CN102008926B - Method for preparing starch microspheres - Google Patents
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- CN102008926B CN102008926B CN 201010546156 CN201010546156A CN102008926B CN 102008926 B CN102008926 B CN 102008926B CN 201010546156 CN201010546156 CN 201010546156 CN 201010546156 A CN201010546156 A CN 201010546156A CN 102008926 B CN102008926 B CN 102008926B
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Abstract
The invention discloses a method for preparing starch microspheres, which comprises the following steps of: stirring 20 to 70 percent of plant starch emulsion at the constant temperature in the critical temperature of starch gelatinization for 10 to 30 minutes under the action of 2 to 15 percent of water-soluble thickening agent, standing, cooling naturally, removing supernate, washing, and drying to prepare the starch microspheres. The surfaces of the prepared starch microspheres are smooth, the inner part is hollow, one or more nano-scale micropores are distributed on the surface, the wall thickness is uniform, the grain diameter is between 10 and 100 micrometers, and the wall thickness is between 1 and 10 micrometers. The prepared starch microspheres have a simple preparation process and readily available materials, and are widely applied to fields of medicines, cosmetics, food modifiers, printing ink, papermaking and the like.
Description
Technical field
The present invention relates to a kind of carrier spherex, be specifically related to a kind of preparation method of spherex.
Background technology
Carrier spherex in the prior art, mostly be the micropore starch microballoon, its surface presents cellular, micropore is covered with whole starch particle surface and is goed deep into to the center by the surface, as pharmaceutical carrier, can control the slow release speed of medicine, but along with the preparation method need not, with the slow release effect that directly causes spherex as carrier.
At present the preparation method about spherex mainly contains enzymatic isolation method, its preparation technology be ative starch under suitable pH value scope enzymolysis, centrifugal, wash, take off enzyme, drying and other steps, obtain the porous-starch microballoon.The influence factor of the micropore starch of enzymatic isolation method preparation is more, will cause the variation of micropore rate larger such as too high or too low pH value; In addition, the particle size of ative starch all directly has influence on the aperture degree of depth and the density of starch, thereby has directly affected the slow release effect of spherex as carrier.
Acid hydrolyzation is as another preparation method of spherex, and its principle is to utilize the weak acid resistance of the intrinsic amorphous area of starch granules, under uniform temperature and hydrochloric acid strong effect, hydrolysis from outward appearance to inner essence occurs and form micropore starch at amorphous area.Because the randomness of starch amorphous area, the micropore of hydrolysis is not of uniform size, and is deep mixed, disperses inhomogeneously, and this has also directly affected the slow release effect of spherex as carrier.
Summary of the invention
The technical problem to be solved in the present invention is that a kind of preparation technology is provided comparatively easy preparation method.
The technical solution used in the present invention is as follows;
A kind of preparation method of spherex may further comprise the steps:
1. plant amylum is mixed with water, the preparation mass percentage concentration is 20～70% plant amylum emulsion;
2. thickener is mixed with water, under 1000～5000 rev/mins speed of agitator, be warming up to 40～80 ℃, the preparation mass percentage concentration is 2～15% thickener soln;
3. adjust thickener soln temperature to 50～65 ℃, under 1000～5000 rev/mins speed of agitator, slowly be added to the plant amylum emulsion in the thickener soln, after the plant amylum emulsion adds, adjust temperature to 65～80 ℃, constant temperature stirred 10～30 minutes, leave standstill, naturally supernatant is abandoned in cooling, washing, drying.
The plant amylum emulsion concentration of step in 1. is preferably 30～50%.
The plant amylum of step in 1. is one or more in tapioca, sweet potato starch, farina, Chinese yam starch, Rhizoma Nelumbinis starch or the pueraria starch.
The thickener of step in 2. is one or more in cyclodextrin, xanthans, agar, sodium alginate, sodium carboxymethylcellulose or the hydroxypropyl methylcellulose.
Thickener can also be selected one or more in polyvinyl alcohol, polyvinylpyrrolidone, polyacrylic acid or the polyacrylamide.
