CN109498545B - Preparation method of ionic strength immune magnetic and fluorescent micro motor - Google Patents
Preparation method of ionic strength immune magnetic and fluorescent micro motor Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 39
- 239000006249 magnetic particle Substances 0.000 claims description 37
- 239000004793 Polystyrene Substances 0.000 claims description 16
- 239000011259 mixed solution Substances 0.000 claims description 16
- 229920002223 polystyrene Polymers 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 16
- 238000010008 shearing Methods 0.000 claims description 13
- 238000012986 modification Methods 0.000 claims description 10
- 230000004048 modification Effects 0.000 claims description 10
- XPBBUZJBQWWFFJ-UHFFFAOYSA-N fluorosilane Chemical compound [SiH3]F XPBBUZJBQWWFFJ-UHFFFAOYSA-N 0.000 claims description 8
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- 230000001804 emulsifying effect Effects 0.000 claims description 6
- 239000000839 emulsion Substances 0.000 claims description 6
- VOFUROIFQGPCGE-UHFFFAOYSA-N nile red Chemical compound C1=CC=C2C3=NC4=CC=C(N(CC)CC)C=C4OC3=CC(=O)C2=C1 VOFUROIFQGPCGE-UHFFFAOYSA-N 0.000 claims description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000007850 fluorescent dye Substances 0.000 claims description 4
- 239000004005 microsphere Substances 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000007885 magnetic separation Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000010992 reflux Methods 0.000 claims description 3
- 238000010907 mechanical stirring Methods 0.000 claims 1
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 abstract description 16
- 238000000034 method Methods 0.000 abstract description 9
- 239000000126 substance Substances 0.000 abstract description 7
- 230000036039 immunity Effects 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 3
- 210000001124 body fluid Anatomy 0.000 abstract description 2
- 239000010839 body fluid Substances 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- 239000002245 particle Substances 0.000 description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 230000005389 magnetism Effects 0.000 description 5
- 239000003921 oil Substances 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000011737 fluorine Substances 0.000 description 3
- 229910052731 fluorine Inorganic materials 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 230000005653 Brownian motion process Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005537 brownian motion Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000004043 responsiveness Effects 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 239000002569 water oil cream Substances 0.000 description 1
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/0002—Galenical forms characterised by the drug release technique; Application systems commanded by energy
- A61K9/0009—Galenical forms characterised by the drug release technique; Application systems commanded by energy involving or responsive to electricity, magnetism or acoustic waves; Galenical aspects of sonophoresis, iontophoresis, electroporation or electroosmosis
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K49/00—Preparations for testing in vivo
- A61K49/001—Preparation for luminescence or biological staining
- A61K49/0013—Luminescence
- A61K49/0017—Fluorescence in vivo
- A61K49/0019—Fluorescence in vivo characterised by the fluorescent group, e.g. oligomeric, polymeric or dendritic molecules
- A61K49/0021—Fluorescence in vivo characterised by the fluorescent group, e.g. oligomeric, polymeric or dendritic molecules the fluorescent group being a small organic molecule
- A61K49/0028—Oxazine dyes
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
- A61K9/51—Nanocapsules; Nanoparticles
- A61K9/5107—Excipients; Inactive ingredients
- A61K9/5115—Inorganic compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
- B81B7/00—Microstructural systems; Auxiliary parts of microstructural devices or systems
Abstract
The invention belongs to the technical field of material preparation, and particularly relates to a preparation method of an ionic strength immune magnetic fluorescent micro motor. Most of the existing chemical driving micro-nano motors utilize metal catalysts to decompose hydrogen peroxide to generate chemical energy to drive the motors. The hydrogen peroxide has biotoxicity, so that the hydrogen peroxide is not suitable for the biomedical field in most application scenes, particularly when the hydrogen peroxide is involved. A second disadvantage of chemically driven motors is non-ionic immunity. With the increase of the ionic strength, the movement activity of the chemical driving motor is greatly reduced, the movement capability is greatly weakened, and the motor basically does not move in the ionic strength environment close to human body fluid. A third disadvantage is that the movement time of the chemical drive motor movement is very short. The magnetic fluorescent micron motor prepared by the method has the outstanding advantages of no biotoxicity, ionic strength immunity, infinite movement time and the like, has huge application prospects in the fields of biomedicine and the like, and is expected to fill the blank of the field and realize large-scale practicability of the micro-nano motor in the field of biomedicine.
