CN104785179A - Preparation method for starch nanospheres - Google Patents
Preparation method for starch nanospheres Download PDFInfo
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Abstract
The invention discloses a preparation method for starch nanospheres. The method comprises the following steps: (1) dissolving amylase in an alkaline solution, and stirring to obtain suspension; (2) completely freezing the suspension obtained in the step (1); (3) thawing a product obtained in the step (2), and obtaining a starch solution; (4) dialyzing the starch solution obtained in the step (3), and obtaining starch dispersion liquid; (5) filtering the starch dispersion liquid obtained in the step (4), and drying to obtain the starch nanospheres. The preparation method is energy-saving, environment-friendly and simple to operate, and a process is easy to control; the preparation method only adopts a general chemical reagent and simple experimental equipment, can realize large-scale production and is easy for industrialized promotion; the starch nanospheres prepared with the method are high in purity, and the starch structure is not changed; the starch nanospheres prepared with the method are controllable in particle size and uniform in particle size distribution, can be stably dispersed in water, and can be used for biomedical carriers and food additives.
Description
Technical field
The present invention relates to a kind of preparation method of arch nanospheres, belong to nano material and field of nanometer technology.
Background technology
Nanometer technology refers in several technology of observing atom, molecule, handle and processing in the range scale of hundreds of nanometer.Research finds, material there occurs many peculiar physical and chemical changes on nanoscale.Except the change occurred in optical, electrical, thermal and magnetic characteristic, nano material also has many new features such as radiation, absorption, catalysis, sterilization, absorption, thus brings breakthrough change to people's life.Nanosecond science and technology have been applied to a lot of field such as electronics, materialogy, biology.
The polysaccharide polymer compound that starch is made up of glucose, having straight chain and side chain two kinds of structures, be extensively present in the seed of plant, block root and fruit, is a kind of abundance, cheap renewable biological source.Arch nanospheres has good characteristic, as large in specific area, absorption and chemism is strong, biocompatibility and biological degradability is good, nontoxic and non-immunogenicity, stable storage etc.As absorption carrier and the embedding medium of medicament, pigment, spices etc., arch nanospheres can be applicable to the field (AntonioG.B.Pereiraa such as biological medicine, agricultural chemicals, food, weaving and daily-use chemical industry, Andr é R.Fajardoa, Samara Nocchi, et al.Starch-based microspheres forsustained-release of curcumin:Preparation and cytotoxic effect on tumor cells, Carbohydrate Polymers 2013; 98:711-720.) (Asha Rodrigues, Martins Emeje.Recentapplications of starch derivatives in nanodrug delivery.Carbohydrate Polymers 2012; 87:987-994.) (Wei Gao, Baoyong Sha, Wei Zou, et al.Cationic amylose-encaps ulated bovinehemoglo bin as a nanosized oxygen carrier.Biomaterials 2011; 32:9425-9433.).Wherein, arch nanospheres is mainly used at field of medicaments: the control delivery of (1) multi-medicament.Some drugs is only at specific conditioned disjunction specific position its pharmacotoxicological effect of competence exertion, and the various enzymes simultaneously again in easy digested system decompose and reduce drug effect.Arch nanospheres then can avoid medicine to be subject to the decomposition of enzyme, as the carrier of medicine, and can the speed of effective Drug controlled release; (2) as a kind of immuno analytical method of routine, antigen, antibody and protein and to play in whole cell quantitative is acted on.Owing to there being more hydroxyl in starch molecule, make it have stronger hydrophily, little to nonspecific protein adsorption quantity, therefore can be used as novel markings thing carrier widely; (3) interventional therapy of some difficult disease or diagnosis.Because arch nanospheres is more much smaller than erythrocytic diameter (6 ~ 9 μm), can moves freely in blood, therefore may be injected into each position of human body, check pathology and treat.