The preparation method of spherex disclosed by the invention, be with the plant amylum emulsion under the effect of water-soluble thickener, in stirring with the gelatinization critical-temperature by force with the molecular melting of starch, take thickener as nuclear, starch molecule again crystallization as spherical state, owing to the thickener dehydration in the spheroid core forms the spheroidal cavity, the spherex particle size of preparation is different because of starch gelatinization temperature, straight chain molecule ratio and thickener concentration when dry.
In the technical solution of the present invention, the effect of preparation plant amylum emulsion mainly is to make starch be easy to flow, and convenient interpolation operation, and when concentration was lower than 20%, starch emulsion was rarer, was unfavorable for the control of production cost; When concentration was higher than 70%, starch emulsion was thicker, was unfavorable for adding operation.It is 30～50% ideal that technical solution of the present invention plant amylum emulsion concentration is preferably.
Among the preparation method for spherex, the control stir speed (S.S.) is 1000～5000 rev/mins of conditions that are absolutely necessary, and mixing speed is excessively low, will cause the balling-up effect undesirable, and in the situation of obtain solution than thickness, will cause stirring ineffective.
According to the kind of prepared spherex, plant amylum is selected one or more any combination in tapioca, sweet potato starch, farina, Chinese yam starch, Rhizoma Nelumbinis starch or the pueraria starch.
During preparation edible kind of starch microballoon, thickener should be selected one or more any combination in foodstuff or food-grade class cyclodextrin, xanthans, agar, sodium alginate, sodium carboxymethylcellulose or the hydroxypropyl methylcellulose.The edible kind of starch microballoon of preparation, the fields such as applicable medicine, cosmetics, food modifier especially at medicine field, can make the slow release effect of medicine greatly strengthen.
The on the other hand application of spherex mainly is the industries such as printing ink, papermaking.It is one or more any combination in polyvinyl alcohol, polyvinylpyrrolidone, polyacrylic acid or the polyacrylamide that this type of spherex prepares employed thickener.
Patent Application Publication of the present invention a kind of preparation method of spherex, prepared spherex, has unique architectural feature, smooth surface, boring, surface distributed have one or several nanometer level microporous, and wall thickness is even, particle diameter is 10～100 μ m, wall thickness is 1～10 μ m, can become very strong medicine portable object, and the boring structure is so that the slow release effect of medicine is more obvious.
Spherex preparation method of the present invention, raw material is commercially available starch and thickener, be simple and easy to, the preparation technology who adopts is simple, need not the complicated loaded down with trivial details technological operations such as adjusting pH value, the spherex of preparation is widely used in the industries such as food, medicine, cosmetics, food modifier, printing ink and papermaking.
Description of drawings
Shown in Figure 1 is the spherex Electronic Speculum picture of the embodiment of the invention 1 preparation.
The specific embodiment
The present invention is further illustrated below in conjunction with embodiment, but these embodiment must not be used for explaining for limiting the scope of the invention.
Among the embodiment, used starch is the commercially available starch of food-grade, cyclodextrin, xanthans, agar, sodium alginate, sodium carboxymethylcellulose and hydroxypropyl methylcellulose are food-grade class thickener, and polyvinyl alcohol, polyvinylpyrrolidone, polyacrylic acid and polyacrylamide are the technical grade thickener.
Preparation sweet potato starch microballoon:
1. the 10g sweet potato starch is mixed with 4.2g water, the preparation mass percentage concentration is 70% sweet potato starch emulsion;
2. the 2g cyclodextrin is mixed with 98g water, under 5000 rev/mins speed of agitator, be warming up to 80 ℃, the preparation mass percentage concentration is 2% cyclodextrin solution;
3. reduce cyclodextrin solution temperature to 58 ℃, under 5000 rev/mins speed of agitator, slowly be added to the sweet potato starch emulsion in the cyclodextrin solution, after the sweet potato starch emulsion adds, rising temperature to 68 ℃, constant temperature stirred 10 minutes, leave standstill, naturally supernatant is abandoned in cooling, and washing, drying can prepare the sweet potato starch microballoon.
Internal structure for the spherex of finding out more intuitively preparation, when the preparation sample of scanning electron microscope observation, the spherex sample is partly ground, (Fig. 1) can find out by electromicroscopic photograph, the prepared sweet potato starch microballoon spherome surface of present embodiment is smooth, pore-free, wall thickness evenly and boring, particle diameter is 10～50 μ m, and wall thickness is 2～3 μ m.
