CN108043372A - A kind of iron-nickel magnetic microballoon for adulterating cobalt ions - Google Patents
A kind of iron-nickel magnetic microballoon for adulterating cobalt ions Download PDFInfo
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- CN108043372A CN108043372A CN201711358048.XA CN201711358048A CN108043372A CN 108043372 A CN108043372 A CN 108043372A CN 201711358048 A CN201711358048 A CN 201711358048A CN 108043372 A CN108043372 A CN 108043372A
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Abstract
This divisional application discloses a kind of iron-nickel magnetic microballoon for adulterating cobalt ions, belongs to chemical material technical field.Main technical schemes are as follows：A kind of iron nickel magnetic ball for adulterating cobalt ions, is used in mixed way cobalt ions and nickel ion in magnetic ball preparation process, the cobalt ions accounts for the 25% of cobalt ions and nickel ion total mole number.The iron-nickel magnetic microballoon of doping cobalt ions synthesized by the present invention can be directly used for purifying with histidine-tagged target protein, without carrying out other modifications, such as antibody modification, and good dispersion in magnetic ball surface, and application effect is rapidly and efficiently, better than the iron-nickel magnetic microballoon of no cobalt doped.It is suitable with reference to the Ago-Gel separating property of nickel ion with the coordination of import to adulterate the iron-nickel magnetic microballoon of cobalt ions, can also be achieved Magnetic Isolation, import separation material can be substituted.
Description
The application for application number 2017104174237, on June 2017 applying date 6, denomination of invention " a kind of cation doping from
The divisional application of the iron-nickel magnetic microballoon of son and its application ".
Technical field
The present invention relates to magnetic microsphere more particularly to a kind of iron-nickel magnetic microballoon for adulterating cobalt ions and its applications.
Background technology
Magnetic macromolecular microsphere is a kind of novel magnetic materials that developed recently gets up, not only with common polymer microsphere
Numerous characteristics also have magnetic responsiveness, can not only by copolymerization and surface be modified the methods of assign its surface functional group, also
There can be guide function under additional magnetic fields.At present, magnetic composite microsphere is widely used in biomedical, cytology and divides
From numerous areas such as engineerings.
The histidine-tagged production process for having been widely used for protein is coagulated using agarose of the coordination with reference to nickel ion
Glue can adsorb histidine-tagged protein quickly and with high selectivity, and improve protein isolates and purifies speed, reduces egg
The purifying cost of white matter, several functions protein have used this production technology to complete merchandized handling and application.
In the production process of these functional proteins, coordination is high with reference to the Ago-Gel price of nickel ion, during isolating and purifying
Shared production cost ratio is excessive, and therefore, exploitation is quick, protein separation method efficiently, inexpensive is always albumen
The bottleneck of matter industry development.
The content of the invention
The present invention is high with reference to the Ago-Gel price of nickel ion to solve coordination in the prior art, pure separating
The excessive deficiency of shared production cost proportion during changing, provides a kind of iron-nickel magnetic microballoon for adulterating cobalt ions, Ke Yizhi
Absorption histidine-tagged protein is connect, and magnetic microsphere is based on thermal decomposition principle and is prepared using one kettle way, and production cost is low, doping
The magnetic microsphere of cobalt ions is to the iron-nickel magnetic microballoon of the adsorption capacity of histidine-tagged protein higher than no ZnO thin film.
The present invention inventive concept be：Iron, nickel, cobalt are most common ferromagnetic materials, may be used to magnetic microsphere system
Standby, we study the performance influence of cation doping ion pair iron-nickel magnetic microballoon therefore；It finds in the course of the research, a small amount of cation doping
Ion can improve adsorption capacity of the iron-nickel magnetic microballoon to histidine-tagged protein.
Technical scheme is specific as follows：A kind of iron-nickel magnetic microballoon for adulterating cobalt ions, in magnetic ball preparation process
Cobalt ions and nickel ion are used in mixed way, the cobalt ions accounts for the 20-30% of cobalt ions and nickel ion total mole number, is preferably
25%.
Further, the cobalt ions is bivalent cation, and existence form is chloride, sulfate, nitrate.
Further, the cobalt ions, nickel ion, iron ion grinding in advance is uniformly used further to magnetic microsphere preparation.
