the potato starch nano particle diameter distribution curve not adopting ultrasonication amidin finally to obtain respectively.
Embodiment
(1) by starch dispersion in water, and gelatinization at 60 ~ 100 DEG C of temperature, obtain amidin, starch concentration is 1 ~ 8g/100mL; With stirring in described gelatinization process; Described starch is one of following starch, W-Gum, waxy corn starch, potato starch, amylose starch, pueraria starch, tapioca (flour), sweet potato starch, rice starch, wheat starch.
(2) the ultrasonication 1 ~ 60min of the 100 ~ 600W produced with ultrasonic generator by gained amidin, obtains the low-viscosity starch aqueous solution; In described ultrasonication process, amidin temperature is 40 DEG C.
(3) the gained low-viscosity starch aqueous solution is added drop-wise in the ethanol be in sonic oscillation, the volume ratio of amidin and ethanol used is 1:2 ~ 10, drip rear continuation sonic oscillation 3 ~ 10min, complete sedimentation, obtain starch nanometer granule suspension;
(4) by the centrifugation of gained starch nanometer granule suspension, removing supernatant liquor, throw out alcohol wash postlyophilization, obtains starch nanometer granule; The parameter of described centrifugation is, rotating speed 4000 ~ 6000r/min, time 3 ~ 5min; Described alcohol wash is ethanol purge; The median size of described starch nanometer granule is 80 ~ 230nm.
Embodiment 1:
Taking 3g W-Gum is dispersed in 100mL water, forms corn starch suspension; This corn starch suspension is stirred gelatinization 60min in boiling water bath, obtains the W-Gum aqueous solution that concentration is 3g/100mL.By the gained W-Gum aqueous solution at 40 DEG C, the ultrasonication 30min of the 100W produced with ultrasonic generator, obtains the low viscosity W-Gum aqueous solution.Be added drop-wise in the ethanol be in sonic oscillation by the gained low viscosity W-Gum aqueous solution, the volume ratio of the W-Gum aqueous solution and ethanol used is 1:5, drips rear continuation sonic oscillation 3min, completes sedimentation, obtain W-Gum nano granule suspension.By gained W-Gum nano granule suspension with 4000r/min rotating speed centrifugation 5min, removing supernatant liquor, throw out alcohol wash postlyophilization, obtains W-Gum nano particle; Detect through laser particle analyzer, gained W-Gum nano particle median size is 99.87nm, PDI (polydispersity coefficient) is 0.329, narrow diameter distribution, as shown in Figure 1.
Embodiment 2:
On embodiment 1 basis, when the concentration of the W-Gum aqueous solution is 5g/100mL, the median size of the W-Gum nano particle finally obtained is 133.4nm, PDI is 0.395.Visible, when amidin concentration improves, the particle diameter of starch nanometer granule increases.
Embodiment 3:
On embodiment 1 basis, when the concentration of the W-Gum aqueous solution is 8g/100mL, the median size of the W-Gum nano particle finally obtained is 229.6nm, PDI is 0.479.The checking further of this example, when amidin concentration improves, the particle diameter of starch nanometer granule increases.
Embodiment 4:
On embodiment 2 basis, the ultrasonication of the 300W produced with ultrasonic generator, the median size of the W-Gum nano particle finally obtained is 123.5nm, PDI is 0.457.Visible, when ultrasonication severe degree improves, the particle diameter of starch nanometer granule reduces.
Embodiment 5:
On embodiment 2 basis, the ultrasonication of the 600W produced with ultrasonic generator, the median size of the W-Gum nano particle finally obtained is 114.9nm, PDI is 0.405.The checking further of this example, when ultrasonic agitation severe degree improves, the particle diameter of starch nanometer granule reduces.
Embodiment 6:
On embodiment 2 basis, ultrasonication 15min, the median size of the W-Gum nano particle finally obtained is 159.0nm, PDI is 0.380.Visible, when the abundant degree of ultrasonication reduces, the particle diameter of starch nanometer granule increases.
Embodiment 7:
On embodiment 2 basis, ultrasonication 7min, the median size of the W-Gum nano particle finally obtained is 183.8nm, PDI is 0.403.The checking further of this example, when the abundant degree of ultrasonication reduces, the particle diameter of starch nanometer granule increases.
Embodiment 8:
On embodiment 2 basis, ultrasonication 2min, the median size of the W-Gum nano particle finally obtained is 205.9nm, PDI is 0.377.The same checking further of this example, when the abundant degree of ultrasonication reduces, the particle diameter of starch nanometer granule increases.
Embodiment 9:
On embodiment 2 basis, the volume ratio of the W-Gum aqueous solution and ethanol used is 1:3, and the median size of the W-Gum nano particle finally obtained is 133.3nm, PDI is 0.458.Visible, the reduction of non-solvent consumption, the change of size of starch nanometer granule is very little.
Embodiment 10:
On embodiment 9 basis, the volume ratio of the W-Gum aqueous solution and ethanol used is 1:10, and the median size of the W-Gum nano particle finally obtained is 126.9nm, PDI is 0.437.Visible, the increase of non-solvent consumption, can make the particle diameter of starch nanometer granule diminish equally.
Embodiment 11:
On embodiment 2 basis, starch adopts potato starch, and the median size of the potato starch nano particle finally obtained is 102.4nm, PDI is 0.331, and size distribution obviously narrows, as shown in Figure 2.Visible, the method for the present invention is used for potato starch with compared with W-Gum, in the particle diameter reducing starch nanometer granule and particle size distribution range, obtains better effect.