Embodiment 2
Preparation tapioca microballoon:
1. the 30g tapioca is mixed with 120g water, the preparation mass percentage concentration is 20% tapioca emulsion;
2. the 7.5g polyvinylpyrrolidone is mixed with 42.5g water, under 1000 rev/mins speed of agitator, be warming up to 40 ℃, the preparation mass percentage concentration is 15% polyvinylpyrrolidonesolution solution;
3. the polyvinylpyrrolidonesolution solution that raises temperature to 50 ℃ under 1000 rev/mins speed of agitator, slowly is added to the tapioca emulsion in the polyvinylpyrrolidonesolution solution, after the tapioca emulsion adds, rising temperature to 65 ℃, constant temperature stirred 10 minutes, leave standstill, naturally supernatant is abandoned in cooling, washing, dry, can prepare the tapioca microballoon, particle diameter is 70～100 μ m, and wall thickness is 7～10 μ m.
Embodiment 3
Preparation Chinese yam starch microballoon:
1. the 10g Chinese yam starch is mixed with 10g water, the preparation mass percentage concentration is 50% Chinese yam starch emulsion;
2. the 5g xanthans is mixed with 45g water, under 3000 rev/mins speed of agitator, be warming up to 45 ℃, the preparation mass percentage concentration is 10% xanthan gum solution;
3. the xanthan gum solution temperature to 60 that raises ℃ under 2000 rev/mins speed of agitator, slowly is added to the Chinese yam starch emulsion in the xanthan gum solution, after the Chinese yam starch emulsion adds, rising temperature to 70 ℃, constant temperature stirred 30 minutes, leave standstill, naturally supernatant is abandoned in cooling, washing, dry, can prepare the Chinese yam starch microballoon, particle diameter is 20～50 μ m, and wall thickness is 1～2 μ m.
Embodiment 4
Preparation pueraria starch microballoon:
1. the 10g pueraria starch is mixed with 20g water, the preparation mass percentage concentration is 33% pueraria starch emulsion;
2. 5g sodium alginate and 5g sodium carboxymethylcellulose are mixed with 60g water, under 3000 rev/mins speed of agitator, be warming up to 40 ℃, the preparation mass percentage concentration is sodium alginate-carboxymethylcellulose sodium solution of 14.3%;
3. sodium alginate-carboxymethylcellulose sodium solution temperature to 56 that raises ℃ under 2500 rev/mins speed of agitator, slowly is added to the pueraria starch emulsion in sodium alginate-carboxymethylcellulose sodium solution, after the pueraria starch emulsion adds, rising temperature to 68 ℃, constant temperature stirred 10 minutes, leave standstill, naturally supernatant is abandoned in cooling, washing, dry, can prepare the pueraria starch microballoon, particle diameter is 10～30 μ m, and wall thickness is 2～4 μ m.
Embodiment 5
Preparation Rhizoma Nelumbinis starch microballoon:
1. the 8g Rhizoma Nelumbinis starch is mixed with 5g water, the preparation mass percentage concentration is 61.5% Rhizoma Nelumbinis starch emulsion;
2. 3g sodium alginate and 5g sodium carboxymethylcellulose are mixed with 60g water, under 2500 rev/mins speed of agitator, be warming up to 67 ℃, the preparation mass percentage concentration is sodium alginate-carboxymethylcellulose sodium solution of 11.7%;
3. reduce sodium alginate-carboxymethylcellulose sodium solution temperature to 63 ℃, under 4000 rev/mins speed of agitator, slowly be added to the Rhizoma Nelumbinis starch emulsion in sodium alginate-carboxymethylcellulose sodium solution, after the Rhizoma Nelumbinis starch emulsion adds, rising temperature to 74 ℃, constant temperature stirred 17 minutes, leave standstill, naturally supernatant is abandoned in cooling, washing, dry, can prepare the Rhizoma Nelumbinis starch microballoon, particle diameter is 20～75 μ m, and wall thickness is 2.5～4 μ m.