The preparation method of spherex mainly comprises: (the LidiaElfstrand such as Physical, chemical method, enzymatic isolation method and reverse microemulsion process, Ann-Charlotte Eliasson, Monica Jonsson, et al.From starch to starchmicrospheres:factors controlling the microspheres quality.Starch/Starke 2006; 58:381-390.) (Li Qing, Lin Hua .CN 101215385 B, 2010.06.23) (.CN104004134 A, 2014.08.27 such as Ma Sude, Min Zhonghua).Physical mainly with ball mill or air blast by various Starch Micronization, have that the cycle is long, particle diameter is large, particle is uneven and the shortcoming such as roundness is poor.Chemical method mainly hydrolyzed starch under acid or alkaline conditions, its hydrolytic process is wayward, and with dextrin, maltose or G/W hydrolysis products, product yield is low.Reverse microemulsion process reaction condition is gentle, and various influence factor is easy to control, and reaction favorable reproducibility, is prepare the most frequently used method of spherex, but can uses the toxic reagents such as toluene, chloroform or POCl3, pollute the biological nature of ative starch.
Summary of the invention
An object of the present invention is to provide a kind of preparation method of arch nanospheres, the arch nanospheres size tunable utilizing the method to prepare and being evenly distributed, can in water the stable dispersion several months do not condense, environmental protection simple to operate, reaction condition is gentle, result favorable reproducibility.
The preparation method of arch nanospheres provided by the invention, comprises the steps:
(1) amylose is dissolved in aqueous slkali, stirs to obtain suspension;
(2) suspension that obtains of freezing step (1) is to completely icing;
(3) product that obtains of thawing step (2), obtains starch solution;
(4) starch solution that step (3) of dialysing obtains, obtains starch dispersion liquid;
(5) starch dispersion liquid that obtains of filtration step (4), can obtain described arch nanospheres after drying.
Above-mentioned preparation method, in step (1), described amylose can be any one in potato amylose, maize amylose or Rice Amylose, and the molecular weight of described amylose can be 40K ~ 340K;
Described in every 0.1g ~ 0.5g, amylose is dissolved in aqueous slkali described in 10mL, specifically can be amylose described in every 0.1g or every 0.5g and is dissolved in aqueous slkali described in 10mL;
The molar concentration of described aqueous slkali can be 0.1 ~ 0.4mol/L, specifically can be 0.1 ~ 0.25mol/L, 0.25 ~ 0.4mol/L, 0.1mol/L, 0.25mol/L or 0.4mol/L;
Described alkali can be any one in lithium hydroxide, NaOH and potassium hydroxide.
Above-mentioned preparation method, in step (1), the time of described stirring can be 30 ~ 60min, specifically can be 30min or 60min; Rotating speed can be 300 ~ 600rpm, specifically can be 400rpm.
Above-mentioned preparation method, in step (2), described freezing temperature can be-8 DEG C ~-10 DEG C, specifically can be-8 DEG C or-10 DEG C; Time can be 40min ~ 60min, specifically can be 40min or 60min.
Above-mentioned preparation method, in step (3), described thawing can be carried out at normal temperatures and pressures.
Above-mentioned preparation method, in step (4), described dialysis, for described starch solution is placed in bag filter, is carried out in ultra-pure water; Often water can be changed once by 8h ~ 12h, specifically often water can be changed once by 8h or 12h; Dialysis time is 7 ~ 9 days, specifically can be 7 days or 9 days;
The intercepting molecular weight of described bag filter can be 3500 ~ 14000, specifically can be 3500,7000 or 14000; Material can be cellulose acetate or regenerated cellulose.
Above-mentioned preparation method, in step (5), adopts aperture to be the membrane filtration 1 ~ 10 time of 0.22 μm ~ 0.45 μm, aperture specifically can be adopted to be the filter membrane of 0.22 μm or 0.45 μm, filter 1 ~ 5 time, 5 ~ 10 times, 1 time, 5 times or 10 times;
The material of described filter membrane is nylon, cellulose acetate or polytetrafluoroethylene (PTFE).
The arch nanospheres structure that the present invention prepares keeps complete, and purity is high, the hydrodynamic radius (R in water
h) be 60 ~ 370nm, the particle diameter of the arch nanospheres under drying regime is 40 ~ 355nm, size tunable, even particle size distribution, and in water, Absorbable organic halogens dispersion reaches 4 months.
Compared with prior art, the present invention has the following advantages:
(1) preparation method's energy-conserving and environment-protective of the present invention, simple to operate, and process is easy to control.
