CN104480145A - Preparation method for high fluorescence efficiency glutathione encapsulated iron-based heterojunctions - Google Patents
Preparation method for high fluorescence efficiency glutathione encapsulated iron-based heterojunctions Download PDFInfo
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- CN104480145A CN104480145A CN201510010980.8A CN201510010980A CN104480145A CN 104480145 A CN104480145 A CN 104480145A CN 201510010980 A CN201510010980 A CN 201510010980A CN 104480145 A CN104480145 A CN 104480145A
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Abstract
The invention relates to a preparation method for high fluorescence efficiency glutathione encapsulated iron-based heterojunctions. The method includes the first step of adopting shewanella putrefaciens MR-1 to restore goethite to obtain nanoscale ferrite and introducing seven kinds of divalent transition metal ions (magnesium, manganese, cobalt, nickel, zinc magnesium, zinc manganese and zinc nickel) to replace ferrous sulfate to obtain core-shell type iron-based heterojunctions of hematite-ferrite, and the second step of dissolving the heterojunctions in a mixed solution of glutathione and calcium chloride, and freezing and drying the mixed solution after the mixed solution is kept in a dark place and stands to obtain the glutathione encapsulated iron-based heterojunctions. According to the method, multiple structures of the heterojunctions with hematite (core)-transition metal modified ferrite-glutathione (two shell layers) are obtained and can be applied to the fields of magnetic resonance imaging, targeted drug delivery, magnetic thermal therapy and the like.
Description
Technical field
The present invention relates to a kind of method preparing high fluorescence efficiency gsh encapsulation iron-based heterojunction, belong to field of compound material.
Background technology
Nano composite granules can the external stimulus such as response temperature, magnetic field, light fast, this can be applicable to biomedical sector, and the such as image-forming contrast medium of Superparamagnetic Iron Oxide nano particle has been widely used in nuclear magnetic resonance, target administration and magnetic thermotherapy etc.In order to meet clinical requirement, the surface of image-forming contrast medium must can in order to tackle the chemical stability of outside temperature and light stimulus and improvement simultaneously by official.At present, magnetic and luminescent material combine the hot subject having become cell marking research.They can by utilizing nuclear magnetic resonance identification intra-operative malignant tissue and the high resolving power fluorescence imaging of Noninvasive, to determine borderline tumor and detailed ubcellular information, to improve the method for operative treatment cancer.Variously merge magnetic nanoparticle, to produce difunctionality nanoparticle.Recently, report the luminescence probe of double stimuli responsive compound such as pH and temperature response as quantum dot and organic dye, study wider material and mostly be that gsh (GSH) encapsulates cadmium telluride, gsh (GSH) encapsulates the fluorescence quantums such as zinc sulphide, but seldom have the report of multifunctional nanoparticle (fluorescence, magnetic and photosensitive).
In numerous fluorescent material to be selected, Z 250 with cheap, bio-toxicity is low, the advantages such as synthesis, ferromagnetism that are easy to have attracted the sight of investigator, but easily occur that doublet degeneracy proceeds to the electron transport mode of triplet state when single ferroferric oxide nano granules and the effect of surface biological small molecules, i.e. fluorescent quenching.In order to solve the fluorescent quenching problem of ferroferric oxide nano granules, multiple transition metal and organism are modified for the electrical conductivity of heterojunction.But, traditional physics or chemical process be all difficult to avoid because of high temperature annealing produce inorganic material surface defect and organic materials molecule aging.In addition, adopt N-shaped rhombohedral iron ore shell coated p-type ferrite kernel easily to cause the transformation of effective electron direction of transfer in heterojunction, the magnetic of reduction nanometer cladding and particle surface catch the speed in effective electron and hole.Therefore, Xi Washi Oneida lake MR-1(Gram-negative, facultative anaerobe is adopted) under room temperature price modification, develop seven kinds of single transition metal modification rhombohedral iron ore and soft magnetic bodies.The object of this work is that investigation iron-based heterojunction is on the impact of gsh (GSH) fluorescent characteristic.The material of the method synthesis is compared with prior art: have the advantages such as hypotoxicity, low surface defect, photo-thermal magnetic is multi-functional.