Further, the iron-nickel magnetic microballoon is prepared using one kettle way, is as follows：
A. soluble ferric iron salt, soluble nickel salt, soluble cobalt by certain mol proportion are mixed, makes original by constantly grinding
Material is uniformly mixed；The soluble ferric iron salt, soluble nickel salt, the convenient source that soluble cobalt is this field, such as：Chlorination
Iron, ferric sulfate, ferric nitrate, nickel chloride, nickel sulfate, nickel nitrate, cobalt chloride, cobaltous sulfate, cobalt nitrate.
B. ethylene glycol under the conditions of 200 DEG C is stirred, and is continually fed into the abundant deoxygenation of nitrogen；
C. under nitrogen protective condition, addition sodium acetate, ethanolamine stir evenly, and addition is pre-mixed uniform solubility
Molysite, soluble nickel salt, soluble cobalt raw material, stirred under nitrogen atmosphere reaction 6h, are then cooled to room under nitrogen protection
Temperature simultaneously stops reacting；
D. the product obtained in step c is washed with deionized 5-7 times, ethanol solution washs 10-15 times, and doping is made
The iron-nickel magnetic microballoon of cobalt ions；
Another object of the present invention is to protect the iron-nickel magnetic microballoon of above-mentioned doping cobalt ions in protein purification
Using, adulterate cobalt ions iron-nickel magnetic microballoon prepare after without additionally modification may be directly applied to histidine-tagged protein point
From purifying.
Experiment through inventor confirms that the iron-nickel magnetic microballoon of doping cobalt ions provided by the invention is to histidine-tagged egg
There is high-affinity in vain, binding ability is better than the iron-nickel magnetic microballoon of no ZnO thin film.
Magnetic microsphere is mixed with crude protein extracting solution, by centrifugation or magnet adsorption, target protein absorption is magnetic micro-
On ball, by the magnetic microsphere with target protein with after appropriate buffer solution for cleaning, the elution buffer containing high concentration imidazoles can be used
Liquid will be eluted with histidine-tagged target protein from magnetic microsphere.
The histidine-tagged principle for protein purification is：Histidine is the amino acid for having heterocycle, each histidine
Containing there are one imidazole group, imidazole group is combined by lone pair electrons with metallic ion coordination.Histidine-tagged is continuous 6 groups
The function section of propylhomoserin, is combined with high-affinity with the metal ion of immobilization, for isolating and purifying for protein.
Compared with prior art, the beneficial effects of the invention are as follows：
(1) the iron-nickel magnetic microballoon of the doping cobalt ions synthesized by the present invention can be directly used for purifying histidine-tagged egg
In vain, without carrying out other modifications, such as antibody modification on magnetic microsphere surface.
(2) the iron-nickel magnetic microballoon of doping cobalt ions produced by the present invention, good dispersion, and application effect is quickly high
Effect, better than the iron-nickel magnetic microballoon of no cobalt doped.
(3) it is of the present invention doping cobalt ions iron-nickel magnetic microballoon using one kettle way prepare, preparation method simply, into
Sheet is low, easily carries out large-scale industrial production.
Description of the drawings
Fig. 1 is the dispersiveness of the iron-nickel magnetic microballoon of doping cobalt ions and adsorptivity detection figure；
Wherein：A, identical bacteria lysis supernatant adulterates the dispersiveness of the iron-nickel magnetic microballoon of cobalt ions in water b,
Detection, c, aggregation of the iron-nickel magnetic microballoon in magnetic field for adulterating cobalt ions and the absorption to albumen.
Fig. 2 is influence schematic diagram of the cobalt ions substitute proportion to the protein adsorption capacity of magnetic microsphere；
Wherein：Ordinate accounts for the percentage of former Tot Prot for residual protein after magnetic microsphere absorption.
The average grain diameter of the magnetic microsphere of Fig. 3 difference cobalt ions substitute proportions；
Fig. 4 elutes the comparison of result after being five kinds of histidine-tagged GFP of magnetic microsphere junction belt；
Wherein, M：Protein molecular weight standard, 1：Centrifuged supernatant after bacteria lysis, 2：The magnetism of 15% degree of substitution is micro-
Supernatant after ball absorption, 3：The magnetic microsphere eluted product of 15% degree of substitution, 4：After the magnetic microsphere absorption of 20% degree of substitution
Supernatant, 5：The magnetic microsphere eluted product of 20% degree of substitution, 6：Supernatant after the magnetic microsphere absorption of 25% degree of substitution, 7：
The magnetic microsphere eluted product of 25% degree of substitution, 8：Supernatant after the magnetic microsphere absorption of 30% degree of substitution, 9：30% degree of substitution
Magnetic microsphere eluted product, 10：Supernatant after the magnetic microsphere absorption of 35% degree of substitution, 11：The magnetism of 35% degree of substitution is micro-
Ball eluted product.