Embodiment 6
Preparation farina microballoon:
1. the 4g farina is mixed with 16g water, the preparation mass percentage concentration is 20% farina emulsion;
2. 1g cyclodextrin, 2g agar, 2g hydroxypropyl methylcellulose are mixed with 85g water, under 3000 rev/mins speed of agitator, be warming up to 70 ℃, the preparation mass percentage concentration is cyclodextrin-agar of 5.6%-Gonak;
3. reduce cyclodextrin-agar-Gonak temperature to 60 ℃, under 4000 rev/mins speed of agitator, the farina emulsion slowly is added in cyclodextrin-agar-Gonak, after the farina emulsion adds, rising temperature to 77 ℃, constant temperature stirred 25 minutes, leave standstill, naturally supernatant is abandoned in cooling, washing, dry, can prepare the farina microballoon, particle diameter is 50～75 μ m, and wall thickness is 2～5 μ m.
Embodiment 7
Preparation tapioca microballoon:
1. the 5g tapioca is mixed with 15g water, the preparation mass percentage concentration is 25% tapioca emulsion;
2. 1.5g polyvinyl alcohol, 2.5g polyacrylic acid, 1g polyacrylic acid amide are mixed with 85g water, under 3500 rev/mins speed of agitator, be warming up to 70 ℃, the preparation mass percentage concentration is 5.6% polyvinyl alcohol-poly acrylic acid-poly acrylic acid amides solution;
3. reduce polyvinyl alcohol-poly acrylic acid-poly acrylic acid amides solution temperature to 65 ℃, under 3500 rev/mins speed of agitator, the tapioca emulsion slowly is added in polyvinyl alcohol-poly acrylic acid-poly acrylic acid amides solution, after the tapioca emulsion adds, rising temperature to 80 ℃, constant temperature stirred 30 minutes, leave standstill, naturally supernatant is abandoned in cooling, washing, dry, can prepare the tapioca microballoon, particle diameter is 10～40 μ m, and wall thickness is 2～3 μ m.
Embodiment 8
Preparation sweet potato-farina microballoon:
1. 5g sweet potato starch and 5g farina are mixed with 15g water, the preparation mass percentage concentration is 40% sweet potato-farina emulsion;
2. 5g agar is mixed with 80g water, under 4000 rev/mins speed of agitator, be warming up to 50 ℃, the preparation mass percentage concentration is 5.9% agar solution;
3. the agar solution temperature to 55 that raises ℃ under 4000 rev/mins speed of agitator, slowly is added to sweet potato-farina emulsion in the agar solution, after sweet potato-farina emulsion adds, rising temperature to 65 ℃, constant temperature stirred 25 minutes, leave standstill, naturally supernatant is abandoned in cooling, washing, dry, can prepare sweet potato-farina microballoon, particle diameter is 10～60 μ m, and wall thickness is 1.5～2.5 μ m.
Embodiment 9
The preparation root of kudzu vine-Rhizoma Nelumbinis starch microballoon:
1. 3g pueraria starch and 5g Rhizoma Nelumbinis starch are mixed with 17g water, the preparation mass percentage concentration is 32% the root of kudzu vine-Rhizoma Nelumbinis starch emulsion;
2. the 5g polyvinyl alcohol is mixed with 95g water, under 3500 rev/mins speed of agitator, be warming up to 68 ℃, the preparation mass percentage concentration is 5% poly-vinyl alcohol solution;
3. reduce poly-vinyl alcohol solution temperature to 60 ℃, under 2500 rev/mins speed of agitator, slowly be added to the root of kudzu vine-Rhizoma Nelumbinis starch emulsion in the poly-vinyl alcohol solution, after the root of kudzu vine-Rhizoma Nelumbinis starch emulsion adds, rising temperature to 65 ℃, constant temperature stirred 15 minutes, leave standstill, naturally supernatant is abandoned in cooling, washing, dry, can prepare the root of kudzu vine-Rhizoma Nelumbinis starch microballoon, particle diameter is 10～50 μ m, and wall thickness is 2～3 μ m.