Summary of the invention
The object of the invention is, a kind of method preparing high fluorescence efficiency gsh encapsulation iron-based heterojunction is provided, the method the method is carried out in two steps, the first step: adopt Shewanella putrefaciens MR-1 reduction pyrrhosiderite to obtain nano-ferrite, and introduce seven kinds of divalent transition metal ion magnesium, manganese, cobalt, nickel, zinc-magnesium, zinc-manganese and zinc-nickels replacement ferrous irons, obtain rhombohedral iron ore-ferritic core-shell type iron-based heterojunction; Second step: dissolved in by heterojunction in gsh and calcium chloride mixing solutions, lucifuge leaves standstill 12 hours postlyophilizations, obtains gsh encapsulation iron-based heterojunction.The method obtains the multiple heterojunction structure with rhombohedral iron ore (kernel)-transition metal modification ferrite-gsh (bivalve layer), can be applicable to the fields such as nuclear magnetic resonance, target administration and magnetic thermotherapy.
A kind of method preparing high fluorescence efficiency gsh encapsulation iron-based heterojunction of the present invention, follows these steps to carry out:
A, be chromium chloride by transition metal, cobalt chloride, Manganous chloride tetrahydrate, nickelous chloride mixes with ferric chloride hexahydrate respectively, or composite mixed transition metal zinc chloride-magnesium chloride, zinc chloride-Manganous chloride tetrahydrate, zinc chloride-nickelous chloride mixes with ferric chloride hexahydrate respectively, then each mixture is refluxed 2 hours respectively under the aqueous nitric acid condition of temperature 85 DEG C with pH 2, leave standstill, true temp 50 DEG C of dryings 20 hours, obtain seven kinds of single transition metal and modify rhombohedral iron ore and soft magnetic bodies, wherein transition metal ion: iron ion mol ratio 1:2, composite mixed transition metal ion: iron ion mol ratio is 0.5:0.5:2,
B, by 30 grams per liter Shewanella putrefaciens MR-1 pancreas peptone soybean broth culture medium culturing 48 hours, under temperature 5 DEG C of freezing conditions centrifugal go out MR-1 bacterial classification, seven kinds that centrifugal MR-1 bacterial classification and step a are obtained single transition metal modification rhombohedral iron ore and soft magnetic bodies 90 mmole join in Mineralized Culture base respectively, regulator solution pH value is 6, and add 1 simultaneously, 4-piperazine two ethyl sulfonic acid and anthraquinone-2,6-disulfonate is alleviated cell and is contacted with FeO (OH) powder, and wherein Mineralized Culture base component is (NH
4)
2sO
49.0mM, K
2hPO
45.7 mM, KH
2pO
43.3 mM, NaHCO
32.0 mM, MgSO
47H
2o 1.01 mM, CaCl
22H
2o 0.485 mM, Sytron 67.2 μMs, H
3bO
356.6 μMs, NaCl 10.0 μMs, FeSO
47H
2o 5.4 μMs, CoSO
45.0 μMs, Ni (NH
4)
2(SO
4)
25.0 μMs, Na
2moO
43.87 μMs, Na
2seO
41.5 μMs, MnSO
41.26 μMs, ZnSO
41.04 μMs, CuSO
40.2 μM, arginase 12 0mg/L, L-glutamic acid 20 mg/L and Serine mg/L;
C, by reaction solution anaerobic sealing of step b, keep in Dark Place 45 days under temperature 30 DEG C of conditions, centrifugal, true temp 70 DEG C of dryings 48 hours, obtain iron-based heterojunction;
D, the iron-based heterojunction that step c is obtained be dissolved in 0.5-1 mmole/gram gsh and calcium chloride mixing the aqueous solution, be made into mol ratio iron-based heterojunction: gsh: the mixing solutions of calcium chloride=1:1:2, sonic oscillation, leave standstill 12 hours, after lyophilize, obtain the iron-based heterojunction of gsh encapsulation.
A kind of method preparing high fluorescence efficiency gsh encapsulation iron-based heterojunction of the present invention, Shewanella putrefaciens MR-1(Gram-negative involved in the method, facultative anaerobe) for buying product, by Midland, MI university, China University of Geosciences, Dong's current chart seminar of Xinan Science and Technology Univ. provides, Shewanella putrefaciens MR-1 genome is 42c type cytopigment, cytopigment (the Trypsin pigment A-OmcA of extracellular matrix, Trypsin pigment C-MtrC and Trypsin pigment B-MtrB) and iron hydrogenase be positioned in the different positions of inner membrance and adventitia, form " molecular line " configuration, provide the path that insoluble electron acceptor(EA) and electronics move turnover cell.
