CN109365128B - Magnetic particle field flow separation device and method based on rotating magnetic field - Google Patents
Magnetic particle field flow separation device and method based on rotating magnetic field Download PDFInfo
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- CN109365128B CN109365128B CN201811327163.5A CN201811327163A CN109365128B CN 109365128 B CN109365128 B CN 109365128B CN 201811327163 A CN201811327163 A CN 201811327163A CN 109365128 B CN109365128 B CN 109365128B
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Abstract
The invention discloses a magnetic particle field flow separating device and a method based on a rotating magnetic field, wherein the device comprises a three-phase winding; the three-phase winding comprises a first phase winding, a second phase winding and a third phase winding; the first phase winding, the second phase winding and the third phase winding are in star connection and are symmetrically arranged on the base by taking the axis of the base as an axis; the head ends of the first phase winding, the second phase winding and the third phase winding are respectively communicated with the output end of a three-phase power supply, and the output current of the three-phase power supply is symmetrical three-phase sinusoidal alternating current; the base is a hollow structure, and a separation channel is arranged in the space enclosed by the base. The invention puts the separation channel into the internal cylindrical space formed by the three-phase winding and the base, and adjusts the three-phase voltage and frequency applied to the three-phase winding through the frequency converter. The frequency of the magnetic particles under the action of the rotating magnetic field is controlled, the magnetic induction intensity of the separation channel is changed, and the field flow separation of the magnetic particles with different particle sizes or the same particle size and different magnetic susceptibilities is realized.
Description
Technical Field
The invention relates to the field of magnetic particle analysis and separation, in particular to a magnetic particle field flow separation device and a magnetic particle field flow separation method based on a rotating magnetic field.
Background
The magnetic particles have wide application prospect in the fields of magnetic medicine manufacturing, magnetic resonance imaging, magnetic thermotherapy, cell screening and the like, and the research of the magnetic particles and the microspheres greatly promotes the development of biological medicines.
The magnetic particles are required to have good monodispersity in the application process. The monodispersity of the magnetic particles means uniformity of particle diameter and uniformity of magnetic susceptibility. The magnetic particles with good monodispersity are still difficult to obtain by optimizing the process conditions in the preparation process of the magnetic particles, and further separation and screening of the prepared magnetic particles become an important means for improving the monodispersity of the magnetic particles.
At present, magnetic particle separation methods based on magnetic fields mainly include magnetophoretic magnetic separation methods, magnetic separation methods of magnetic capture and release, and magnetic field flow separation methods. Magnetophoresis is the separation of particles by using the change or deviation of the motion trajectory of magnetic particles under the action of a magnetic field. The basic principle of the magnetic separation method based on magnetophoresis is that magnetic particles with different particle sizes or different saturation magnetizations are subjected to different magnetic field forces, and the magnetophoresis speeds are different. The particles will be in different positions in the separation channel and if the outlet end is divided into several side-by-side channels, different particles will flow out of different outlets. The separation method of magnetic capture and release is that when magnetic particles pass near a magnetic pole under the drive of current carrying, the magnetic field force of a sample with magnetic responsiveness is larger than viscous resistance, the particles are adsorbed near the magnetic pole and retained in the magnetic field, so that the separation method is called as 'capture'; when the flow rate of the carrier current is increased or the magnetic induction intensity is reduced, the magnetic field force borne by the magnetic particles with weak magnetic responsiveness is smaller than the viscous resistance, and the particles are eluted out of the magnetic field under the drive of the viscous resistance, so that the release is called. The separation method of magnetic field capture and release utilizes the retention of magnetic particles by a magnetic field, and selectively flows out the particles with weak magnetism and retains the particles with strong magnetism by adjusting the magnetic field intensity. The magnetic field flow separation method is characterized in that a magnetic field is used as an external field, particles enter different laminar flows in a separation channel by utilizing the comprehensive action of magnetic responsiveness and gravity of magnetic particles, in a liquid flow phase of a parabolic flow type, the flow velocity near the center of the channel is high, the flow velocity near the wall of the channel is low, and the magnetic particles in different flow layers obtain different flow velocities to realize separation.
