CN1271135C - Biological polysaccharide macromolecule magnetic microsphere and preparation method - Google Patents
Biological polysaccharide macromolecule magnetic microsphere and preparation method Download PDFInfo
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- CN1271135C CN1271135C CNB2004100572581A CN200410057258A CN1271135C CN 1271135 C CN1271135 C CN 1271135C CN B2004100572581 A CNB2004100572581 A CN B2004100572581A CN 200410057258 A CN200410057258 A CN 200410057258A CN 1271135 C CN1271135 C CN 1271135C
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Abstract
The present invention relates to magnetic microspheres with superior magnetic responsiveness which are prepared from tamarind gum, artemisia gum, xanthan gum, guar gum and other biological polysaccharide macromolecules as preparation materials, Fe3O4 as a magnetic fluid, and formaldehyde as a crosslinking agent by carrying out sulfonylation on polysaccharide hydroxyl groups with aminobenzenesulfonic acid. The surfaces of the magnetic microspheres have a porous honeycomb structure, the grain diameter is from 2.0*10<2> to 6.3*10<2>mum, the specific magnetism is from 1.393 to 1.726 emu/g, and the functional groups on the surfaces of the magnetic microspheres are-OSO2(C6H4)NH2; the magnetic microspheres have the advantages of no toxicity, good biocompatibility and favorable operation performance and reaction performance, and can be used as the superior carriers of enzyme or other biological materials and used in different fields.
Description
Technical field
The present invention relates generally to a kind of biological polysaccharide polymer magnetic microsphere and preparation method.
Background technology
Magnetic macromolecular microsphere is meant that inside contains the ultrafine powder of magneticmetal or metal oxide and have the polymer microsphere of magnetic responsiveness.It is a kind of new functional macromolecule material that recent two decades grows up.Magnetic macromolecular microsphere can be introduced multiple reactive functional group at microsphere surface by chemical reactions such as copolymerization, surface modifications, and has specific reactivity, can come biologically active substances such as desmoenzyme, antibody, cell by covalent linkage.Magnetic macromolecular microsphere has certain magnetic responsiveness, thereby has good processing property and production performance, and the carrier that can be used as enzyme, antibody, cell or other biomaterial is applied to different field.
The biopolymer magnetic microsphere is meant with the biopolymer to be the magnetic macromolecular microsphere that the surface of material preparation is connected with the specific function group.The biopolymer magnetic microsphere is compared with the chemosynthesis high molecule magnetic microsphere has advantages such as nontoxic, good biocompatibility, and the good carrier that can be used as enzyme or other biomaterial is applied to different field such as food, biomedicine, biotechnology, environmental science and Chemical Manufacture.
Polymer microsphere and preparation thereof, the investigator attaches great importance to both at home and abroad.Japanese Patent 2554835 has been applied for a kind of preparation method of oil hydrosol microballoon; The open 02-286729 of Japanese Patent has applied for a kind of preparation method of vinyl aromatic compounds magnetic microsphere; The open 01-133304 of Japanese Patent has applied for a kind of polysiloxane magnetic microsphere and application thereof; The open 62-244438 of Japanese Patent has applied for a kind of magnetic microsphere and use thereof that unsaturated fatty acids forms of adsorbing; The open 61-174229 of Japanese Patent has applied for a kind of magnetic thermoplastic resin lipoid microsphere preparation; U.S. Patent application 20040126902 has applied for containing the magnetic microsphere and uses thereof of the compound of silicon and aluminium; Chinese patent CN1485362, Chinese patent CN1328083, Chinese patent CN1290524 etc. have applied for the chitosan microball preparation method and its usage; Chinese patent CN1314430, Chinese patent CN1293952 etc. have applied for chitosan and composite method and the purposes that prepare polymer microsphere such as polyacrylic acid or fibroin; Chinese patent CN1275619, Chinese patent CN1234444 etc. have applied for the preparation and the application thereof of the fixed cell carrier that the poly-mannosans in carrageenin and Portugal or konjac polysaccharide are composite; Prepare magnetic microsphere with synthesized polymer material abroad; Domestic patent does not relate to the preparation of biological polysaccharide polymer magnetic microspheres such as tamarind seed gum, artemisia glue, xanthan gum, guar gum.
Summary of the invention
The invention provides a kind of biological polysaccharide polymer magnetic microsphere and preparation method, be intended to utilize a kind of nontoxic, good biocompatibilities of biological polysaccharide polymer material preparation such as tamarind seed gum, artemisia glue, konjac polysaccharide, xanthan gum, guar gum, and the functional high molecule material with good operation performance, production performance and response characteristic is as the carrier of enzyme or other bioactive molecules.