Embodiment 10
The preparation root of kudzu vine-Chinese yam starch microballoon:
1. 3g pueraria starch and 4g Chinese yam starch are mixed with 13g water, the preparation mass percentage concentration is 35% Pueraria lobota phase-Chinese yam starch emulsion;
2. 2.5g xanthans, 2.5g cyclodextrin are mixed with 85g water, under 2500 rev/mins speed of agitator, be warming up to 60 ℃, the preparation mass percentage concentration is xanthans-cyclodextrin solution of 5.5%;
3. reduce xanthans-cyclodextrin solution temperature to 55 ℃, under 2500 rev/mins speed of agitator, slowly be added to the root of kudzu vine-Chinese yam starch emulsion in xanthans-cyclodextrin solution, after the root of kudzu vine-Chinese yam starch emulsion adds, rising temperature to 73 ℃, constant temperature stirred 10 minutes, leave standstill, naturally supernatant is abandoned in cooling, washing, dry, can prepare the root of kudzu vine-Chinese yam starch microballoon, particle diameter is 20～60 μ m, and wall thickness is 2～3 μ m.
Embodiment 11
Preparation sweet potato-cassava-farina microballoon:
1. 2g sweet potato starch, 2.5g tapioca and 1.5g farina are mixed with 14g water, the preparation mass percentage concentration is sweet potato-cassava of 30%-farina emulsion;
2. the 2.5g sodium alginate is mixed with 85g water, under 2500 rev/mins speed of agitator, be warming up to 67 ℃, the preparation mass percentage concentration is 5.5% sodium alginate soln;
3. reduce sodium alginate soln temperature to 58 ℃, under 2500 rev/mins speed of agitator, slowly be added to sweet potato-cassava-farina emulsion in the sodium alginate soln, after sweet potato-cassava-farina emulsion adds, rising temperature to 65 ℃, constant temperature stirred 15 minutes, leave standstill, naturally supernatant is abandoned in cooling, washing, dry, can prepare sweet potato-cassava-farina microballoon, particle diameter is 20～40 μ m, and wall thickness is 1～2 μ m.
Embodiment 12
Preparation sweet potato-Chinese yam-Rhizoma Nelumbinis starch microballoon:
1. 1g sweet potato starch, 1.5g Chinese yam starch and 2.5g Rhizoma Nelumbinis starch are mixed with 5g water, the preparation mass percentage concentration is sweet potato-Chinese yam of 50%-Rhizoma Nelumbinis starch emulsion;
2. 2g polyvinylpyrrolidone, 2.5g polyvinyl alcohol are mixed with 85g water, under 3000 rev/mins speed of agitator, be warming up to 45 ℃, the preparation mass percentage concentration is polyvinylpyrrolidone-poly-vinyl alcohol solution of 5%;
3. the sodium alginate soln temperature to 58 that raises ℃ under 4000 rev/mins speed of agitator, slowly is added to sweet potato-Chinese yam-Rhizoma Nelumbinis starch emulsion in polyvinylpyrrolidone-poly-vinyl alcohol solution, after sweet potato-Chinese yam-Rhizoma Nelumbinis starch emulsion adds, rising temperature to 66 ℃, constant temperature stirred 25 minutes, leave standstill, naturally supernatant is abandoned in cooling, washing, dry, can prepare sweet potato-Chinese yam-Rhizoma Nelumbinis starch microballoon, particle diameter is 60～70 μ m, and wall thickness is 2～4 μ m.
Embodiment 13
Preparation Chinese yam-lotus root-pueraria starch microballoon:
1. 1.5g Chinese yam starch, 2.5g Rhizoma Nelumbinis starch and 1.5g pueraria starch are mixed with 5g water, the preparation mass percentage concentration is Chinese yam-lotus root of 35.5%-pueraria starch emulsion;
2. 1g cyclodextrin, 2.5g agar, 2.5g hydroxypropyl methylcellulose are mixed with 84g water, under 3000 rev/mins speed of agitator, be warming up to 70 ℃, the preparation mass percentage concentration is cyclodextrin-agar of 6.6%-Gonak;
3. reduce sodium alginate soln temperature to 60 ℃, under 4000 rev/mins speed of agitator, Chinese yam-lotus root-pueraria starch emulsion slowly is added in cyclodextrin-agar-Gonak, after Chinese yam-lotus root-pueraria starch emulsion adds, rising temperature to 67 ℃, constant temperature stirred 15 minutes, leave standstill, naturally supernatant is abandoned in cooling, washing, dry, can prepare Chinese yam-lotus root-pueraria starch microballoon, particle diameter is 10～50 μ m, and wall thickness is 2～3 μ m.