Description
Technical Field
The invention belongs to the technical field of material preparation, and particularly relates to a preparation method and a specific case demonstration of an ionic strength immune magnetic fluorescent micro motor.
Background
The invention belongs to the technical field of material preparation, and particularly relates to a preparation method of an ionic strength immune magnetic fluorescent micro motor. Most of the existing chemical driving micro-nano motors utilize metal catalysts to decompose hydrogen peroxide to generate chemical energy to drive the motors.
The hydrogen peroxide has biotoxicity, so that the hydrogen peroxide is not suitable for the biomedical field in most application scenes, particularly when the hydrogen peroxide is involved. A second disadvantage of chemically driven motors is non-ionic immunity. Along with the increase of the ionic strength, the motor movement activity is greatly reduced, the movement capability is greatly weakened, and the motor basically does not move in the ionic strength environment close to human body fluid. A third disadvantage is that the movement time of the chemical drive motor movement is very short.
The magnetic fluorescent micron motor prepared by the method has the outstanding advantages of no biotoxicity, ionic strength immunity, infinite movement time and the like, has huge application prospects in the fields of biomedicine and the like, and is expected to fill the blank of the field and realize large-scale practicability of the micro-nano motor in the field of biomedicine.
Disclosure of Invention
In view of three problems in the prior art, the magnetic fluorescent micro motor prepared by the invention overcomes the problems and realizes the application of the micro-nano motor in the field of biological medicine. The magnetic fluorescent micron motor prepared by the invention has the outstanding advantages of no biotoxicity, ionic strength immunity, infinite movement time and the like, has huge application prospect in the fields of biomedicine and the like, and is expected to fill the blank of the field and realize the large-scale practicability of the micro-nano motor in the field of biomedicine.
The preparation method of the magnetic fluorescent micro motor comprises the following steps:
step S1: adding 10-100 mg of magnetic particle ferroferric oxide into a mixed solution of 40mL of deionized water and 200mL of isopropanol, and carrying out ultrasonic treatment for 30min until the magnetic particles are uniformly dispersed in the mixed solution;
as a preferable technical scheme of the method, the usage amount of the magnetic particle ferroferric oxide in the step is preferably 40 mg.
The content of the magnetic particle ferroferric oxide is selected according to the fact that the particles are uniformly dispersed in the mixed solution. When the content is too low, the yield and the productivity are too low, and the practicability is not realized; when the content is too high, the particles are not monodisperse, and agglomerated magnetic particles are easily formed, so that the magnetic performance of a magnetic motor prepared subsequently is influenced.
Step S2: respectively adding 7mL of ammonia water (25 wt%) and 0.1-1.2 mL of tetraethoxysilane into the mixed solution obtained in the step S1, mechanically stirring for 4-6 hours, and carrying out magnetic separation and drying to obtain magnetic particles with silicon-shelled surfaces;
as a preferred technical scheme of the method, the usage amount of the tetraethoxysilane in the step is preferably 0.6 mL.
The content of the tetraethoxysilane is selected according to the fact that a silicon dioxide core-shell structure layer is formed on the surface of the magnetic particles. When the content of the tetraethoxysilane is too low, the formed silicon dioxide coating layer is too thin, and even incomplete coating occurs; when the content of the tetraethoxysilane is too high, the magnetic particles are easy to agglomerate, and further surface modification and use of the magnetic particles are influenced.
Step S3: and (4) adding 60mg of the magnetic particles with the surface silicon-shelled surfaces obtained in the step (S2) into a mixed solution of 50mL of ethanol and 0.3mL-1.0mL of fluorosilane, and heating and refluxing at 80 ℃ for 24 hours to obtain the magnetic particles with oleophylic and modified surfaces.
As a preferred technical scheme of the method, the usage amount of fluorosilane in the step is preferably 0.5 mL.
The content of fluorosilane is selected based on the realization of surface modification of the surface layer of silica from hydrophilic to hydrophobic. The content of fluorosilane is too low, the surface modification effect is poor, and the surface of silicon dioxide still shows hydrophilicity; the content of fluorosilane is too high, the surface modification effect is too good, the magnetic particles are easy to agglomerate, and the subsequent loading and use in the micro-nano motor are influenced.
The magnetic particles prepared by the step have uniform particle size distribution, the particle size is about 300nm, and the specific morphology is shown in figure 1 c.