The present invention designs as follows:
With biological polyoses such as tamarind seed gum, artemisia glue, xanthan gum, guar gums is material, Fe
3O
4Be magnetic fluid, formaldehyde is linking agent, and Sulphanilic Acid is the magnetic microsphere with certain magnetic responsiveness of aminating agent preparation, and the magnetic microsphere surface functional group is-OSO
2(C
6H
4) NH
2
Step of the present invention is as follows,
Step 1: preparation 34.8%FeSO
47H
2The O aqueous solution, 54.1% FeCl
36H
2The O aqueous solution, 36.0% the NaOH aqueous solution;
Step 2: with perferrite solution and 4: 5 mixings of molysite aqueous solution (V/V), stir,
Step 3: be warming up to 55 ℃, add 5 parts of (V/V) alkaline solutions, add PEG100003.6% (W/V) behind the reaction 30min;
Step 4: be warming up to 80 ℃, and stopped reaction behind the reaction 30min, be cooled to room temperature, be neutralized to neutrality with hydrochloric acid, leave standstill, supernatant liquid is water-soluble magnetic fluid;
Step 5: in 1.0% anhydrous Sulphanilic Acid aqueous solution 50ml, add the water-soluble magnetic fluid of 1ml, tamarind seed gum or artemisia glue or xanthan gum or guar gum, room temperature reaction 2hr, add organic paraffin, ethyl acetate, span-80, under the rotating speed of 500rpm/min, stir 20min, slowly drip formaldehyde 3ml, continue to stir 1hr, supernatant liquor inclines, with sherwood oil, washing with acetone, make the solvent wash several times with dehydrated alcohol more at last, 50 ℃ of vacuum-dryings promptly get the biological polysaccharide polymer magnetic microsphere.Characteristics of the present invention: the present invention serves as the preparation material with biological polysaccharide polymers such as tamarind seed gum, artemisia glue, xanthan gum, guar gums, Fe
3O
4Be magnetic fluid, formaldehyde is linking agent, with Sulphanilic Acid sulfonylation polysaccharide hydroxyl, has prepared the magnetic microsphere with higher magnetic responsiveness.Magnetic microsphere is the porous surface polynuclear plane, and particle diameter is 2.0 * 10
2-6.3 * 10
2μ m, susceptibility is 1.393-1.726emu/g, surface functional group is-OSO
2(C
6H
4) NH
2Such magnetic microsphere, nontoxic, good biocompatibility, processing property and reactivity worth are good, and the good carrier that can be used as enzyme or other biomaterial is applied to different field.
Description of drawings
The present invention is further described below in conjunction with drawings and Examples.
Fig. 1 is tamarind seed gum magnetic microsphere pattern figure.
Embodiment
Embodiment 1: the preparation of tamarind seed gum magnetic microsphere,
Step 1: preparation 34.8%FeSO
47H
2The O aqueous solution, 54.1% FeCl
36H
2The O aqueous solution, 36.0% the NaOH aqueous solution;
Step 2: with perferrite solution and 4: 5 mixings of molysite aqueous solution (V/V), stir,
Step 3: be warming up to 55 ℃, add 5 parts of (V/V) alkaline solutions, add PEG100003.6% (W/V) behind the reaction 30min;
Step 4: be warming up to 80 ℃, and stopped reaction behind the reaction 30min, be cooled to room temperature, be neutralized to neutrality with hydrochloric acid, leave standstill, supernatant liquid is water-soluble magnetic fluid;
Step 5: in 1.0% anhydrous Sulphanilic Acid aqueous solution 50ml, add the water-soluble magnetic fluid of 1ml, 0.5g tamarind seed gum, room temperature reaction 2hr, add organic paraffin, ethyl acetate, span-80, under the rotating speed of 500rpm/min, stir 20min, slowly drip formaldehyde 3ml, continue to stir 1hr, supernatant liquor inclines, with sherwood oil, washing with acetone, make the solvent wash several times with dehydrated alcohol more at last, 50 ℃ of vacuum-dryings promptly get surperficial containing-OSO
2(C
6H
4) NH
2The tamarind seed gum magnetic microsphere, tamarind seed gum magnetic microsphere susceptibility 1.463emu/g.
Embodiment 2: the preparation of artemisia glue magnetic microsphere
Replace the 0.5g tamarind seed gum with the 0.40g artemisia glue in step 5, the kind of other reagent, proportioning and preparation method are described with embodiment 1, get the artemisia glue magnetic microsphere, artemisia glue magnetic microsphere susceptibility 1.726emu/g.
Embodiment 3: the preparation of xanthan gum glue magnetic microsphere
Replace the 0.5g tamarind seed gum with the 0.8g xanthan gum in step 5, the kind of other reagent, proportioning and preparation method are described with embodiment 1, get xanthan gum glue magnetic microsphere, xanthan gum magnetic microsphere susceptibility 1.393emu/g.
Embodiment 4: the preparation of guar gum magnetic microsphere
Replace the 0.5g tamarind seed gum with the 0.6g guar gum in step 5, the kind of other reagent, proportioning and preparation method are described with embodiment 1, get the guar gum magnetic microsphere, guar gum magnetic microsphere susceptibility 1.562emu/g.