Claims (3)
1. the preparation method of a spherex is characterized in that, may further comprise the steps:
1. plant amylum is mixed with water, the preparation mass percentage concentration is 20～70% plant amylum emulsion;
2. thickener is mixed with water, under 1000～5000 rev/mins speed of agitator, be warming up to 40～80 ℃, the preparation mass percentage concentration is 2～15% thickener soln;
3. adjust thickener soln temperature to 50～65 ℃, under 1000～5000 rev/mins speed of agitator, slowly be added to the plant amylum emulsion in the thickener soln, after the plant amylum emulsion adds, adjust temperature to 65～80 ℃, constant temperature stirred 10～30 minutes, leave standstill, naturally supernatant is abandoned in cooling, washing, drying;
Wherein, described thickener is one or more in cyclodextrin, xanthans, agar, sodium alginate, sodium carboxymethylcellulose or the hydroxypropyl methylcellulose;
Perhaps;
Described thickener is one or more in polyvinyl alcohol, polyvinylpyrrolidone, polyacrylic acid or the polyacrylamide.
2. the preparation method of spherex according to claim 1 is characterized in that, step 1. described plant amylum is in tapioca, sweet potato starch, farina, Chinese yam starch, Rhizoma Nelumbinis starch or the pueraria starch one or more.
3. the preparation method of spherex according to claim 1 is characterized in that, the step 1. concentration of described plant amylum emulsion is 30～50%.
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| JP2013169122A (en) | 2012-02-17 | 2013-08-29 | Panasonic Corp | Non-contact charge module and portable terminal having the same |
| CN103554275B (en) * | 2013-10-14 | 2015-11-25 | 广西红豪淀粉开发有限公司 | A kind of preparation method of tapioca (flour) |
| CN104130066B (en) * | 2014-08-06 | 2016-03-02 | 成都新柯力化工科技有限公司 | A kind of spherex slow release fertilizer and its preparation method and application |
| CN104815348A (en) * | 2014-11-28 | 2015-08-05 | 杨子中 | Preparation method for composite micro-sphere for stopping bleeding in clinical operation |
| CN105435236A (en) * | 2015-12-04 | 2016-03-30 | 中国林业科学研究院林产化学工业研究所 | Preparation method of gingko resistant starch microspheres |
| CN105869912B (en) * | 2016-04-12 | 2018-06-15 | 湘潭大学 | A kind of preparation method and applications of starch base Monodispersed activated carbon microballon material |
| 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 |
| CN106902716B (en) * | 2017-02-27 | 2020-02-14 | 广西科学院 | Preparation method of small-particle-size starch microspheres |
| US20210032373A1 (en) | 2017-08-22 | 2021-02-04 | China Petroleum & Chemical Corporation | Starch-containing microsphere and preparation method and use 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 |
| CN115462520B (en) * | 2022-08-29 | 2023-08-18 | 江苏大学 | Ultrasonic preparation of lotus root starch pickering emulsion and application of lotus root starch pickering emulsion as functional food |
| CN117385667A (en) * | 2023-11-28 | 2024-01-12 | 仙鹤股份有限公司 | Preparation method of lining paper for food-grade stainless steel plate |
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| CN101045790A (en) * | 2007-04-28 | 2007-10-03 | 陕西科技大学 | Synthesis method of shell starch microsphere |
| CN101125133A (en) * | 2007-09-27 | 2008-02-20 | 武汉麦可得生物技术有限公司 | Unsaturated fatty acid microcapsule preparing technology and application |
| CN101205304A (en) * | 2007-12-10 | 2008-06-25 | 中国农业大学 | Starch microspheres and method for preparing the same |
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| SE518008C2 (en) * | 2000-11-16 | 2002-08-13 | Bioglan Ab | Microparticles containing biologically active compound useful in controlled release comprise a biodegradable starch as a matrix containing biologically active substance |
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| CN101045790A (en) * | 2007-04-28 | 2007-10-03 | 陕西科技大学 | Synthesis method of shell starch microsphere |
| CN101125133A (en) * | 2007-09-27 | 2008-02-20 | 武汉麦可得生物技术有限公司 | Unsaturated fatty acid microcapsule preparing technology and application |
| CN101205304A (en) * | 2007-12-10 | 2008-06-25 | 中国农业大学 | Starch microspheres and method for preparing the same |
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