(2) the present invention only adopts general chemistry reagent and simple experiment equipment, can scale, is easy to industrialization promotion.
(3) the arch nanospheres product purity for preparing of the present invention is high, and starch structure does not change.
(4) arch nanospheres for preparing of the present invention, size tunable, even particle size distribution, can in water stable dispersion, can be used for biological medicine carrier and food additives.
Accompanying drawing explanation
Fig. 1 be in embodiment 1 starch material (RAA) and arch nanospheres (RLA1) at the contrast photo of aqueous dispersion, wherein Fig. 1 (a) is the dispersion liquid just obtained, Fig. 1 (b) is for leaving standstill the dispersion liquid after 4 months, left figure in Fig. 1 (a) and Fig. 1 (b) is the photo of starch material (RAA), and right figure is the photo of arch nanospheres (RLA1).
Fig. 2 is SEM (SEM) photo that the particle diameter prepared in embodiment 3 is about the arch nanospheres of 250nm.
Fig. 3 is the grain size distribution adding up the arch nanospheres obtained according to Fig. 2.
Fig. 4 is infrared spectrum (IR) comparison diagram of amylose raw material and arch nanospheres in embodiment 3, wherein, Fig. 4 (a) is the infrared spectrogram of amylose raw material, infrared spectrum (IR) figure that Fig. 4 (b) is nanometer amylose microballoon.
Fig. 5 is photoelectron spectroscopy (XPS) comparison diagram of amylose raw material and arch nanospheres in embodiment 3, wherein, photoelectron spectroscopy (XPS) figure that photoelectron spectroscopy (XPS) figure that Fig. 5 (a) is amylose raw material, Fig. 5 (b) are nanometer amylose microballoon.
Fig. 6 is X-ray diffraction (XRD) comparison diagram of amylose raw material and arch nanospheres in embodiment 3, wherein, X-ray diffraction (XRD) figure that Fig. 6 (a) is amylose raw material, X-ray diffraction (XRD) figure that spectrogram (b) is nanometer amylose microballoon.
Detailed description of the invention
The experimental technique used in following embodiment if no special instructions, is conventional method.
Material used in following embodiment, reagent etc., if no special instructions, all can obtain from commercial channels.
The preparation of arch nanospheres in embodiment 1, LiOH solution
(1) 0.1g maize amylose (is purchased from Sigma Aldrich, molecular weight 40 ~ 340K) join in the sample bottle of the LiOH solution filling 10mL 0.25mol/L, the starch suspension that under normal temperature and pressure, 400rpm constant speed magnetic agitation 30min uniformly disperses.
(2) above-mentioned starch suspension is put into freezer compartment of refrigerator and leave standstill 40min to completely icing, the design temperature of freezer compartment of refrigerator is-10 DEG C.
(3) taken out from freezer compartment of refrigerator by the pre-freeze sample of step (2) gained, normal temperature and pressure rests on experimental bench and melts completely to it, obtains the starch solution of transparent clarification.
(4) by the starch solution dislocation of step (3) gained in intercepting molecular weight be in the cellulose acetate bag filter of 3500, in ultra-pure water, every 12h changes water once, dialyse 7 days, removing hydroxyl and lithium ion etc., obtain homodisperse micro-blue starch suspension.
(5) by the product dislocation syringe of step (4) gained, the nylon leaching film in 0.22 μm of aperture was pushed respectively through 1 time, namely the arch nanospheres of stable dispersion in water is obtained, arch nanospheres is obtained through vacuum freeze drying (temperature :-50 DEG C, pressure: 10Pa).
Hydrodynamic radius (the R of the arch nanospheres prepared in the present embodiment in water
h) ≈ 168nm, particle diameter ≈ 160nm under drying regime, even particle size distribution.
The preparation of arch nanospheres in embodiment 2, KOH solution
(1) 0.1g Rice Amylose (is purchased from Sigma Aldrich, molecular weight 40 ~ 340K) join in the sample bottle of the KOH solution filling 10mL 0.25mol/L, the starch suspension that under normal temperature and pressure, 400rpm constant speed magnetic agitation 60min uniformly disperses.
(2) above-mentioned starch suspension is put into freezer compartment of refrigerator and leave standstill 60min to completely icing, the design temperature of freezer compartment of refrigerator is-10 DEG C.