The magnetic field used in the magnetic field flow separation method mainly comprises a static magnetic field and a rotating magnetic field. If the external magnetic field is a static magnetic field, the action range is limited, the migration action range of the magnetic field on the particles is limited, the length of a separation channel is limited, and the separation degree is reduced. Irreversible adsorption and particle magnetic agglomeration caused by a static magnetic field can cause severe peak broadening. Compared with a static magnetic field, the rotating magnetic field improves the separation effect of the magnetic particles and has certain advantages. The periodic rotating magnetic field expands the action range of the magnetic field, is convenient for prolonging the separation channel and ensures that the adjustment of the magnetic field is simpler and more convenient. The rotating magnetic field can eliminate the irreversible capture of the magnetic field and inhibit the particle agglomeration. In the existing rotating magnetic field, a permanent magnet is fixed on a rotating shaft connected with a motor, the magnet is driven by the motor to do periodic circular motion along a separation channel right above or below the separation channel, and the rotating direction of the magnet is the same as the current-carrying direction. The rotating magnetic field changes the acting frequency of the magnetic field on the magnetic particles in the separation channel by adjusting the rotating speed of the motor, and the precision is not high. Changing the magnetic induction intensity in the separation channel requires adjusting the distance between the magnet and the separation channel, and ensuring the parallelism of the magnet rotation motion track and the separation channel is difficult to realize.
Disclosure of Invention
In view of the above-mentioned technical problems, a magnetic particle field flow separating device and method based on a rotating magnetic field are provided. The technical means adopted by the invention are as follows:
a magnetic particle field flow separating device based on a rotating magnetic field comprises a three-phase winding;
the three-phase winding comprises a first phase winding, a second phase winding and a third phase winding;
the first phase winding, the second phase winding and the third phase winding are in star connection and are symmetrically arranged on the base by taking the axis of the base as an axis;
the head ends of the first phase winding, the second phase winding and the third phase winding are respectively communicated with the output end of a three-phase power supply, and the output current of the three-phase power supply is symmetrical three-phase sinusoidal alternating current;
the base is of a hollow structure, and a separation channel is arranged in a space surrounded by the base;
the input end of the separation channel is respectively communicated with the sample injection syringe and the infusion pump through a three-way valve.
The three-phase power supply is obtained by the following method:
the three-phase alternating voltage or the single-phase alternating voltage (the frequency is 50Hz) is rectified by a rectifier in the frequency converter to be changed into direct current voltage, and then the direct current voltage is changed into three-phase alternating current with certain frequency and voltage through an inverter in the frequency converter.
The frequency converter is used for adjusting the frequency of the rotating magnetic field and the voltage of the three-phase winding.
The currents input into the first phase winding, the second phase winding and the third phase winding by the three-phase power supply are i respectivelyU、iV、iWAnd i isU、iV、iWThe following formula is satisfied:
when the head ends of the first phase winding, the second phase winding and the third phase winding are respectively communicated with the output end of the frequency converter for outputting three-phase voltage, symmetrical three-phase sinusoidal alternating current i exists in the three-phase windingU、iV、iWWhen the current flows through the coil, the resultant magnetic field generated by the coil continuously rotates in the winding space along with the change of the current, and a rotating magnetic field is formed.
The separation channel is a microtube or a flat channel.
And a rotating magnetic field generated by the three-phase winding is used as an external field to enable the magnetic particles to achieve the separation effect in the laminar flow in the liquid phase in the separation channel.
In a magnetic field flow separation system constructed by using a rotating magnetic field, factors such as fluid speed, rotating magnetic field frequency and magnetic induction intensity influence the retention and separation of magnetic particles.
When the frequency of the rotating magnetic field is high, the magnetic particles will undergo magnetophoresis in the direction of the current carrying.
The micro-fine tube is in a meter-level shape, has a micrometer-level inner diameter and is in a spiral shape, and the spiral shape is designed to increase the length of the separation channel located in the space surrounded by the base.
The inner wall of the base is provided with a plastic cylinder, and the inner wall of the plastic cylinder is provided with a spiral groove for embedding the microtube.
The output end of the separation channel is communicated with a waste liquid collecting bottle through an ultraviolet-visible light detector. The ultraviolet-visible light detector is used for detecting the separation condition of the magnetic particles, and the waste liquid collecting bottle can collect the liquid flow flowing out of the separation channel.
The invention also discloses a method for separating the magnetic particle field flow according to the magnetic particle field flow separating device based on the rotating magnetic field, which comprises the following steps:
s1, inputting current i to the first phase winding, the second phase winding and the third phase winding respectively by the three-phase power supplyU、iV、iWIn the space surrounded by the baseA rotating magnetic field is formed in the chamber, and the frequency of the rotating magnetic field and the voltage of the three-phase winding are adjusted through the frequency converter;
s2, under the condition that the thickness of the plastic cylinder is not changed, the radial position of the microtube is adjusted by changing the diameter of the inner wall and the diameter of the outer wall of the plastic cylinder, and the magnetic induction intensity at the position of the separation channel is changed;
s3, the magnetic particles with different magnetic susceptibilities injected by the sample injection injector and the mobile phase pumped by the infusion pump enter the separation channel from the input end of the separation channel through the three-way valve to perform magnetic particle field flow separation.