Mineralized Culture base component is that wherein Mineralized Culture base component is (NH
4)
2sO
49.0mM, K
2hPO
45.7 mM, KH
2pO
43.3 mM, NaHCO
32.0 mM, MgSO
47H
2o 1.01 mM, CaCl
22H
2o 0.485 mM, Sytron 67.2 μMs, H
3bO
356.6 μMs, NaCl 10.0 μMs, FeSO
47H
2o 5.4 μMs, CoSO
45.0 μMs, Ni (NH
4)
2(SO
4)
25.0 μMs, Na
2moO
43.87 μMs, Na
2seO
41.5 μMs, MnSO
41.26 μMs, ZnSO
41.04 μMs, CuSO
40.2 μM, arginase 12 0mg/L, L-glutamic acid 20 mg/L and Serine mg/L.
Accompanying drawing explanation
The stereoscan photograph figure of Fig. 1 seven kinds of iron-based heterojunction that to be the present invention obtain through microbial mineralization process in 45 days;
Fig. 2 is that the present invention modifies the Energy Dispersive X-ray spectrum of iron-based heterojunction and zinc-nickel modification iron-based heterojunction through the chromium that microbial mineralization process in 45 days obtains;
Fig. 3 is the inversion fluorescence photo figure of the final product that the present invention obtains after gsh encapsulation iron-based heterojunction under 488 nanometer lasers excite.
Embodiment
Embodiment 1
A, in molar ratio for chromium, cobalt, manganese, nickel: iron=1:2 takes chromium chloride, cobalt chloride, Manganous chloride tetrahydrate, nickelous chloride and ferric chloride hexahydrate raw material mixing respectively, then be reflux in 2 aqueous nitric acid in the pH value of temperature 85 DEG C respectively by each mixture, namely there is peptization back flow reaction in reactant, solution becomes red (chromium), yellow (cobalt), green (manganese) and blue (nickel) look suspension liquid from water white transparency, reaction in 2 hours terminates, temperature 50 C vacuum-drying 20 hours after leaving standstill, obtain khaki color powdered product, namely iron oxide hydroxide modified by four kinds of single transition metal;
B, 30 grams per liter Shewanella putrefaciens MR-1 to be cultivated 48 hours in pancreas peptone soybean broth substratum, under temperature 5 DEG C of freezing conditions centrifugal go out Shewanella putrefaciens MR-1 bacterial classification, four kinds that centrifugal MR-1 bacterial classification and step a are obtained single transition metal are modified iron oxide hydroxide 90 mmoles and are joined Mineralized Culture base component respectively for (NH
4)
2sO
49.0mM, K
2hPO
45.7 mM, KH
2pO
43.3 mM, NaHCO
32.0 mM, MgSO
47H
2o 1.01 mM, CaCl
22H
2o 0.485 mM, Sytron 67.2 μMs, H
3bO
356.6 μMs, NaCl 10.0 μMs, FeSO
47H
2o 5.4 μMs, CoSO
45.0 μMs, Ni (NH
4)
2(SO
4)
25.0 μMs, Na
2moO
43.87 μMs, Na
2seO
41.5 μMs, MnSO
41.26 μMs, ZnSO
41.04 μMs, CuSO
40.2 μM, in arginase 12 0mg/L, L-glutamic acid 20 mg/L and Serine mg/L, adjust ph is 6, and add 0.2 micromoles per liter Isosorbide-5-Nitrae-piperazine two ethyl sulfonic acid and 0.2 micromoles per liter anthraquinone-2,6-disulfonate simultaneously and alleviate cell and contact with FeO (OH) powder;
C, by reaction solution anaerobic sealing of step b, under temperature 30 DEG C of conditions, lucifuge is vibrated 45 days, and namely microorganism Fe occurs reactant
3+-Fe
2+reduction and divalent transition metal replace Fe
2+reaction, surface color becomes khaki color suspension liquid from reddish brown (chromium), the colour of loess (cobalt), light green (manganese) and light blue (nickel) look, red (chromium) look and khaki color powder is obtained after reaction terminates, true temp 70 DEG C of dryings 48 hours, obtain four kinds of single transition metal and modify iron-based heterojunction, the rate of recovery is all greater than 85%;
D, utilize 2 moles of calcium chloride fixing 1 mole of glutathione molecules two ends to electronics end group, obtain the glutathione solution of exposed coloured glaze base, solution is water white transparency shape, then the transition metal that obtained by step c modifies iron-based heterojunction 1 mole and is dissolved in 0.5 milli and rubs/gram gsh and the aqueous solution of calcium chloride mixing, be made into mol ratio iron-based heterojunction: gsh: the mixing solutions of calcium chloride=1:1:2, sonic oscillation, leave standstill 12 hours, namely there is Surface coating reaction in reactant, solution colour becomes muddiness from clarification, obtain gsh after lyophilize and encapsulate single transition metal modification iron-based heterojunction, the rate of recovery 100%, chromium and nickel are modified the local of iron-based heterojunction under 488 nanometers light excite and are occurred enhancement effect of fluorescence, manganese and cobalt are modified iron-based heterojunction and are excited lower generation Fluorescence quenching effect in 488 nanometers light.
