CN1687195A - Glucomannan microgel particles of konnjaku and preparation method - Google Patents
Glucomannan microgel particles of konnjaku and preparation method Download PDFInfo
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- CN1687195A CN1687195A CN 200510018518 CN200510018518A CN1687195A CN 1687195 A CN1687195 A CN 1687195A CN 200510018518 CN200510018518 CN 200510018518 CN 200510018518 A CN200510018518 A CN 200510018518A CN 1687195 A CN1687195 A CN 1687195A
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- glucomannan
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- konnjaku
- alkaline aqueous
- rhizoma amorphophalli
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Abstract
The present invention discloses a konjak glucomannal gel particle and its preparation method. It is characterized by that under the action of surfactant the konjak glucomannan alkaline aqueous solution can be dispersed in the liquid paraffin, and heated so as to form gel particles. The grain size of said gel particles is uniform, and can be regulated, it has good biological compatibility and degradability, so that it has extensive application range.
Description
Technical field
The present invention relates to a kind of biodegradable glucomannan microgel particles of konnjaku and preparation method thereof.Belong to the natural macromolecular material field.
Background technology
Hydrogel is that hydrophilic polymer passes through the cross-linked network that chemical bond, hydrogen bond, Van der Waals force or physical entanglement form, and is water insoluble but can absorb a large amount of water and swelling keeps solid shape simultaneously in water.Hydrogel has caused scientific worker's common concern in many purposes in fields such as biological chemistry, medical science, agricultural, daily-use chemical industry.Most of up to now hydrogels are nonbiodegradable, and this has limited their application aspect medicine and environmental protection.
The stem tuber of konjaku is rich in Rhizoma amorphophalli glucomannan, and it is the main component of konjaku powder, accounts for the heavy 50%-60% of dry product.Rhizoma amorphophalli glucomannan has many good properties as a kind of natural macromolecule amylose, such as biocompatibility, and film-forming properties, biodegradable etc.Can be applicable to food, biochemistry, medicine and daily life all respects.Deacetylation takes place when Rhizoma amorphophalli glucomannan heats under the effect of alkali, and self-crosslinking forms the gel of heat irreversible.Existing konjak gel mostly is bulk or globular, and volume is bigger, thereby its purposes is restricted.
And particulate konjak gel has bigger specific surface area, is prepared into suspension easily, aspect medicine sustained release carrier and polymer water-absorbent wider purposes is being arranged.
The present invention adopts the Rhizoma amorphophalli glucomannan alkaline aqueous solution to be dispersed in the whiteruss, obtains particulate gel through adding Thermogelling, and technology is comparatively easy, and raw material is inexpensive, wide material sources.Products obtained therefrom is biodegradable, has uniform particle diameter, and size is adjustable, and the not available advantage of large volume gel is arranged, and purposes is widely arranged.
Summary of the invention
The purpose of this invention is to provide a kind of glucomannan microgel particles of konnjaku and preparation method thereof, resulting glucomannan microgel particles of konnjaku volume is less, have bigger specific surface area, be prepared into suspension easily, aspect medicine sustained release carrier and polymer water-absorbent, wider purposes arranged.
Technical scheme provided by the invention is: a kind of glucomannan microgel particles of konnjaku, be dispersed in the whiteruss under Action of Surfactant by the Rhizoma amorphophalli glucomannan alkaline aqueous solution, and add the thermosetting microgel particle and obtain.
The preparation method of above-mentioned glucomannan microgel particles of konnjaku: Rhizoma amorphophalli glucomannan is mixed with the alkaline aqueous solution of pH value for 9-13, the alkaline aqueous solution of Rhizoma amorphophalli glucomannan is dispersed in the whiteruss under Action of Surfactant, add the thermosetting microgel particle, separate obtaining glucomannan microgel particles of konnjaku.
Above-mentioned alkali is yellow soda ash or sodium hydroxide or potassium hydroxide, and its consumption is for making the Rhizoma amorphophalli glucomannan pH value of aqueous solution in the 9-13 scope, and is better in the 10-12 scope with the pH value.
The concentration of the alkaline aqueous solution of above-mentioned Rhizoma amorphophalli glucomannan is 1-10wt%, and is better with 1-2%; The alkaline aqueous solution of Rhizoma amorphophalli glucomannan and the volume ratio of whiteruss are 1: 1-8, with 1: 4 for well; The temperature that forms gel is 60-110 ℃, and the time is 1-15 hour, and with 80-90 ℃, 12-14 hour better.
Above-mentioned tensio-active agent is Si Ban or tween, and is better with span-80 or tween 85, and consumption is the 0.5-2.5% (weight) of whiteruss.