Step S4: adding 20mg-200mg of the magnetic particles subjected to oleophylic modification on the surface in the step S3 and fluorescent dye nile red into 10mL of toluene solution of polystyrene, wherein the mass fraction of the polystyrene is preferably 3%, the mass fraction of the nile red is preferably 0.02%, and performing ultrasonic treatment and uniformly mixing to obtain the toluene solution of the magnetic polystyrene;
as a preferred embodiment of the method, the step preferably uses 70mg of the oleophilic-surface-modified magnetic particles.
The content of the magnetic particles is selected according to the excellent magnetism given to the micro-nano motor so as to realize the control under the magnetic field. The content of the magnetic particles is too low, the magnetism of the micro-nano motor is too weak, and the controllability of the responsiveness under a magnetic field is weak; the content of the magnetic particles is too high, and the magnetism of the micro-nano motor is too strong, so that the self-connection phenomenon of the micro-nano motor also influences the control performance under a magnetic field.
Step S5: adding 70mL of a sodium dodecyl sulfate solution to 1mL-10mL of the toluene solution of the magnetic polystyrene in the step S4 to obtain a mixed solution;
as a preferred technical scheme of the method, the content of the toluene solution in the step is preferably 10 mL.
The content of the toluene solution is selected based on the formation of a stable oil-water emulsion for shearing. The content of the toluene solution is too small, the oil phase is too small, the cutting of the oil phase is insufficient during shearing, and the shearing efficiency is low; the content of the toluene solution is too high, the oil phase is too high, the volume of the oil phase is too much after shearing, and the oil phase is unstable and is easy to phase split.
Step S6: and (4) emulsifying the mixed emulsion obtained in the step (S5) by using an emulsifying machine, wherein the shearing speed is 3000r/min-25000r/min, and the shearing time is 10min, so as to obtain the emulsion, and mechanically stirring and drying for 2 days to obtain the magnetic polystyrene microspheres, namely the magnetic fluorescent micro-motor.
As a preferred embodiment of the method, the drying temperature is preferably room temperature, and the shear rate in this step is preferably room temperature
6000r/min。
The shearing speed is selected according to the appropriate optical observation and magnetic field control of the particle size of the micro-nano motor. The shearing speed is too small, the micro-nano motor is too large, and the micro-nano motor is not suitable for micro-nano observation and magnetic field control of a microscope; the shearing speed is too high, the micro-nano motor is too small, the resolution of a microscope cannot be observed, and the Brownian motion is too strong and is not suitable for magnetic field control.
The magnetic fluorescent micromotor is placed under a scanning electron microscope to observe morphology and element analysis, the particle size is about 5 micrometers, the magnetic fluorescent micromotor contains carbon elements, iron elements, oxygen elements and fluorine elements, and specific morphology characteristics and element analysis results are shown in fig. 2; the figure clearly shows that the carbon element, the iron element, the oxygen element and the fluorine element correspond to the micro-nano motor prepared by the user, the specific content of each element in the micro-nano motor can be further determined by a table attached to the figure, and the components and the composition of the motor can be further confirmed.
The beneficial effects of the invention compared with the prior art comprise:
(1) the micron motor prepared by the invention is not influenced by the ionic strength in the system, namely, the ionic strength immunity.
(2) The invention introduces the magnetic particles and the fluorescent dye into the micrometer motor by a one-step method, is simple and convenient, and realizes the functionalization of the motor magnetism, fluorescence and the like.
(3) The motor of the invention has magnetism which can be guided by an external magnetic field, which means that the micron motor can be guided by the magnetic field and is basically harmless to human bodies if being applied to medicine carrying in the future, and simultaneously has fluorescence which is convenient for medical development and imaging.
Drawings
FIG. 1 is a schematic diagram of a magnetic particle prepared according to the present invention, wherein a) the magnetic particle is schematically modified; b) a magnetic particle SEM; c) covering the surface of the magnetic particles with a silicon dioxide layer by SEM; d) performing fluorosilane modification on the surfaces of the magnetic particles by using SEM;
FIG. 2, SEM and EDS schematic of a magnetic fluorescent micromotor made according to the present invention;
FIG. 3 shows the motion of the micrometer motor along the broken line locus at different times;
fig. 4 shows the movement of the writing trace of the micrometer motor at different moments.
FIG. 5 is a flow chart of the motor assembly and application of the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the embodiments of the invention are not limited thereto.