After Fig. 5 is the magnetic microsphere combination His-tag-GFP of 25% degree of substitution, the comparison knot of imidazole concentration and eluting power
Fruit detects (SDS-PAGE)；
Wherein, M：Protein molecular weight standard, 1：Centrifuged supernatant after bacteria lysis, 2：The magnetic microsphere of 25% degree of substitution
Supernatant after absorption, 3-8：The elution effect of the different eluent of imidazoles final concentration compares, and wherein imidazoles final concentration is respectively：
0.20mol/L, 0.25mol/L, 0.3mol/L, 0.5mol/L, 1mol/L and 2mol/L.
Fig. 6 is Ago-Gel (Ni-NTA of the magnetic microsphere of 25% degree of substitution with import coordination with reference to nickel ion
Agarose performance comparison result)；
Wherein, M：Protein molecular weight standard, 1：Not plus the supernatant of derivant bacterial lysate；2：Bacteria lysis after induction
The supernatant of liquid；3：The direct sample preparation detection of thalline after induction；4：Centrifuged supernatant after Ago-Gel absorption；5：Ago-Gel is inhaled
Attached eluate；6：Centrifuged supernatant after the magnetic microsphere absorption of 25% degree of substitution；7：The magnetic microsphere absorption of 25% degree of substitution
Eluate afterwards.
Specific embodiment
The invention will be further described for 1-6 and specific embodiment below in conjunction with the accompanying drawings.Following embodiment simply describes
Property, it is not limited, it is impossible to which protection scope of the present invention is limited with this.The chemical reagent and instrument that the present invention is applied
Such as without illustrating, can be bought from commercial channel.Preferably, three kinds of metal salts select cobalt nitrate, nickel sulfate, trichlorine respectively
Change iron, be purchased from Sinopharm Chemical Reagent Co., Ltd..
Embodiment 1
By cobalt nitrate, nickel sulfate in molar ratio 1:4 mixing (are denoted as 20%, it is total with nickel ion to represent that cobalt ions accounts for cobalt ions
The 20% of molal quantity), then mixed with iron ion, it is fully ground after mixing to adulterate the preparation of the iron nickel magnetic ball of cobalt ions.Magnetic
Ball preparation is based on thermal decomposition method principle, is prepared and completed using one kettle way, metal cation salt after mixing is added under nitrogen protection
Enter into 200 DEG C of ethylene glycol solution (abundant deoxygenation, and add in sodium acetate, ethanolamine stirs evenly), keep nitrogen protect
6h is stirred to react under the conditions of shield, be then cooled to room temperature under nitrogen protection and stops reacting；By synthetic product deionized water
Washing 5 times, ethanol solution wash 5 times, and the iron nickel magnetic ball of 20% doping cobalt ions is made.
Embodiment 2
Cobalt nitrate, nickel sulfate are pressed to the molar ratio 1 of ion:3 mixing (are denoted as 25%, represent that cobalt ions accounts for cobalt ions and nickel
The 25% of ion total mole number), then mixed with iron ion, it is fully ground after mixing to adulterate the system of the iron nickel magnetic ball of cobalt ions
It is standby.The preparation of magnetic ball is based on thermal decomposition method principle, is prepared and completed using one kettle way, and metal cation salt after mixing is protected in nitrogen
Under be added in 200 DEG C of ethylene glycol solution (abundant deoxygenation, and add in sodium acetate, ethanolamine stirs evenly), keep nitrogen
6h is stirred to react under the conditions of gas shielded, be then cooled to room temperature under nitrogen protection and stops reacting；By synthetic product spend from
Sub- water washing 7 times, ethanol solution wash 15 times, and the iron nickel magnetic ball of 25% doping cobalt ions is made.