The temperature of above-mentioned formation gel is that 80-90 ℃ of time is 12-14 hour.
The microgel particle of above-mentioned formation is by standing demix, and water layer uses organic solvent-normal hexane, sherwood oil (boiling range 60-90 ℃), distilled water wash to not containing organic solvent and being neutral successively, takes the freeze-drying mode to obtain particulate.
The glucomannan microgel particles of konnjaku of gained of the present invention has the performance of a large amount of suctions fast, and the footpath grain is evenly distributed, and observing its particle dia through scanning electronic microscope (SEM) is 0.5-2.0 μ m, and size can be regulated by preparation condition.Preparation technology is easy, and Rhizoma amorphophalli glucomannan itself has useful physiologically active from agricultural-food cheap and easy to get.The present invention also provides an effective way for the comprehensive utilization of agricultural byproducts.
Glucomannan microgel particles of konnjaku of the present invention has biocompatibility and biological degradability, and particularly it does not have and can be used as medicine conlon targeting sustained release pharmaceutical adjunct by the characteristic of the enzyme liberating of intracolic microorganism by the human consumption enzymic digestion.As water-absorbing resin, also can be applicable to biological chemistry, medical science, agricultural, food, filed of daily-use chemical industry, for example dentistry imbibition material, operation bandage, sanitary belt, nursing pad; As filtration, parting material; As antistatic fiber, sealing material and filler; Spices sustained release dosage, deodorizing composition, vegetables and fruits are fresh-keeping, moisture adsorbent of various wrapping material, sludge curing treatment agent etc., and its waste does not cause environmental pollution.
Embodiment
Glucomannan microgel particles of konnjaku of the present invention is to be dispersed in the whiteruss under Action of Surfactant by the Rhizoma amorphophalli glucomannan alkaline aqueous solution, adds the thermosetting microgel particle and obtains.The diameter of gained glucomannan microgel particles of konnjaku is about 0.5-2.0 μ m.
Embodiment one:
Take by weighing 0.2g konjak glucomannan fine powder, be dissolved in 20ml pH12 sodium carbonate solution under the room temperature (15-25 ℃), stir and make its abundant swelling.Under mechanical stirring, its adding is contained in the 80ml whiteruss of 1.0wt% span-80, fully emulsified.Airbath 80-85 ℃ of heating and continuous stir about 14 hours obtains the microgel particle suspension liquid.Standing demix, water layer use normal hexane, sherwood oil (boiling range 60-90 ℃) washing to not containing organic solvent and being neutral successively, and freeze-drying obtains glucomannan microgel particles of konnjaku.Median size is about 0.5 μ m.
Embodiment two:
Take by weighing 0.5g konjak glucomannan fine powder, be dissolved in 20ml pH12 sodium carbonate solution under the room temperature, stir and make its abundant swelling.Under mechanical stirring, its adding is contained in the 80ml whiteruss of 1.0wt% span-80, fully emulsified.Airbath 80-85 ℃ of heating and continuous stir about 14 hours obtains the microgel particle suspension liquid.Standing demix, water layer use normal hexane, sherwood oil (boiling range 60-90 ℃) washing to not containing organic solvent and being neutral successively, and freeze-drying obtains glucomannan microgel particles of konnjaku.Median size is about 2 μ m.
Embodiment three:
Get 2g konjak glucomannan fine powder, be dissolved in 20ml pH12 sodium carbonate solution under the room temperature (15-25 ℃), stir and make its abundant swelling.Under mechanical stirring, its adding is contained in the 160ml whiteruss of 2.0wt% span-80, fully emulsified.Airbath 80-85 ℃ of heating and continuous stir about 14 hours obtains the microgel particle suspension liquid.Standing demix, water layer use normal hexane, sherwood oil (boiling range 60-90 ℃) washing to not containing organic solvent and being neutral successively, and freeze-drying obtains glucomannan microgel particles of konnjaku.Median size is about 4 μ m.
Embodiment four:
Get 0.5g konjak glucomannan fine powder, be dissolved in 20ml pH12 sodium carbonate solution under the room temperature, stir and make its abundant swelling.Under mechanical stirring, its adding is contained in the 80ml whiteruss of 1.0wt% tween 85, fully emulsified.Airbath 80-85 ℃ of heating and continuous stir about 14 hours obtains the microgel particle suspension liquid.Standing demix, water layer use normal hexane, sherwood oil (boiling range 60-90 ℃) washing to not containing organic solvent and being neutral successively, and freeze-drying obtains glucomannan microgel particles of konnjaku.Median size is about 2 μ m.