(3) taken out from freezer compartment of refrigerator by the pre-freeze sample of step (2) gained, normal temperature and pressure rests on experimental bench and melts completely to it, obtains the starch solution of transparent clarification.
(4) by the starch solution dislocation of step (3) gained in intercepting molecular weight be in the cellulose acetate bag filter of 3500, in ultra-pure water, every 12h changes water once, dialyse 7 days, removing hydroxyl and potassium ion etc., obtain homodisperse micro-blue starch suspension.
(5) by the product dislocation syringe of step (4) gained, the nylon leaching film in 0.22 μm of aperture was pushed respectively through 1 time, namely the arch nanospheres of stable dispersion in water is obtained, arch nanospheres is obtained through vacuum freeze drying (temperature :-50 DEG C, pressure: 10Pa).
Hydrodynamic radius (the R of the arch nanospheres prepared in the present embodiment in water
h) ≈ 345nm, particle diameter ≈ 330nm under drying regime, even particle size distribution.
The preparation of arch nanospheres in the NaOH solution of embodiment 3,0.25mol/L
(1) 0.1g potato amylose (is purchased from Sigma Aldrich, molecular weight 40 ~ 340K) join in the sample bottle of the NaOH solution filling 10mL 0.25mol/L, the starch suspension that under normal temperature and pressure, 400rpm constant speed magnetic agitation 30min uniformly disperses.
(2) above-mentioned suspension is put into freezer compartment of refrigerator and leave standstill 40mim to completely icing, the design temperature of freezer compartment of refrigerator is-10 DEG C.
(3) the pre-freeze sample of step (2) gained is taken out from freezer compartment of refrigerator, rest under normal temperature and pressure on experimental bench and melt completely to it, obtain the starch solution of transparent clarification.
(4) by the starch solution dislocation of step (3) gained in intercepting molecular weight be in the bag filter of 3500, in ultra-pure water, every 12h changes water once, dialyses 7 days, remove hydroxyl and sodium ion etc., obtain homodisperse micro-blue starch suspension.
(5) by the product dislocation syringe of step (4) gained, the nylon leaching film in 0.22 μm of aperture was pushed respectively through 1 time, namely the arch nanospheres of stable dispersion in water is obtained, arch nanospheres is obtained through vacuum freeze drying (temperature :-50 DEG C, pressure: 10Pa).
By the hydrodynamic radius (R of arch nanospheres in water prepared in the present embodiment
h) ≈ 230nm, particle diameter ≈ 250nm under drying regime, even particle size distribution.
The preparation of arch nanospheres in the NaOH solution of embodiment 4,0.1mol/L
(1) 0.1g potato amylose (is purchased from Sigma Aldrich, molecular weight 40 ~ 340K) join in the sample bottle of the NaOH solution filling 10mL 0.1mol/L, the starch suspension that under normal temperature and pressure, 400rpm constant speed magnetic agitation 30min uniformly disperses.
(2) above-mentioned suspension is put into freezer compartment of refrigerator and leave standstill 40mim to completely icing, the design temperature of freezer compartment of refrigerator is-8 DEG C.
(3) the pre-freeze sample of step (2) gained is taken out from freezer compartment of refrigerator, rest under normal temperature and pressure on experimental bench and melt completely to it, obtain the starch solution of transparent clarification.
(4) by the starch solution dislocation of step (3) gained in intercepting molecular weight be in the bag filter of 14000, in ultra-pure water, every 12h changes water once, dialyses 7 days, remove hydroxyl and sodium ion etc., obtain homodisperse micro-blue starch suspension.
(5) by the product dislocation syringe of step (4) gained, the nylon leaching film in 0.45 μm of aperture was pushed through 1 time, namely size tunable epigranular is obtained, the arch nanospheres of stable dispersion in water, arch nanospheres is obtained through vacuum freeze drying (temperature :-50 DEG C, pressure: 10Pa).
Hydrodynamic radius (the R of the arch nanospheres that the present embodiment prepares in water
h) scope is 370nm, under drying regime, particle size range is 355nm, even particle size distribution.