Embodiment 3
Cobalt nitrate, nickel sulfate are pressed to the molar ratio 3 of ion:7 mixing (are denoted as 30%, represent that cobalt ions accounts for cobalt ions and nickel
The 30% of ion total mole number), then mixed with iron ion, it is fully ground after mixing to adulterate the system of the iron nickel magnetic ball of cobalt ions
It is standby.The preparation of magnetic ball is based on thermal decomposition method principle, is prepared and completed using one kettle way, and metal cation salt after mixing is protected in nitrogen
Under be added in 200 DEG C of ethylene glycol solution (abundant deoxygenation, and add in sodium acetate, ethanolamine stirs evenly), keep nitrogen
6h is stirred to react under the conditions of gas shielded, be then cooled to room temperature under nitrogen protection and stops reacting；By synthetic product spend from
Sub- water washing 6 times, ethanol solution wash 10 times, and the iron nickel magnetic ball of 30% doping cobalt ions is made.
Embodiment 4
Cobalt nitrate, nickel sulfate are pressed to the molar ratio 7 of ion:13 mixing (are denoted as 35%, represent that cobalt ions accounts for cobalt ions and nickel
The 35% of ion total mole number), then mixed with iron ion, it is fully ground after mixing to adulterate the system of the iron nickel magnetic ball of cobalt ions
It is standby.The preparation of magnetic ball is based on thermal decomposition method principle, is prepared and completed using one kettle way, and metal cation salt after mixing is protected in nitrogen
Under be added in 200 DEG C of ethylene glycol solution (abundant deoxygenation, and add in sodium acetate, ethanolamine stirs evenly), keep nitrogen
6h is stirred to react under the conditions of gas shielded, be then cooled to room temperature under nitrogen protection and stops reacting；By synthetic product spend from
Sub- water washing 5 times, ethanol solution wash 15 times, and the iron nickel magnetic ball of 35% doping cobalt ions is made.
Embodiment 5
Cobalt nitrate, nickel sulfate are pressed to the molar ratio 3 of ion:17 mixing (are denoted as 15%, represent that cobalt ions accounts for cobalt ions and nickel
The 15% of ion total mole number), then mixed with iron ion, it is fully ground after mixing to adulterate the system of the iron nickel magnetic ball of cobalt ions
It is standby.The preparation of magnetic ball is based on thermal decomposition method principle, is prepared and completed using one kettle way, and metal cation salt after mixing is protected in nitrogen
Under be added in 200 DEG C of ethylene glycol solution (abundant deoxygenation, and add in sodium acetate, ethanolamine stirs evenly), keep nitrogen
6h is stirred to react under the conditions of gas shielded, be then cooled to room temperature under nitrogen protection and stops reacting；By synthetic product spend from
Sub- water washing 7 times, ethanol solution wash 15 times, and the iron nickel magnetic ball of 15% doping cobalt ions is made.
Embodiment 6
Cobalt nitrate, nickel sulfate are pressed to the molar ratio 1 of ion:1 mixing (is denoted as 50%, represents that cobalt ions accounts for cobalt ions and nickel
The 50% of ion total mole number), then mixed with iron ion, it is fully ground after mixing to adulterate the system of the iron nickel magnetic ball of cobalt ions
It is standby.The preparation of magnetic ball is based on thermal decomposition method principle, is prepared and completed using one kettle way, and metal cation salt after mixing is protected in nitrogen
Under be added in 200 DEG C of ethylene glycol solution (abundant deoxygenation, and add in sodium acetate, ethanolamine stirs evenly), keep nitrogen
6h is stirred to react under the conditions of gas shielded, be then cooled to room temperature under nitrogen protection and stops reacting；By synthetic product spend from
Sub- water washing 6 times, ethanol solution wash 10 times, and the iron nickel magnetic ball of 50% doping cobalt ions is made.
Embodiment 7
It only uses nickel sulfate and prepares magnetic ball, the cobalt ions that undopes (is denoted as 0%, represent without cobalt ions, as control), directly
It connects and is mixed with nickel sulfate with iron ion, be fully ground after mixing to compare the preparation of iron nickel magnetic ball.The preparation of magnetic ball is based on heat
Decomposition method principle is prepared using one kettle way and completed, metal cation salt after mixing is added to 200 DEG C of second two under nitrogen protection
In alcoholic solution (abundant deoxygenation, and add in sodium acetate, ethanolamine stirs evenly), keep nitrogen protective condition under be stirred to react
Then 6h is cooled to room temperature and stops reacting under nitrogen protection；Synthetic product is washed with deionized 7 times, ethanol solution
The control iron nickel magnetic ball without ZnO thin film is made in washing 5 times.
