CN103382226A - Preparation method and application for octyl succinic anhydride modified starch micro nanometer particles of same category - Google Patents
Preparation method and application for octyl succinic anhydride modified starch micro nanometer particles of same category Download PDFInfo
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Abstract
A preparation method and an application for octyl succinic anhydride modified starch micro nano particles of the same category belong to the technical field of particle emulsifiers. The preparation method includes conducting acid degradation on native starch to obtain starch micro nano particles, then utilizing octyl succinic anhydride (OSA) to conduct hydrophobic modification on the starch micro nano particles to obtain the octyl succinic anhydride modified starch micro nano particles. The average diameter of the starch micro nano particles obtained through the acid degradation is between 30nm and 1mum. The OSA modified starch micro nano particles can serve as an emulsifier for preparing emulsion with high stability, or serve as a foam stabilizer for stabilizing the emulsifier, and especially can serve as an emulsifier for food, cosmetics and biological medicine.
Description
Technical field
The present invention relates to preparation and the application of starch micro-nano particle emulsifying agent, specially refer to the purposes that octyl group succinyl oxide treated starch micro-nano particle emulsifying agent is used in food, makeup and biological medicine, belong to particle emulsifying agent technical field.
Background technology
Emulsion with the preparation of particle emulsifying agent is again the Pickering emulsion, and it is found in 1907 by Pickering first.Emulsifying agent with routines such as tensio-active agent and protein is compared, and this particle emulsifying agent has following characteristics (1) and intercepted the Ostwald maturing process fully, and this is that the bubble/drop of emulsion and foam becomes large major cause; (2) permanent stability are high; (3) complicated hierarchy is the desirable presoma of constructing novel material; (4) unique rheological characteristics (Tcholakova, S., Denkov, N. D., Lips, A., Comparison of solid particles, globular proteins and surfactants as emulsifiers,
Phys. Chem. Chem. Phys.2008,1608-1627).In addition, bibliographical information is also arranged, and it is compared with the emulsion that small-molecular emulsifier forms, and the active substance that this emulsion coats has better transdermal characteristic.These features make it in fields such as food, makeup, medicine and novel materials, great application prospect be arranged.
Along with the development of nanosecond science and technology, some micro-nano particles as: the emulsifying property of silica, calcium carbonate, clay and emulsification mechanism have obtained comparatively systematic research.The particle that natural polymer forms also can be used for emulsifying agent.Report recently the micro-gel particles emulsifying agent that the derivatived cellulose original position forms, can obtain the emulsion of super stable.Also there is report to utilize virus to form particle as efficient emulsifying agent.But the particle emulsifying agent in overwhelming majority's research is not edible, and therefore the application at field of food is restricted.
Starch is second largest natural polymer of occurring in nature content, and is cheap and easy to get.The starch of some hydrophobically modifieds has been used as emulsifying agent and has been used for the fields such as food, makeup, as: S. Tesh, Ch. Gerhards, H. Schubert. Stabilization of emulsions by OSA starches.
Journal of Food Engineering, 2002,54,167-174; R. Chanamai, D.J. McClements, Comparison of Gum Arabic, Modified Starch, and whey protein isolate as emulsifiers:Influence of pH, CaCl
2And Temperature,
Journal of Food Science, 2002,67,120-125. but these treated starches are as emulsifying agent, be all that treated starch is dissolved in aqueous phase, treated starch is adsorbed on oil/water termination and stable emulsion with molecular conformation, rather than is adsorbed on oil/water termination and stable emulsion with particle form.The nearest hydrophobically modified starch granules that studies show that can be used as particle emulsifying agent stable emulsion (M. Rayner, A. Timgren, M. Sj, P. Dejmek, Quinoa starch granules:a candidate for stabilising food-grade Pickering emulsions
J. Sci. Food Agric.2012,92,1841-1847; A. Yusoff, B. S. Murray, Modified starch granules as particle-stabilizers of oil-in-water emulsions,
Food hydrocolloids,2011,25,42-55).But the size of these starch granuless too large (mean sizes〉1mm), the emulsion droplet that therefore obtains is larger, and stability of emulsion is relatively poor.