Embodiment five:
Take by weighing 1.0g konjak glucomannan fine powder, be dissolved in 20ml pH9 sodium hydroxide solution, stir and make its abundant swelling.Under mechanical stirring, its adding is contained in the 140ml whiteruss of span-80 of 1.5wt%, fully emulsified.100 ℃ of heating and continuous stir abouts of airbath 6 hours obtain the microgel particle suspension liquid.Standing demix, water layer use normal hexane, sherwood oil (boiling range 60-90 ℃) washing to not containing organic solvent and being neutral successively, and freeze-drying obtains glucomannan microgel particles of konnjaku.Median size is about 0.8 μ m.
Embodiment six:
Take by weighing 2g konjak glucomannan fine powder, be dissolved in 20ml pH9 sodium hydroxide solution, stir and make its abundant swelling.Under mechanical stirring, its adding is contained in the 140ml whiteruss of span-80 of 2.5wt%, fully emulsified.100 ℃ of heating and continuous stir abouts of airbath 3 hours obtain the microgel particle suspension liquid.Standing demix, water layer use normal hexane, sherwood oil (boiling range 60-90 ℃) washing to not containing organic solvent and being neutral successively, and freeze-drying obtains glucomannan microgel particles of konnjaku.Median size is about 1 μ m.
Embodiment seven:
Take by weighing 2g konjak glucomannan fine powder, be dissolved in 20ml pH9 sodium hydroxide solution, stir and make its abundant swelling.Under mechanical stirring, its adding is contained in the 140ml whiteruss of tween 85 of 2.5wt%, fully emulsified.100 ℃ of heating and continuous stir abouts of airbath 3 hours obtain the microgel particle suspension liquid.Standing demix, water layer use normal hexane, sherwood oil (boiling range 60-90 ℃) washing to not containing organic solvent and being neutral successively, and freeze-drying obtains glucomannan microgel particles of konnjaku.Median size is about 1.5 μ m.
Embodiment eight:
Take by weighing 0.3g konjak glucomannan fine powder, be dissolved in 20ml pH9 potassium hydroxide solution, stir and make its abundant swelling.Under mechanical stirring, its adding is contained in the 30ml whiteruss of span-80 of 1.5wt%, fully emulsified.70 ℃ of heating and continuous stir abouts of airbath 14 hours obtain the microgel particle suspension liquid.Standing demix, water layer use normal hexane, sherwood oil (boiling range 60-90 ℃) washing to not containing organic solvent and being neutral successively, and freeze-drying obtains glucomannan microgel particles of konnjaku.Median size is about 4 μ m.
Embodiment nine:
Take by weighing 0.8g konjak glucomannan fine powder, be dissolved in 20ml pH9 potassium hydroxide solution, stir and make its abundant swelling.Under mechanical stirring, its adding is contained in the 80ml whiteruss of span-80 of 2.5wt%, fully emulsified.70 ℃ of heating and continuous stir abouts of airbath 12 hours obtain the microgel particle suspension liquid.Standing demix, water layer use normal hexane, sherwood oil (boiling range 60-90 ℃) washing to not containing organic solvent and being neutral successively, and freeze-drying obtains glucomannan microgel particles of konnjaku.Median size is about 1.5 μ m.
Embodiment ten:
Take by weighing 0.8g konjak glucomannan fine powder, be dissolved in 20ml pH9 potassium hydroxide solution, stir and make its abundant swelling.Under mechanical stirring, its adding is contained in the 80ml whiteruss of tween 85 of 2.5wt%, fully emulsified.70 ℃ of heating and continuous stir abouts of airbath 12 hours obtain the microgel particle suspension liquid.Standing demix, water layer use normal hexane, sherwood oil (boiling range 60-90 ℃) washing to not containing organic solvent and being neutral successively, and freeze-drying obtains glucomannan microgel particles of konnjaku.Median size is about 2 μ m.
Claims (10)
1. a glucomannan microgel particles of konnjaku is dispersed in the whiteruss under Action of Surfactant by the Rhizoma amorphophalli glucomannan alkaline aqueous solution, adds the thermosetting microgel particle and obtains.
2. the preparation method of the described glucomannan microgel particles of konnjaku of claim 1, it is characterized in that: Rhizoma amorphophalli glucomannan is mixed with the alkaline aqueous solution of pH value for 9-13, the alkaline aqueous solution of Rhizoma amorphophalli glucomannan is dispersed in the whiteruss under Action of Surfactant, add the thermosetting microgel particle, separate obtaining glucomannan microgel particles of konnjaku.
3. preparation method according to claim 2 is characterized in that: alkali is yellow soda ash or sodium hydroxide or potassium hydroxide.