Embodiment 2
A, in molar ratio for magnesium, manganese or nickel: zinc: iron=0.5:0.5:2 takes zinc chloride-magnesium chloride, zinc chloride-Manganous chloride tetrahydrate, zinc chloride-nickelous chloride and mixes with ferric chloride hexahydrate raw material respectively, then be reflux in 2 aqueous nitric acid by the pH value of each mixture respectively at temperature 85 DEG C, namely there is peptization back flow reaction in reactant, solution becomes khaki color suspension liquid from water white transparency, reaction in 2 hours terminates, leave standstill, temperature 50 C vacuum-drying 20 hours, obtain khaki color powdered product, namely obtain three kinds of co-modified iron oxide hydroxides of composite mixed transition metal;
B, 30 grams per liter Shewanella putrefaciens MR-1 to be cultivated 48 hours in pancreas peptone soybean broth substratum, under temperature 5 DEG C of freezing conditions centrifugal go out Shewanella putrefaciens MR-1 bacterial classification, four kinds that centrifugal MR-1 bacterial classification and step a are obtained single transition metal are modified iron oxide hydroxide 90 mmoles and are joined Mineralized Culture base component respectively for (NH
4)
2sO
49.0mM, K
2hPO
45.7 mM, KH
2pO
43.3 mM, NaHCO
32.0 mM, MgSO
47H
2o 1.01 mM, CaCl
22H
2o 0.485 mM, Sytron 67.2 μMs, H
3bO
356.6 μMs, NaCl 10.0 μMs, FeSO
47H
2o 5.4 μMs, CoSO
45.0 μMs, Ni (NH
4)
2(SO
4)
25.0 μMs, Na
2moO
43.87 μMs, Na
2seO
41.5 μMs, MnSO
41.26 μMs, ZnSO
41.04 μMs, CuSO
40.2 μM, in arginase 12 0mg/L, L-glutamic acid 20 mg/L and Serine mg/L, adjust ph is 6, and add 0.2 micromoles per liter Isosorbide-5-Nitrae-piperazine two ethyl sulfonic acid and 0.2 micromoles per liter anthraquinone-2,6-disulfonate simultaneously and alleviate cell and contact with FeO (OH) powder;
C, be 6 by the reaction solution adjust ph of step b, anaerobic sealing, under temperature 30 DEG C of conditions, lucifuge is vibrated 45 days, and namely microorganism Fe occurs reactant
3+-Fe
2+reduction and transition metal replace Fe altogether
2+reaction, surface color becomes light yellow suspension liquid from khaki color powder, and obtain khaki color powder, true temp 70 DEG C of dryings 48 hours after reaction terminates, obtain three kinds of co-modified iron-based heterojunction of composite mixed transition metal, the rate of recovery is all greater than 90.5%;
D, utilize the calcium chloride of 2 moles fixing the glutathione molecules two ends of 1 mole to electronics end group, obtain the glutathione solution of exposed coloured glaze base, solution is water white transparency shape, then the transition metal of 1 mole is modified calcium chloride-glutathione solution that iron-based heterojunction is dissolved in 1 mole, sonic oscillation, leave standstill 12 hours, namely there is Surface coating reaction in reactant, solution colour becomes muddiness from clarification, the co-modified iron-based heterojunction of gsh encapsulation transition metal is obtained after lyophilize, the rate of recovery 100%, all enhancement effect of fluorescence is there is in the final product obtained under 488 nanometers light excite, and extent of fluorescence modifies iron-based heterojunction higher than single transition metal.
A kind of method preparing high fluorescence efficiency gsh encapsulation iron-based heterojunction of the present invention, as can be seen from Figure 1 product is the reactant enwrapped granule of below a large amount of 200 nanometers, this illustrates that transition metal all can reduce the surface reunion of iron-based heterojunction, improves the dispersiveness of powder.In addition, judge that product is made up of two phase structure by various granule-morphology; As can be seen from Figure 2 comprise certain density transition metal ion in final product, and judge that transition metal ion has entered in the middle of crystalline network in conjunction with stereoscan photograph; As can be seen from Figure 3 due to the electronic orbit of cobalt or mn ion and iron ion comparatively close, the recombination probability in effective electron and hole is higher, therefore, when gsh (GSH) encapsulates this two kinds of iron-based heterojunction, the effective electron-hole of the electron-donating group-electron-withdrawing group on surface is buried in oblivion by heterojunction, creates quenching of fluorescence.Poor by the electronic orbit improving transition metal ion and iron ion, to produce the transition energy level of multiple gradients of effective electron, the present invention obtains chromium and nickel ion is modified separately or zinc-magnesium and zinc-nickel modify ferrite jointly, and it obviously can strengthen the fluorescence intensity of iron-based heterojunction.