Can obtain nano level starch crystal by acid degradation starch, the size of these nanocrystals is at 40-100nm.These starch nano crystal as emulsifying agent can prepare stable emulsion (C. Li, P. Sun, C. Yang, Emulsion stabilized by starch nanocrystals,
Starch/St rke, 2012,64,497-502). but these nanometer starch crystals are due to a large amount of negative charges, so under low pH value and high salt concentration, emulsion is extremely unstable.The present invention carries out hydrophobically modified by the starch micro-nano particle that the acidolysis to ative starch obtains, obtained the starch micro-nano particle emulsifying agent of excellent emulsifying property, can be used for field of food replace amphiphilic starch molecule emulsifying agent, based on the emulsifying agent of protein (as casein etc.) or other emulsifying agent (as glyceryl monostearate or bi-tristearin), octyl group succinyl oxide treated starch micro-nano particle emulsifying agent of the present invention also can be used for emulsifying agent or the suds-stabilizing agent in makeup.
Summary of the invention
Purpose of the present invention: prepare the starch micro-nano particle by the acid degradation ative starch, and with the octyl group succinyl oxide, it is carried out hydrophobically modified, and prepare high stability emulsion used as the particle emulsifying agent.
Technical scheme of the present invention: the preparation method of a class octyl group succinyl oxide treated starch micro-nano particle, its preparation process is:
(1) starch granules falls preparation starch micro-nano particle by acid: take 10.0g starch and join in the round-bottomed flask that fills 100mL, 1-5mol/L acid solution, flask is put into the oil bath pan of 40 ℃, 100 to turn/the speed uniform stirring of min, react after 1-10 days, with reaction product repeatedly centrifugal washing until become neutral, with high-shear homogenizer, the insoluble product that obtains is dispersed in water, forms the starch micro-nano particle dispersion liquid of stable uniform; Perhaps will be repeatedly product vacuum-drying after centrifugal washing obtain the starch micro-nano particle;
Described starch is a kind of of waxy corn starch, W-Gum, yam starch, tapioca (flour), wheat starch, Starch rice; Described acid is a kind of of sulfuric acid, hydrochloric acid, nitric acid;
By acidolysis ative starch particle, obtain the starch micro-nano particle, its mean diameter is between 30nm-1 μ m, between preferred average diameter 50-300nm.
(2) with the octyl group succinyl oxide, this starch micro-nano particle is carried out hydrophobically modified again: the aqueous dispersions that the starch micro-nano particle of step (1) gained is mixed with 0.01-50wt% concentration, be preferably 0.1-20wt%, and adjusting pH is 6-10, then progressively drip a certain amount of octyl group succinyl oxide OSA with the dehydrated alcohol dilution, the OSA addition is 0.001-0.3 times of starch micro-nano particle weight, be preferably 0.01-0.1 doubly, be controlled in 1-5h and add, after reaction finishes, HCI solution with 0.1M transfers to pH value 6.5 with system, use respectively ethanol, water washing, wash away responseless octyl group succinyl oxide, get OSA treated starch micro-nano particle after vacuum-drying.
The octyl group succinyl oxide treated starch micro-nano particle of preparation obtains with the octyl group succinyl oxide, this starch micro-nano particle to be carried out hydrophobically modified again after the starch micro-nano particle by the ative starch particle by acid degradation and gets.
The application of prepared octyl group succinyl oxide treated starch micro-nano particle, be used for food, makeup or medicament, comprise emulsion or for emulsion form, as the particle emulsifying agent, or be used for the purposes of stable foam as suds-stabilizing agent with described octyl group succinyl oxide treated starch micro-nano particle.
Beneficial effect of the present invention: the present invention obtains the starch micro-nano particle by the acid degradation ative starch, and with the octyl group succinyl oxide, this starch micro-nano particle is carried out hydrophobically modified.This octyl group succinyl oxide treated starch micro-nano particle can directly prepare high stability emulsion and foam as the particle emulsifying agent, and these emulsions have excellent acidproof and salt resistant character.The emulsion of same tensio-active agent, polymer, protein stabilization is compared, and the stable emulsion of this treated starch micro-nano particle has higher stability.Octyl group succinyl oxide treated starch micro-nano particle emulsifying agent of the present invention can be widely used in emulsion and the suds-stabilizing agent of food, makeup and biological medicine.
Description of drawings
The stereoscan photograph of Fig. 1 octyl group succinyl oxide treated starch micro-nano particle.