The separation channel is a microtube or a flat channel.
The micro-fine tube is meter-level in length, micron-level in inner diameter and spiral;
the inner wall of the base is provided with a plastic cylinder, and the inner wall of the plastic cylinder is provided with a spiral groove for embedding the microtube.
The invention provides a device and a method for separating magnetic particles by using a rotating magnetic field generated by a three-phase winding as an external field in magnetic field current separation, wherein a separation channel is arranged in an internal cylindrical space formed by the three-phase winding and a base, and the size and the frequency of three-phase voltage applied to the three-phase winding are adjusted by a frequency converter. The frequency of the magnetic particles under the action of the rotating magnetic field is controlled, the magnetic induction intensity of the separation channel is changed, and the field flow separation of the magnetic particles with different particle sizes or the same particle size and different magnetic susceptibilities is realized.
For the above reasons, the present invention can be widely applied to the field of magnetic particle separation and the like.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
Fig. 1 is a schematic diagram of a three-phase winding and base connection in an embodiment of the present invention.
FIG. 1 illustrates a base; 2. and (4) three-phase windings.
Fig. 2 is a schematic view of a star connection of a first phase winding, a second phase winding and a third phase winding in an embodiment of the present invention.
Fig. 3 is a waveform diagram of a symmetrical three-phase sinusoidal ac current in an embodiment of the present invention.
Fig. 4 is a schematic diagram of a combined magnetic field generated by three-phase currents in a three-phase winding according to an embodiment of the present invention, where (a) ω t is 0 °, (b) ω t is 60 °, (c) ω t is 120 ° (v/v) °
Fig. 5 is a schematic structural diagram of a magnetic particle field flow separating device based on a rotating magnetic field according to an embodiment of the present invention.
FIG. 1 illustrates a base; 2. a three-phase winding; 3. a microtube; 4. a plastic cylindrical barrel; 5. a frequency converter; 6. a three-way valve; 7. an infusion pump; 8. a sample injection syringe; 9. an ultraviolet-visible light detector; 10. and a waste liquid collecting bottle.
FIG. 6 is a schematic diagram illustrating the connection between a microtube and a plastic cylinder according to an embodiment of the present invention.
FIG. 7 is a graph showing the effect of magnetic particle separation at saturation induction of 2.32emu/g and 3.50emu/g, respectively, in accordance with an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
As shown in fig. 1 to 6, a magnetic particle field flow separating device based on a rotating magnetic field includes a three-phase winding 2;
the three-phase winding 2 comprises a first phase winding, a second phase winding and a third phase winding;
the first phase winding, the second phase winding and the third phase winding are in star connection and are symmetrically arranged on the base 1 by taking the axis of the base 1 as an axis;
the base 1 is a cast iron base;
head ends U of the first phase winding, the second phase winding and the third phase winding1、V1、W1Respectively connected with the output end L of a three-phase power supply1、L2、L3The three-phase power supply is connected, and the output current of the three-phase power supply is symmetrical three-phase sinusoidal alternating current;
the base 1 is of a hollow structure, and a separation channel is arranged in a space surrounded by the base 1;
the input end of the separation channel is respectively communicated with a sample injection syringe 8 and an infusion pump 7 through a three-way valve 6.
The three-phase power supply is obtained by the following method:
the three-phase ac voltage or the single-phase ac voltage (frequency is 50Hz) is rectified by the rectifier of the frequency converter 5 to be a dc voltage, and then is converted into a three-phase ac with a certain frequency and voltage by the inverter of the frequency converter 5.
The currents input into the first phase winding, the second phase winding and the third phase winding by the three-phase power supply are i respectivelyU、iV、iWAnd i isU、iV、iWThe following formula is satisfied:
and analyzing the condition of the magnetic field distribution of the three-phase winding 2 according to the current of each phase winding and the direction thereof at different moments. The waveform diagram of a symmetrical three-phase sinusoidal alternating current is shown in fig. 2. Defining the winding head end (U)1、V1、W1) To the end (U)2、V2、W2) As a reference direction for the current. In thatThe magnetic field produced by the three-phase current varies at different times (angles):
when ω t is 0 °, the U-phase current iUPhase current i of 0, WWIs positive, i.e. from W1End flows in at W2End-bleed, V-phase current iVIs negative, i.e. from V2End inflow at V1End current, according to the current direction, applying the right hand screw rule, from iVAnd iWThe resultant magnetic field is shown in FIG. 4 (a).