4. according to claim 2 or 3 described preparation methods, it is characterized in that: the pH value of the alkaline aqueous solution of Rhizoma amorphophalli glucomannan is 10-12.
5. according to claim 2 or 3 described preparation methods, it is characterized in that: the concentration of the alkaline aqueous solution of Rhizoma amorphophalli glucomannan is 1-10wt%; The alkaline aqueous solution of Rhizoma amorphophalli glucomannan and the volume ratio of whiteruss are 1: 1-8; The temperature that forms gel is 60-110 ℃, and the time is 1-15 hour.
6. according to claim 2 or 3 described preparation methods, it is characterized in that: tensio-active agent is Si Ban or tween, and consumption is the 0.5-2.5wt% of whiteruss.
7. preparation method according to claim 6 is characterized in that: tensio-active agent is span-80 or tween 85.
8. according to claim 2 or 3 described preparation methods, it is characterized in that: the concentration of konjak portuguese gansu polyose sugar aqueous solution is 1-2wt%.
9. according to claim 2 or 3 described preparation methods, it is characterized in that: the temperature that forms gel is 80-90 ℃, and the time is 12-14 hour.
10. according to claim 2 or 3 described preparation methods, it is characterized in that: the microgel particle of formation passes through standing demix, water layer is that 60-90 ℃ sherwood oil, distilled water wash to water layer do not contain organic solvent and be neutral with organic solvent-normal hexane, boiling range successively, takes the freeze-drying mode to obtain glucomannan microgel particles of konnjaku.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101884909A (en) * | 2010-06-29 | 2010-11-17 | 湖北工业大学 | Method for preparing konjac glucomannan adsorbing material |
| CN103418020A (en) * | 2013-08-31 | 2013-12-04 | 西南大学 | Devilstongue gulcomannan hemostatic sponge and preparation method thereof |
| CN103848996A (en) * | 2012-12-09 | 2014-06-11 | 湖北文理学院 | Preparation method of uniform-dimension konjac glucomannan microspheres |
| CN106511271A (en) * | 2016-10-21 | 2017-03-22 | 湖北工业大学 | KGM (Konjac Glucomannan)-g (grafted)-AH (Alicyclic Amine) drug loaded nano micelle and preparation method |
| CN112753980A (en) * | 2020-12-26 | 2021-05-07 | 湖北一致魔芋生物科技股份有限公司 | Preparation method of instant konjac freeze-dried particle fruit juice sauce |
| CN114751996A (en) * | 2022-04-13 | 2022-07-15 | 合肥工业大学 | Preparation method of konjac glucomannan gel |
-
2005
- 2005-04-07 CN CN 200510018518 patent/CN1272366C/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101884909A (en) * | 2010-06-29 | 2010-11-17 | 湖北工业大学 | Method for preparing konjac glucomannan adsorbing material |
| CN101884909B (en) * | 2010-06-29 | 2014-01-01 | 湖北工业大学 | Method for preparing konjac glucomannan adsorbing material |
| CN103848996A (en) * | 2012-12-09 | 2014-06-11 | 湖北文理学院 | Preparation method of uniform-dimension konjac glucomannan microspheres |
| CN103848996B (en) * | 2012-12-09 | 2016-04-20 | 湖北文理学院 | The preparation of the Konjac Glucomannan Granules of size uniformity |
| CN103418020A (en) * | 2013-08-31 | 2013-12-04 | 西南大学 | Devilstongue gulcomannan hemostatic sponge and preparation method thereof |
| CN103418020B (en) * | 2013-08-31 | 2015-01-07 | 西南大学 | Devilstongue gulcomannan hemostatic sponge and preparation method thereof |
| CN106511271A (en) * | 2016-10-21 | 2017-03-22 | 湖北工业大学 | KGM (Konjac Glucomannan)-g (grafted)-AH (Alicyclic Amine) drug loaded nano micelle and preparation method |
| CN106511271B (en) * | 2016-10-21 | 2019-05-03 | 湖北工业大学 | Fatty amine is grafted konjaku glucomannan medicament-carried nano micelle and preparation method |
| CN112753980A (en) * | 2020-12-26 | 2021-05-07 | 湖北一致魔芋生物科技股份有限公司 | Preparation method of instant konjac freeze-dried particle fruit juice sauce |
| CN114751996A (en) * | 2022-04-13 | 2022-07-15 | 合肥工业大学 | Preparation method of konjac glucomannan gel |
| CN114751996B (en) * | 2022-04-13 | 2023-02-14 | 合肥工业大学 | Preparation method of konjac glucomannan gel |
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| CN1272366C (en) | 2006-08-30 |
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