The infrared spectrogram of Fig. 2 unmodified starch micro-nano particle and octyl group succinyl oxide treated starch micro-nano particle.
The O/W emulsion photo (placing for two weeks) (treated starch micro-nano particle concentration is respectively 0.02wt% from left to right, 0.05wt%, 0.1wt%, 0.5wt%, 1.0wt%) that Fig. 3 octyl group succinyl oxide treated starch micro-nano particle is stable.
The microphotograph (concentration is respectively 0.02wt%, 1.0wt% from left to right) of the O/W emulsion that Fig. 4 octyl group succinyl oxide treated starch micro-nano particle is stable.
The scanning electron microscope (SEM) photograph of the emulsion that Fig. 5 octyl group succinyl oxide treated starch micro-nano particle is stable.
The lower stable emulsion (pH is respectively 2.19,3.43,4.40,5.47,6.38 from left to right) of unmodified starch micro-nano particle of the different pH values of Fig. 6.
The lower stable emulsion (pH is respectively 2.37,3.31,4.13,5.10,6.36 from left to right) of octyl group succinyl oxide treated starch micro-nano particle of the different pH values of Fig. 7.
The stable emulsion of unmodified starch micro-nano particle under the different salt concn of Fig. 8 (NaCl concentration is respectively 0,50 from left to right, and 100,150,200,300,500 mM).
The stable emulsion of octyl group succinyl oxide treated starch micro-nano particle under the different salt concn of Fig. 9 (NaCl concentration is respectively 0,50 from left to right, and 100,150,200,300,500 mM).
Embodiment
The invention will be further elaborated for following example.
Embodiment 1:
Taking the 10.0g waxy corn starch joins and fills 100mL, 3.16mol/L H
2SO
4In the round-bottomed flask of solution, flask is put into the oil bath pan of 40 ℃, with the speed uniform stirring of 100 r/min.React after 6 days, the centrifugal collecting precipitation product, and with its repeatedly centrifugal washing until become neutral postlyophilization to get the starch micro-nano particle.
The micro-nano starch granules of 1g gained is mixed with the aqueous dispersions of 20wt% concentration, and to regulate pH be 9.5, then progressively be added dropwise to the 0.03g octyl group succinyl oxide (OSA) with the dilution of 2mL dehydrated alcohol, be controlled in 5h and add.After reaction finishes, with the HCI solution of 0.1M, system is transferred to pH value 6.5, use respectively ethanol, water washing, wash away responseless acid anhydrides, must octyl group succinyl oxide treated starch micro-nano particle after vacuum-drying.
Pattern and the particle size determination of octyl group succinyl oxide treated starch micro-nano particle: the treated starch micro-nano particle is dispersed in water, drawing drop with suction pipe drips on copper mesh, observe the microscopic pattern of sample after the water volatilization with scanning electron microscope (S-4800, Hitachi, Japan).Operating voltage is 1.0KV.Fig. 1 is the stereoscan photograph of octyl group succinyl oxide treated starch micro-nano particle.Can see having the starch nanometer granule of many 40～100nm Uniform Dispersion to come, their shapes differ, and mostly are Polygons, but all are more or less the same on size.
The infrared spectra of modification and unmodified starch micro-nano particle is measured by Bruker Vector 22 infrared spectras (Bruker Co., Germany).Fig. 2 is unmodified and the infrared spectrogram treated starch micro-nano particle, as can be seen from Figure 2 compares with unmodified starch micro-nano particle, and the infrared spectrogram of OSA treated starch micro-nano particle is at 1724 cm
-1With 1572 cm
-1New ester carbonyl group characteristic peak has appearred in the place, has proved that octenyl succinic acid anhydride has been grafted on the starch micro-nano particle.
Emulsifying property test: a certain amount of OSA modification or unmodified starch micro-nano particle are dispersed in water, being mixed with concentration is 1wt% starch granules dispersion liquid, be 1:1 preparation emulsion by whiteruss and water volume ratio, utilize clarifixator to carry out homogeneous 2min (5000 r/ min) to emulsion.The emulsion photo is taken by the OLYMPUS digital camera, and the emulsion Photomicrograph is taken by the digital opticmicroscope of VHX-1000 (Keyence Int. Trading Co. Ltd., Japan).