The preparation of arch nanospheres in the NaOH solution of embodiment 5,0.4mol/L
(1) 0.5g potato amylose (is purchased from Sigma Aldrich, molecular weight 40 ~ 340K) join in the sample bottle of the NaOH solution filling 10mL 0.4mol/L, the starch suspension that under normal temperature and pressure, 400rpm constant speed magnetic agitation 60min uniformly disperses;
(2) above-mentioned suspension is put into freezer compartment of refrigerator and leave standstill 60mim to completely icing, the design temperature of freezer compartment of refrigerator is-10 DEG C;
(3) the pre-freeze sample of step (2) gained is taken out from freezer compartment of refrigerator, rest under normal temperature and pressure on experimental bench and melt completely to it, obtain the starch solution of transparent clarification;
(4) by the starch solution dislocation of step (3) gained in intercepting molecular weight be in the bag filter of 7000, in ultra-pure water, every 8h changes water once, dialyses 9 days, remove hydroxyl and sodium ion etc., obtain homodisperse micro-blue starch suspension;
(5) by the product dislocation syringe of step (4) gained, the nylon leaching film in 0.45 μm of aperture was pushed through 1 time, namely size tunable epigranular is obtained, stabilized scattering nano spherex in water, arch nanospheres is obtained through vacuum freeze drying (temperature :-50 DEG C, pressure: 10Pa).
Hydrodynamic radius (the R of the arch nanospheres prepared in the present embodiment in water
h) scope is 145nm, under drying regime, particle size range is 130nm, even particle size distribution.
Arch nanospheres is prepared in embodiment 6,5 filtrations
(1) 0.1g potato amylose (is purchased from Sigma Aldrich, molecular weight 40 ~ 340K) join in the sample bottle of the NaOH solution filling 10mL 0.25mol/L, the starch suspension that under normal temperature and pressure, 400rpm constant speed magnetic agitation 30min uniformly disperses.
(2) above-mentioned suspension is put into freezer compartment of refrigerator and leave standstill 40mim to completely icing, the design temperature of freezer compartment of refrigerator is-10 DEG C.
(3) the pre-freeze sample of step (2) gained is taken out from freezer compartment of refrigerator, rest under normal temperature and pressure on experimental bench and melt completely to it, obtain the starch solution of transparent clarification.
(4) by the starch solution dislocation of step (3) gained in intercepting molecular weight be in the bag filter of 3500, in ultra-pure water, every 12h changes water once, dialyses 7 days, remove hydroxyl and sodium ion etc., obtain homodisperse micro-blue starch suspension.
(5) by the product dislocation syringe of step (4) gained, the nylon leaching film in 0.22 μm of aperture was pushed respectively through 5 times, namely the arch nanospheres of stable dispersion in water is obtained, arch nanospheres is obtained through vacuum freeze drying (temperature :-50 DEG C, pressure: 10Pa).
By the hydrodynamic radius (R of arch nanospheres in water prepared in the present embodiment
h) ≈ 120nm, particle diameter ≈ 110nm under drying regime, even particle size distribution.
Arch nanospheres is prepared in embodiment 7,10 filtrations
(1) 0.1g potato amylose (is purchased from Sigma Aldrich, molecular weight 40 ~ 340K) join in the sample bottle of the NaOH solution filling 10mL 0.25mol/L, the starch suspension that under normal temperature and pressure, 400rpm constant speed magnetic agitation 30min uniformly disperses.
(2) above-mentioned suspension is put into freezer compartment of refrigerator and leave standstill 40mim to completely icing, the design temperature of freezer compartment of refrigerator is-10 DEG C.
(3) the pre-freeze sample of step (2) gained is taken out from freezer compartment of refrigerator, rest under normal temperature and pressure on experimental bench and melt completely to it, obtain the starch solution of transparent clarification.
(4) by the starch solution dislocation of step (3) gained in intercepting molecular weight be in the bag filter of 3500, in ultra-pure water, every 12h changes water once, dialyses 7 days, remove hydroxyl and sodium ion etc., obtain homodisperse micro-blue starch suspension.
(5) by the product dislocation syringe of step (4) gained, the nylon leaching film in 0.22 μm of aperture was pushed respectively through 10 times, namely the arch nanospheres of stable dispersion in water is obtained, arch nanospheres is obtained through vacuum freeze drying (temperature :-50 DEG C, pressure: 10Pa).