Embodiment 12:
On embodiment 2 basis, starch adopts waxy corn starch, and the median size of the waxy corn starch nano particle finally obtained is 80.86nm, PDI is 0.321.Visible, the method for the present invention is used for waxy corn starch with compared with W-Gum, in the particle diameter reducing starch nanometer granule, obtain beyond thought effect.
Embodiment 13:
On embodiment 2 basis, starch adopts amylose starch, and the median size of the amylose starch nano particle finally obtained is 175.98nm, PDI is 0.383.Visible, the method for the present invention is used for amylose starch, and the particle diameter of the starch nanometer granule of acquisition also within the acceptable range.
Claims (5)
1. adopt a starch nanometer granule particle sedimentation method for ultrasonication amidin, it is characterized in that:
(1) by starch dispersion in water, and gelatinization at 60 ~ 100 DEG C of temperature, obtain amidin, starch concentration is 1 ~ 8g/100mL;
(2) the ultrasonication 1 ~ 60min of the 100 ~ 600W produced with ultrasonic generator by gained amidin, obtains the low-viscosity starch aqueous solution;
(3) the gained low-viscosity starch aqueous solution is added drop-wise in the ethanol be in sonic oscillation, the volume ratio of amidin and ethanol used is 1:2 ~ 10, drip rear continuation sonic oscillation 3 ~ 10min, complete sedimentation, obtain starch nanometer granule suspension;
(4) by the centrifugation of gained starch nanometer granule suspension, removing supernatant liquor, throw out alcohol wash postlyophilization, obtains starch nanometer granule.
2. the starch nanometer granule particle sedimentation method of employing ultrasonication amidin according to claim 1, is characterized in that, with stirring in described gelatinization process.
3. the starch nanometer granule particle sedimentation method of employing ultrasonication amidin according to claim 1, it is characterized in that, described starch is one of following starch, W-Gum, waxy corn starch, potato starch, amylose starch, pueraria starch, tapioca (flour), sweet potato starch, rice starch, wheat starch.
4. the starch nanometer granule particle sedimentation method of employing ultrasonication amidin according to claim 1, its
Be characterised in that, in described ultrasonication process, amidin temperature is 40 DEG C.
5. the starch nanometer granule particle sedimentation method of employing ultrasonication amidin according to claim 1, is characterized in that, the parameter of described centrifugation is, rotating speed 4000 ~ 6000r/min, time 3 ~ 5min; Described alcohol wash is ethanol purge; The median size of described starch nanometer granule is 80 ~ 230nm.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106822040A (en) * | 2017-02-22 | 2017-06-13 | 青岛农业大学 | The preparation technology of starch hollow Nano particle and its application |
| CN108329533A (en) * | 2018-01-26 | 2018-07-27 | 江南大学 | A kind of preparation method of non-crosslinked type starch-beta-cyclodextrin composite nanometer particle |
| CN109293953A (en) * | 2018-09-17 | 2019-02-01 | 中南林业科技大学 | A kind of preparation method of alcohol precipitation nano-starch particle |
| CN109548949A (en) * | 2019-01-18 | 2019-04-02 | 宁波海通食品科技有限公司 | A kind of conditioning ice cream Ma Rice-cakes skin and preparation method thereof to extend the shelf life |
| CN111330728A (en) * | 2020-04-29 | 2020-06-26 | 广西大学 | Method for separating starch with different particle sizes by polyethylene glycol 200 solution gravity suspension |
| CN113621142A (en) * | 2021-08-02 | 2021-11-09 | 南京中医药大学 | Specific-morphology nano starch with efficient urea adsorption function and preparation method and application thereof |
| CN115739056A (en) * | 2022-11-23 | 2023-03-07 | 西北农林科技大学 | Nano material for separating polyphenol in plant extract, preparation method and application |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106822040A (en) * | 2017-02-22 | 2017-06-13 | 青岛农业大学 | The preparation technology of starch hollow Nano particle and its application |
| CN106822040B (en) * | 2017-02-22 | 2019-07-16 | 青岛农业大学 | The preparation process and its application of starch hollow Nano particle |
| CN108329533A (en) * | 2018-01-26 | 2018-07-27 | 江南大学 | A kind of preparation method of non-crosslinked type starch-beta-cyclodextrin composite nanometer particle |
| CN108329533B (en) * | 2018-01-26 | 2020-07-24 | 江南大学 | Preparation method of non-crosslinked starch- β -cyclodextrin composite nano-particles |
| CN109293953A (en) * | 2018-09-17 | 2019-02-01 | 中南林业科技大学 | A kind of preparation method of alcohol precipitation nano-starch particle |
| CN109548949A (en) * | 2019-01-18 | 2019-04-02 | 宁波海通食品科技有限公司 | A kind of conditioning ice cream Ma Rice-cakes skin and preparation method thereof to extend the shelf life |
| CN111330728A (en) * | 2020-04-29 | 2020-06-26 | 广西大学 | Method for separating starch with different particle sizes by polyethylene glycol 200 solution gravity suspension |
| CN111330728B (en) * | 2020-04-29 | 2021-06-08 | 广西大学 | Method for separating starch with different particle sizes by polyethylene glycol 200 solution gravity suspension |
| CN113621142A (en) * | 2021-08-02 | 2021-11-09 | 南京中医药大学 | Specific-morphology nano starch with efficient urea adsorption function and preparation method and application thereof |
| CN113621142B (en) * | 2021-08-02 | 2024-02-23 | 南京中医药大学 | Nano starch with specific morphology and high-efficiency urea adsorption function, and preparation method and application thereof |
| CN115739056A (en) * | 2022-11-23 | 2023-03-07 | 西北农林科技大学 | Nano material for separating polyphenol in plant extract, preparation method and application |
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