Fig. 3 is with the stable O/W emulsion photo of OSA treated starch micro-nano particle (placing for two weeks), can see that what form take OSA treated starch micro-nano particle as emulsifying agent is O/W type emulsion, and stability is high.This is because starch granules has stronger wetting ability, therefore easily forms O/W type emulsion.Fig. 4 is the Photomicrograph with the stable O/W emulsion of OSA treated starch micro-nano particle, can see that emulsion particle is circular, be increased to 1.0wt % with treated starch micro-nano particle concentration from 0.02wt %, the mean sizes of emulsion particle is reduced to about 14 μ m from 37 μ m.
Fig. 5 is the scanning electron microscope (SEM) photograph of the stable emulsion of OSA treated starch micro-nano particle, can see clearly that from figure OSA treated starch micro-nano particle is adsorbed on emulsion interface stability emulsion, this is different from the stable emulsion of hydrophobically modified starch molecule, above their emulsion droplet surface smoothing is just looked at and is adsorbed on less than particle.This illustrates the stable by the treated starch micro-nano particle really of emulsion, rather than stable by starch molecule.
Fig. 6 is the stable emulsion of unmodified starch micro-nano particle under different pH values.Can see under low pH value, the less stable of emulsion, easy breakdown of emulsion, this is that the starch micro-nano particle is easily assembled due to the electronegative conductively-closed under low pH value of unmodified starch micro-nano particle, causes emulsion unstable.Fig. 7 is the stable emulsion of OSA treated starch micro-nano particle under different pH values.Can see that emulsion all has good stability under wider pH value, the starch micro-nano particle after this explanation OSA modification has improved greatly than the resistance to acid of unmodified starch micro-nano particle.Fig. 8 is the stable emulsion of unmodified starch micro-nano particle under different salt concn.Can see under high salt concn, the less stable of emulsion, easy breakdown of emulsion, this is also that the starch micro-nano particle is easily assembled, and causes emulsion unstable due to the electronegative conductively-closed of unmodified starch micro-nano particle under high ion concentration.Fig. 9 is the stable emulsion of OSA treated starch micro-nano particle under different salt concn.Can see that under high salt concn, emulsion still has good stability, the starch micro-nano particle after this explanation modification has improved greatly than the salt resistance of unmodified starch micro-nano particle.
Embodiment 2:
Taking the 10.0g wheat starch joins and fills 100mL, 3.16mol/L H
2SO
4In the round-bottomed flask of solution, flask is put into the oil bath pan of 40 ℃, with the speed uniform stirring of 100 r/min.React after 6 days, the centrifugal collecting precipitation product, and with its repeatedly centrifugal washing until become neutral postlyophilization to get the starch micro-nano particle.
The starch micro-nano particle of 1g gained is mixed with the aqueous dispersions of 20wt % concentration, and to regulate pH be 9.5, then be added dropwise to the 0.03g octyl group succinyl oxide (OSA) of 2mL dehydrated alcohol dilution, be controlled in 5h and add.After reaction finishes, with the HCI solution of 0.1M, system is transferred to pH value 6.5, use respectively ethanol, water washing, wash away responseless acid anhydrides, must octyl group succinyl oxide treated starch micro-nano particle after vacuum-drying.
Embodiment 3:
Take the 10.0g Starch rice and join in the round-bottomed flask that fills 100mL, 3.16mol/L HCl solution, flask is put into the oil bath pan of 40 ℃, with the speed uniform stirring of 100 r/min.React after 6 days, the centrifugal collecting precipitation product, and with its repeatedly centrifugal washing until become neutral postlyophilization to get the starch micro-nano particle.
The starch micro-nano particle of 1g gained is mixed with the aqueous dispersions of 15wt % concentration, and to regulate pH be 9, then be added dropwise to the 0.06g octyl group succinyl oxide (OSA) of 2mL dehydrated alcohol dilution, be controlled in 5h and add.After reaction finishes, with the HCI solution of 0.1M, system is transferred to pH value 6.5, use respectively ethanol, water washing, wash away responseless acid anhydrides, must octyl group succinyl oxide treated starch micro-nano particle after vacuum-drying.