By the hydrodynamic radius (R of arch nanospheres in water prepared in the present embodiment
h) ≈ 60nm, particle diameter ≈ 40nm under drying regime, even particle size distribution.
The test of embodiment 8, starch nano-microsphere characterizes
(1) stability of arch nanospheres
After dispersion liquid before drying in step (5) in embodiment 1 is at room temperature left standstill 4 months, arch nanospheres of the present invention still can in water stable dispersion, as shown in photo in Fig. 1.Therefore, the arch nanospheres (RLA1) that the present invention prepares can in water stable dispersion, arch nanospheres the present invention prepared is dispersed in water, and can reach same effect.
(2) form of arch nanospheres
As can be seen from Fig. 2 stereoscan photograph, the pattern of the arch nanospheres that embodiment 3 prepares is the ball of Edge divider, and even particle size distribution, particle size concentrates on about 250nm, as shown in Figure 3.The pattern of the arch nanospheres prepared in other embodiment and embodiment 3, without significant difference, are the arch nanospheres of Edge divider, even particle size distribution, and difference is only that particle size is different.
(3) structural characterization of starch nano-microsphere
The infrared spectrum of A, starch and arch nanospheres
The infrared spectrum comparison diagram of arch nanospheres that Fig. 4 is embodiment 3 Raw starch and prepares, the major absorbance peak of comparison diagram 4 (a) and Fig. 4 (b) IR spectrogram can be found out, arch nanospheres does not cause the change of ative starch characteristic group, illustrates that nano-starch structure keeps complete.In other embodiment, the infrared spectrum of starch and arch nanospheres and Fig. 4 are without substantive difference, and characteristic group does not all change.Therefore, the arch nanospheres structure that the present invention prepares keeps complete.
The XPS spectrum figure of B, starch and arch nanospheres
The XPS spectrum figure comparison diagram of arch nanospheres that Fig. 5 is embodiment 3 Raw starch and prepares, in comparison diagram 5, (a) and (b) XPS spectrum figure can find out, arch nanospheres does not introduce new element, illustrates that nano-starch purity is high, is not polluted.In other embodiment, XPS spectrum figure and Fig. 4 of starch and arch nanospheres is without substantive difference, does not all introduce new element.Therefore, the arch nanospheres that the present invention prepares is not polluted, and purity is high.
The XRD spectra of C, starch and arch nanospheres
The XRD spectra comparison diagram of arch nanospheres that Fig. 6 is embodiment 3 Raw starch and prepares, in comparison diagram 6, the Rayleigh diffraction maximum of (a) and (b) XRD spectra can be found out, stronger diffraction maximum is there is in arch nanospheres at 6.4 °, 17.0 °, 22.4 ° and 23.8 ° of places, its crystal formation is Type B, illustrate that the degree of crystallinity of arch nanospheres improves, regularity strengthens, and mechanical performance improves.In other embodiment, XPS spectrum figure and Fig. 4 of starch and arch nanospheres is without substantive difference, and all occur stronger diffraction maximum at 5.8 °, 17.0 °, 22.4 ° and 23.8 ° of places, crystal formation is also Type B.Therefore, the arch nanospheres degree of crystallinity that the present invention prepares improves, and regularity strengthens, and mechanical performance improves.
Claims (7)
1. a preparation method for arch nanospheres, comprises the steps:
(1) amylose is dissolved in aqueous slkali, stirs to obtain suspension;
(2) suspension that obtains of freezing step (1) is to completely icing;
(3) product that obtains of thawing step (2), obtains starch solution;
(4) starch solution that step (3) of dialysing obtains, obtains starch dispersion liquid;
(5) starch dispersion liquid that obtains of filtration step (4), can obtain described arch nanospheres after drying.
2. preparation method according to claim 1, it is characterized in that: in step (1), described amylose is any one in potato amylose, maize amylose and Rice Amylose, and the molecular weight of described amylose is 40K ~ 340K;
Described in every 0.1g ~ 0.5g, amylose is dissolved in aqueous slkali described in 10mL, and the molar concentration of described aqueous slkali is 0.1 ~ 0.4mol/L;
Described alkali is any one in lithium hydroxide, NaOH and potassium hydroxide.