Example 1
A method of making a magnetic and fluorescent micromotor comprising the steps of:
step S1: adding 40mg of magnetic particle ferroferric oxide into a mixed solution of 40mL of deionized water and 200mL of isopropanol, and carrying out ultrasonic treatment for 30min until the magnetic particles are uniformly dispersed in the mixed solution;
step S2: respectively adding 7mL of ammonia water (25 wt%) and 0.6mL of ethyl orthosilicate into the mixed solution obtained in the step S1, mechanically stirring for 4-6 hours, and carrying out magnetic separation and drying to obtain magnetic particles with silicon-shelled surfaces;
step S3: and (4) adding the magnetic particles with the surface silicon-shelled obtained in the step (S2) into a mixed solution of 50mL of ethanol and 0.5mL of fluorosilane, and heating and refluxing for 24 hours at 80 ℃ to obtain the magnetic particles with oleophilic and modified surfaces. The magnetic particles have uniform particle size distribution, the particle size is about 300nm, and the specific morphology is shown in figure 1;
step S4: 70mg of the magnetic particles subjected to oleophylic modification on the surface in the step S3 and the fluorescent dye Nile Red are added into 10mL of a toluene solution of polystyrene (the mass fraction of the polystyrene is 3%, and the mass fraction of the Nile Red is 0.02%), and the toluene solution of the magnetic polystyrene is obtained after ultrasonic treatment and uniform mixing;
step S5: adding 70mL of a sodium dodecyl sulfate solution to 10mL of the toluene solution of magnetic polystyrene in the step S4 to obtain a mixed solution;
step S6: emulsifying the mixed emulsion obtained in the step S5 by using an emulsifying machine, wherein the shearing speed is 6000r/min, the shearing time is 10min, obtaining the emulsion, mechanically stirring and drying for 2 days to obtain the magnetic polystyrene microsphere, namely the magnetic fluorescent micromotor, observing the morphology and element analysis under an electron microscope, wherein the particle size is about 5 microns, the magnetic polystyrene microsphere contains the carbon elements, the iron elements, the oxygen elements and the fluorine elements, and the specific result is shown in figure 2. The motor composition and application flow are shown in fig. 5.
Example 2 Performance testing
The micromotor prepared in example 1 was placed in deionized water and allowed to move in a precise orientation under the control of a magnetic field of about 90 gauss average intensity to allow adequate observation under a microscope field of view and independent of ion intensity.
The magnetic field is controlled according to the pattern shown in fig. 3, and the motor moves as a broken line track shown in fig. 3.
Example 3 Performance testing
The micromotor prepared in example 1 was placed in deionized water and allowed to move in a precise orientation under the control of a magnetic field of about 90 gauss average intensity to allow adequate observation under a microscope field of view and independent of ion intensity.
The magnetic field is controlled according to the pattern shown in fig. 4, and the motor moves as a broken line track shown in fig. 4.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (1)
1. The preparation method of the magnetic fluorescent micrometer motor is characterized in that,
step S1: adding 40mg of magnetic particle ferroferric oxide into a mixed solution of 40mL of deionized water and 200mL of isopropanol, and carrying out ultrasonic treatment for 30min until the magnetic particles are uniformly dispersed in the mixed solution;
step S2: respectively adding 7mL of ammonia water with the concentration of 25 wt% and 0.6mL of ethyl orthosilicate into the mixed solution obtained in the step S1, mechanically stirring for 4-6 hours, and carrying out magnetic separation and drying to obtain magnetic particles with silicon-shelled surfaces;
step S3: adding the magnetic particles with the surface silicon-shelled obtained in the step S2 into a mixed solution of 50mL of ethanol and 0.5mL of fluorosilane, and heating and refluxing for 24 hours at 80 ℃ to obtain surface oleophylic modified magnetic particles;
step S4: 70mg of the magnetic particles subjected to oleophylic modification on the surface in the step S3 and the fluorescent dye Nile Red are added into 10mL of a toluene solution of polystyrene, wherein the mass fraction of the polystyrene is 3%, the mass fraction of the Nile Red is 0.02%, and the toluene solution of the magnetic polystyrene is obtained after ultrasonic treatment and uniform mixing;
step S5: adding 70mL of a sodium dodecyl sulfate solution to 10mL of the toluene solution of magnetic polystyrene in the step S4 to obtain a mixed solution;
step S6: emulsifying the mixed emulsion obtained in the step S5 by using an emulsifying machine, wherein the shearing speed is 6000r/min, the shearing time is 10min, the emulsion is obtained, and the magnetic polystyrene microspheres, namely the magnetic fluorescent micrometer motor, are obtained after mechanical stirring and drying for 2 days, and the element composition is as follows:
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