Claims (4)
1. the preparation method of a class octyl group succinyl oxide treated starch micro-nano particle is characterized in that preparation process is:
(1) starch granules falls preparation starch micro-nano particle by acid: take 10.0g starch and join in the round-bottomed flask that fills 100mL, 1-5mol/L acid solution, flask is put into the oil bath pan of 40 ℃, 100 to turn/the speed uniform stirring of min, react after 1-10 days, with reaction product repeatedly centrifugal washing until become neutral, with high-shear homogenizer, the insoluble product that obtains is dispersed in water, forms the starch micro-nano particle dispersion liquid of stable uniform; Perhaps will be repeatedly product vacuum-drying after centrifugal washing obtain the starch micro-nano particle;
Described starch is a kind of of waxy corn starch, W-Gum, yam starch, tapioca (flour), wheat starch, Starch rice; Described acid is a kind of of sulfuric acid, hydrochloric acid, nitric acid;
Starch micro-nano particle mean diameter is between 30nm-1 μ m;
(2) with the octyl group succinyl oxide, this starch micro-nano particle is carried out hydrophobically modified again: the aqueous dispersions that the starch micro-nano particle of step (1) gained is mixed with 0.01-50wt% concentration, and adjusting pH is 6-10, then progressively drip a certain amount of octyl group succinyl oxide OSA with the dehydrated alcohol dilution, the OSA addition is 0.001-0.3 times of starch micro-nano particle weight, be controlled in 1-5h and add, after reaction finishes, HCI solution with 0.1M transfers to pH value 6.5 with system, use respectively ethanol, water washing, wash away responseless octyl group succinyl oxide, get OSA treated starch micro-nano particle after vacuum-drying.
2. the preparation method of octyl group succinyl oxide treated starch micro-nano particle according to claim 1 is characterized in that in preparation process (2), the starch micro-nano particle being mixed with the aqueous dispersions of 0.1-20wt% concentration; The OSA addition is 0.01-0.1 times of starch micro-nano particle weight.
3. octyl group succinyl oxide treated starch micro-nano particle with the preparation of the described method of claim 1 is characterized in that obtaining with the octyl group succinyl oxide, this starch micro-nano particle to be carried out hydrophobically modified again after the starch micro-nano particle by the ative starch particle by acid degradation gets.
4. use the application of the octyl group succinyl oxide treated starch micro-nano particle of the described method preparation of claim 1, it is characterized in that for food, makeup or medicament, comprise emulsion or be emulsion form, as the particle emulsifying agent, or be used for the purposes of stable foam as suds-stabilizing agent with described octyl group succinyl oxide treated starch micro-nano particle.
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Cited By (4)
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| CN104546539A (en) * | 2014-12-03 | 2015-04-29 | 华南理工大学 | Moisturizing cream containing superfine starch grains and preparation method of moisturizing cream |
| CN110869395A (en) * | 2017-05-16 | 2020-03-06 | 嘉吉公司 | Articles containing starch conversion materials |
| CN111053181A (en) * | 2019-11-13 | 2020-04-24 | 河南农业大学 | Preparation method and application of food pickering emulsion for delaying lipid oxidation |
| CN114044942A (en) * | 2021-11-24 | 2022-02-15 | 湖北人福药用辅料股份有限公司 | Modified starch capsule shell and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104546539A (en) * | 2014-12-03 | 2015-04-29 | 华南理工大学 | Moisturizing cream containing superfine starch grains and preparation method of moisturizing cream |
| CN104546539B (en) * | 2014-12-03 | 2017-10-20 | 华南理工大学 | One kind is containing fine starch granules moisturiser and preparation method thereof |
| CN110869395A (en) * | 2017-05-16 | 2020-03-06 | 嘉吉公司 | Articles containing starch conversion materials |
| US11441017B2 (en) | 2017-05-16 | 2022-09-13 | Cargill, Incorporated | Article of manufacture containing a starch-converted material |
| CN111053181A (en) * | 2019-11-13 | 2020-04-24 | 河南农业大学 | Preparation method and application of food pickering emulsion for delaying lipid oxidation |
| CN111053181B (en) * | 2019-11-13 | 2022-06-21 | 河南农业大学 | Preparation method and application of food pickering emulsion for delaying lipid oxidation |
| CN114044942A (en) * | 2021-11-24 | 2022-02-15 | 湖北人福药用辅料股份有限公司 | Modified starch capsule shell and preparation method thereof |
| CN114044942B (en) * | 2021-11-24 | 2023-02-10 | 湖北人福药用辅料股份有限公司 | Modified starch capsule shell and preparation method thereof |
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Application publication date: 20131106 |