3. preparation method according to claim 1 and 2, is characterized in that: in step (1), and the time of described stirring is 30 ~ 60min, and rotating speed is 300 ~ 600rpm.
4. the preparation method according to any one of claim 1-3, is characterized in that: in step (2), and described freezing temperature is-8 DEG C ~-10 DEG C, and the time is 40 ~ 60min.
5. the preparation method according to any one of claim 1-4, is characterized in that: in step (3), described thawing is carried out at normal temperatures and pressures.
6. the preparation method according to any one of claim 1-5, is characterized in that: in step (4), and described dialysis, for described starch solution is placed in bag filter, is carried out in ultra-pure water, and every 6h ~ 12h changes water once, dialyses 7 ~ 9 days;
The intercepting molecular weight of described bag filter is 3500 ~ 14000, and material is cellulose acetate or regenerated cellulose.
7. the preparation method according to any one of claim 1-6, it is characterized in that: in step (5), adopt aperture to be the membrane filtration 1 ~ 10 time of 0.22 μm ~ 0.45 μm, the material of described filter membrane is nylon, cellulose acetate or polytetrafluoroethylene (PTFE).
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Cited By (6)
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| CN107375244A (en) * | 2017-09-12 | 2017-11-24 | 吉林大学珠海学院 | A kind of nanoscale docetaxel and preparation method thereof |
| CN109293954A (en) * | 2018-09-17 | 2019-02-01 | 中南林业科技大学 | A kind of method that biological enzyme combination alkali Refrigeration Technique prepares nano-starch particle |
| WO2019037743A1 (en) * | 2017-08-22 | 2019-02-28 | 中国石油化工股份有限公司 | Starch-containing microsphere and preparation method therefor and application thereof |
| CN109422817A (en) * | 2017-08-22 | 2019-03-05 | 中国石油化工股份有限公司 | A kind of micron-level crosslinked spherex and its preparation method and application |
| CN110960508A (en) * | 2019-11-13 | 2020-04-07 | 湖北大学 | Starch nano-particle with protein adsorption resistance and targeting capability and preparation method thereof |
| CN113912870A (en) * | 2021-11-12 | 2022-01-11 | 重庆联佰博超医疗器械有限公司 | Starch modification method and application |
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2015
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| ZHE ZHANG ET.AL.: ""Facile preparation of corn starch nanoparticles by alkali-freezing treatment"", 《THE ROYAL SOCIETY OF CHEMISTRY》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019037743A1 (en) * | 2017-08-22 | 2019-02-28 | 中国石油化工股份有限公司 | Starch-containing microsphere and preparation method therefor and application thereof |
| CN109422817A (en) * | 2017-08-22 | 2019-03-05 | 中国石油化工股份有限公司 | A kind of micron-level crosslinked spherex and its preparation method and application |
| CN109422817B (en) * | 2017-08-22 | 2020-11-06 | 中国石油化工股份有限公司 | Micron-sized crosslinked starch microspheres and preparation method and application thereof |
| US11891458B2 (en) | 2017-08-22 | 2024-02-06 | China Petroleum & Chemical Corporation | Starch-containing microsphere and preparation method and use thereof |
| CN107375244A (en) * | 2017-09-12 | 2017-11-24 | 吉林大学珠海学院 | A kind of nanoscale docetaxel and preparation method thereof |
| CN109293954A (en) * | 2018-09-17 | 2019-02-01 | 中南林业科技大学 | A kind of method that biological enzyme combination alkali Refrigeration Technique prepares nano-starch particle |
| CN110960508A (en) * | 2019-11-13 | 2020-04-07 | 湖北大学 | Starch nano-particle with protein adsorption resistance and targeting capability and preparation method thereof |
| CN110960508B (en) * | 2019-11-13 | 2021-11-23 | 湖北大学 | Starch nano-particle with protein adsorption resistance and targeting capability and preparation method thereof |
| CN113912870A (en) * | 2021-11-12 | 2022-01-11 | 重庆联佰博超医疗器械有限公司 | Starch modification method and application |
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