Microsphere characterizes
As shown in Figure 1, utilize characterising biological high molecule magnetic microspheres such as scanning electron microscope, infrared spectra, ancient Erichsen magnetic balance is measured susceptibility.
Scanning electron microscopic observation confirms that magnetic microsphere is the porous surface polynuclear plane, microballoon form homogeneous, and particle diameter is 2.0 * 10
2-6.3 * 10
2In the mu m range; It is 1.393-1.726emu/g that ancient Erichsen magnetic balance is measured susceptibility, and surface functional group is-OSO
2(C
6H
4) NH
2, show that magnetic microsphere has stronger magnetic responsiveness.
Claims (4)
1. a biological polysaccharide polymer magnetic microsphere preparation method is characterized in that: utilize tamarind seed gum or artemisia glue or xanthan gum or guar gum material with Fe
3O
4For magnetic fluid prepares magnetic microsphere; Follow these steps to:
Step 1: preparation 34.8%FeSO
47H
2The O aqueous solution, 54.1% FeCl
36H
2The O aqueous solution, 36.0% the NaOH aqueous solution;
Step 2: with perferrite solution and molysite aqueous solution V/V4: 5 mixings, stir,
Step 3: be warming up to 55 ℃, add 5 parts of V/V alkaline solutions, add PEG100003.6%W/V behind the reaction 30min;
Step 4: be warming up to 80 ℃, and stopped reaction behind the reaction 30min, be cooled to room temperature, be neutralized to neutrality with hydrochloric acid, leave standstill, supernatant liquid is water-soluble magnetic fluid;
Step 5: in 1.0% anhydrous Sulphanilic Acid aqueous solution 50ml, add the water-soluble magnetic fluid of 1ml, tamarind seed gum 0.5g or xanthan gum 0.8g or artemisia glue 0.40g or guar gum 0.6g, room temperature reaction 2hr, add organic paraffin, ethyl acetate, span-80, under the rotating speed of 500rpm/min, stir 20min, slowly drip formaldehyde 3ml, continue to stir 1hr, supernatant liquor inclines, with sherwood oil, washing with acetone, make the solvent wash several times with dehydrated alcohol more at last, 50 ℃ of vacuum-dryings promptly get the biological polysaccharide polymer magnetic microsphere.
2. a kind of biological polysaccharide polymer magnetic microsphere of method preparation according to claim 1, it is characterized in that: microsphere is the porous surface polynuclear plane, and particle diameter is 2.0 * 10
2-6.3 * 10
2μ m.
3. a kind of biological polysaccharide polymer magnetic microsphere as claimed in claim 2 is characterized in that surface functional group is-OSO
2(C
6H
4) NH
2
4. as claim 2 or 3 described a kind of biological polysaccharide polymer magnetic microspheres, it is characterized in that: tamarind seed gum magnetic microsphere susceptibility 1.463emu/g, artemisia glue magnetic microsphere susceptibility 1.726emu/g, xanthan gum magnetic microsphere susceptibility 1.393emu/g, guar gum magnetic microsphere susceptibility 1.562emu/g.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100572581A CN1271135C (en) | 2004-08-30 | 2004-08-30 | Biological polysaccharide macromolecule magnetic microsphere and preparation method |
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|---|---|---|---|
| CNB2004100572581A CN1271135C (en) | 2004-08-30 | 2004-08-30 | Biological polysaccharide macromolecule magnetic microsphere and preparation method |
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|---|---|
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| CN1271135C true CN1271135C (en) | 2006-08-23 |
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|---|---|---|---|
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100335545C (en) * | 2005-10-31 | 2007-09-05 | 西北师范大学 | Composite biopolysaccharide magnetic microsphere preparation method |
| WO2008141475A1 (en) * | 2007-05-18 | 2008-11-27 | Beijing Dingguochangsheng Biotech. Co., Ltd. | A simple method of introducing magnetic particles into macromolecule |
| CN103054814B (en) * | 2013-01-16 | 2014-06-11 | 南京理工大学 | Preparation method for polysaccharide microspheres based on medicine cross-linking |
| CN103824671B (en) * | 2014-03-12 | 2016-07-06 | 中国石油大学(华东) | A kind of nanometer magnetofluid for induced fracture monitoring and preparation method thereof |
| CN104827049B (en) * | 2015-02-11 | 2017-03-15 | 北京建筑大学 | A kind of zeroth order iron ball preparation method |
| CN104861215B (en) * | 2015-06-04 | 2019-02-26 | 中国海洋石油集团有限公司 | A method of improving the dispersing and dissolving performance of oil field biological polyoses |
| CN108753273A (en) * | 2018-06-21 | 2018-11-06 | 山东禹王生态食业有限公司 | A kind of modified soluble dietary fiber thickener and preparation method thereof |
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2004
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