Claims (1)
1. prepare a method for high fluorescence efficiency gsh encapsulation iron-based heterojunction, it is characterized in that following these steps to carry out:
A, be chromium chloride by transition metal, cobalt chloride, Manganous chloride tetrahydrate, nickelous chloride mixes with ferric chloride hexahydrate respectively, or composite mixed transition metal zinc chloride-magnesium chloride, zinc chloride-Manganous chloride tetrahydrate, zinc chloride-nickelous chloride mixes with ferric chloride hexahydrate respectively, then each mixture is refluxed 2 hours respectively under the aqueous nitric acid condition of temperature 85 DEG C with pH 2, leave standstill, true temp 50 DEG C of dryings 20 hours, obtain seven kinds of single transition metal and modify rhombohedral iron ore and soft magnetic bodies, wherein transition metal ion: iron ion mol ratio 1:2, composite mixed transition metal ion: iron ion mol ratio is 0.5:0.5:2,
B, by 30 grams per liter Shewanella putrefaciens MR-1 pancreas peptone soybean broth culture medium culturing 48 hours, under temperature 5 DEG C of freezing conditions centrifugal go out MR-1 bacterial classification, seven kinds that centrifugal MR-1 bacterial classification and step a are obtained single transition metal modification rhombohedral iron ore and soft magnetic bodies 90 mmole join in Mineralized Culture base respectively, regulator solution pH value is 6, and add 1 simultaneously, 4-piperazine two ethyl sulfonic acid and anthraquinone-2,6-disulfonate is alleviated cell and is contacted with FeO (OH) powder, and wherein Mineralized Culture base component is (NH
4)
2sO
49.0mM, K
2hPO
45.7 mM, KH
2pO
43.3 mM, NaHCO
32.0 mM, MgSO
47H
2o 1.01 mM, CaCl
22H
2o 0.485 mM, Sytron 67.2 μMs, H
3bO
356.6 μMs, NaCl 10.0 μMs, FeSO
47H
2o 5.4 μMs, CoSO
45.0 μMs, Ni (NH
4)
2(SO
4)
25.0 μMs, Na
2moO
43.87 μMs, Na
2seO
41.5 μMs, MnSO
41.26 μMs, ZnSO
41.04 μMs, CuSO
40.2 μM, arginase 12 0mg/L, L-glutamic acid 20 mg/L and Serine mg/L;
C, by reaction solution anaerobic sealing of step b, keep in Dark Place 45 days under temperature 30 DEG C of conditions, centrifugal, true temp 70 DEG C of dryings 48 hours, obtain iron-based heterojunction;
D, the iron-based heterojunction that step c is obtained be dissolved in 0.5-1 mmole/gram gsh and calcium chloride mixing the aqueous solution, be made into mol ratio iron-based heterojunction: gsh: the mixing solutions of calcium chloride=1:1:2, sonic oscillation, leave standstill 12 hours, after lyophilize, obtain the iron-based heterojunction of gsh encapsulation.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020187889A1 (en) * | 1999-10-28 | 2002-12-12 | Lauf Robert J. | Mixed oxide nanoparticles and apparatus for making same |
| CN101031513A (en) * | 2004-06-27 | 2007-09-05 | 朱马国际公司 | A method for producing iron oxide nano particles |
-
2015
- 2015-01-10 CN CN201510010980.8A patent/CN104480145B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020187889A1 (en) * | 1999-10-28 | 2002-12-12 | Lauf Robert J. | Mixed oxide nanoparticles and apparatus for making same |
| CN101031513A (en) * | 2004-06-27 | 2007-09-05 | 朱马国际公司 | A method for producing iron oxide nano particles |
Non-Patent Citations (2)
| Title |
|---|
| 欧阳冰洁等: "瓦氏奥奈达菌MR-1还原针铁矿的实验研究及地球化学意义", 《矿物学报》 * |
| 王青等: "还原型和氧化型谷胱甘肽在磁性Fe3O4纳米粒子的吸附组装", 《化学通报》 * |
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