Cobalt ions is adulterated in iron nickel magnetic ball preparation process, absorption of the magnetic ball to histidine-tagged protein can be improved；Its
In, bivalent cation is used in mixed way cobalt ions and nickel ion, and cobalt ions accounts for bivalent cation (cobalt ions and nickel ion) and always rubs
Effect is good when the ratio of your number is 20-30%.
Contrast experiment is carried out by 25% magnetic ball of ZnO thin film ratio, by the magnetic ball that ZnO thin film ratio is 25%
With containing bacteria lysis supernatant mix, centrifuged after being sufficiently mixed and supernatant and measure protein residues amount, after absorption
Supernatant residual protein accounts for the 23.08% of former Tot Prot, and is 49.62% without cobalt ions control magnetic ball, 25% ZnO thin film
The protein adsorption capacity of magnetic ball be doubled (see attached drawing 2).
ZnO thin film ratio for 15%-35% magnetic balls average grain diameter between 274.03nm-290.63nm (see attached drawing
3) protein absorption, is used equally for (see attached drawing 4, attached drawing 5).
The histidine-tagged protein adsorbed on iron nickel magnetic ball can be separated using the eluent containing imidazoles, complete mesh
Mark albumen isolates and purifies (see attached drawing 5).Adulterate cobalt ions iron nickel magnetic ball histidine-tagged protein separating property with into
The coordination of mouth is suitable (see attached drawing 6) with reference to Ago-Gel (Ni-NTA agarose) performance of nickel ion, and can realize magnetic
Property separation, imported material can be substituted completely.
Claims (1)
1. it is a kind of adulterate cobalt ions iron-nickel magnetic microballoon, which is characterized in that be used in mixed way in magnetic ball preparation process cobalt ions with
Nickel ion, the cobalt ions account for the 25% of cobalt ions and nickel ion total mole number；
The cobalt ions is bivalent cation, and existence form is chloride, sulfate, nitrate；
The grinding in advance of the cobalt ions, nickel ion, iron ion is uniformly used further to magnetic microsphere preparation；
The iron-nickel magnetic microballoon is prepared using one kettle way, is as follows：
A. soluble ferric iron salt, soluble nickel salt, soluble cobalt are mixed in certain molal quantity ratio, by constantly grinding
Mill is uniformly mixed raw material；
B. ethylene glycol under the conditions of 200 DEG C is stirred, and is continually fed into the abundant deoxygenation of nitrogen；
C. under nitrogen protective condition, addition sodium acetate, ethanolamine stir evenly, and addition is pre-mixed uniform soluble iron
Salt, soluble nickel salt, soluble cobalt raw material, stirred under nitrogen atmosphere reaction 6h, are then cooled to room temperature under nitrogen protection
And stop reacting；
D. the product obtained in step c is washed with deionized 5-7 times, ethanol solution washs 10-15 time, obtained cation doping from
The iron-nickel magnetic microballoon of son.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711358048.XA CN108043372A (en) | 2017-06-06 | 2017-06-06 | A kind of iron-nickel magnetic microballoon for adulterating cobalt ions |
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| CN201711358048.XA CN108043372A (en) | 2017-06-06 | 2017-06-06 | A kind of iron-nickel magnetic microballoon for adulterating cobalt ions |
| CN201710417423.7A CN107175089A (en) | 2017-06-06 | 2017-06-06 | A kind of iron-nickel magnetic microballoon of cobalt ions that adulterates and its application |
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| CN108554412B (en) * | 2018-05-11 | 2020-10-30 | 江西理工大学 | Preparation method and application of large-size high-porosity Fe-doped photocatalytic magnetic porous microspheres |
| CN110038533B (en) * | 2019-04-04 | 2020-08-04 | 深圳市南科征途有限公司 | High-magnetism micro-particle size nanometer magnetic bead and preparation method thereof |
| CN109954517A (en) * | 2019-04-28 | 2019-07-02 | 大连民族大学 | A kind of Au@NH2- MIL-125 nanometers of enzyme catalysts and preparation method thereof |
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