When ω t is 60 °, the directions of currents in the three-phase winding 2 and the resultant magnetic fields of the three-phase currents are as shown in fig. 4 (b). The resultant magnetic field is rotated by 60 ° clockwise compared to when ω t is 0 °. When ω t is 120 °, the resultant magnetic field of the three-phase current is as shown in fig. 4 (c). The resultant magnetic field is rotated by 60 ° clockwise, compared to the case where ω t is 60 °. Similarly, when ω t is 180 °, the resultant magnetic field is rotated 180 ° as compared with when ω t is 0 °. When ω t is 360 °, the resultant magnetic field is improving by one revolution.
When the head ends of the first phase winding, the second phase winding and the third phase winding are respectively communicated with the output end of a three-phase power supply, symmetrical three-phase sinusoidal alternating current i exists in the three-phase winding 2U、iV、iWWhen the current flows through the coil, the resultant magnetic field generated by the coil continuously rotates in the winding space along with the change of the current, and a rotating magnetic field is formed.
The separation channel is a microtube 3.
The micro-fine tube 3 is meter-level in length, micron-level in inner diameter and spiral;
the inner wall of the base 1 is provided with a plastic cylinder 4, and the inner wall of the plastic cylinder 4 is provided with a spiral groove for embedding the microtube 3.
The output end of the separation channel is communicated with a waste liquid collecting bottle 10 through an ultraviolet-visible light detector 9.
Example 2
A method for magnetic particle field separation by the rotating magnetic field-based magnetic particle field separation device according to embodiment 1, comprising the steps of:
s1, the three-phase powerInputting a current i to the first phase winding, the second phase winding and the third phase winding respectivelyU、iV、iWA rotating magnetic field is formed in a space enclosed by the base 1, and the frequency of the rotating magnetic field and the voltage of a three-phase winding are adjusted through the frequency converter 5;
s2, under the condition that the thickness of the plastic cylinder is not changed, the radial position of the microtube is adjusted by changing the diameter of the inner wall and the diameter of the outer wall of the plastic cylinder, and the magnetic induction intensity at the position of the separation channel is changed;
s3, the magnetic particles with different magnetic susceptibilities injected by the sample injection injector 8 and the mobile phase pumped by the infusion pump 7 enter the separation channel from the input end of the separation channel through the three-way valve 6 to perform magnetic particle field flow separation.
For magnetic particles with the same particle size, the frequency of the rotating magnetic field and the three-phase voltage are adjusted. When the magnetic poles of the rotating magnetic field rotate above the magnetic particles, the magnetic particles are attracted to the upper wall of the microtube 3. The magnetic particles with high magnetic susceptibility are close to the upper wall of the microtube 3, but do not reach the upper wall of the microtube 3, and have a certain distance from the upper wall of the microtube 3. The magnetic particles with low magnetic susceptibility are farther away from the tube wall of the microtube 3, so that liquid flow layering of the magnetic particles with different magnetic susceptibilities is realized. The magnetic particles with low magnetic susceptibility are closer to the central position of the liquid flow phase parabolic flow pattern than the magnetic particles with high magnetic susceptibility, and the migration speed is high. The magnetic particles with low magnetic susceptibility flow out of the microtube 3 first, and then the magnetic particles with high magnetic susceptibility flow out, so that the separation of the magnetic particles with the same particle size and different magnetic susceptibilities is realized.
Acetonitrile is selected as a mobile phase, the rotation direction of a rotating magnetic field is the same as the current carrying direction, and the flow velocity of liquid flow is 0.4m L/min. The frequency of the frequency converter 5 is adjusted so that the rotation frequency of the rotating magnetic field is small, 2 Hz. The saturation induction is a physical quantity that measures the magnitude of the magnetic susceptibility of the magnetic particles. Magnetic particles with high magnetic susceptibility have high saturation magnetic induction intensity; the magnetic particles with small magnetic susceptibility have small saturation magnetic induction intensity. The magnetic particles with saturation magnetic induction intensities of 2.32emu/g and 3.50emu/g respectively have the particle diameters of 5.36 mu m and the sample injection amounts of 20 mu g, and the two magnetic particles with different magnetic responsivities can be well separated in a rotating magnetic field flow separation device to meet the requirements of separation and analysis. As shown in FIG. 7, the magnetic particles had a diameter of 5.36 μm and saturation induction densities of 2.32emu/g (peak a) and 3.50emu/g (peak b), respectively.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (3)
1. A magnetic particle field flow separating device based on a rotating magnetic field is characterized by comprising:
a base;
the base is provided with a three-phase winding which is axisymmetrical with the axis of the base as an axis; the three-phase winding comprises a first phase winding, a second phase winding and a third phase winding; the first phase winding, the second phase winding and the third phase winding are star-connected; the head ends of the first phase winding, the second phase winding and the third phase winding are respectively communicated with the output end of a three-phase power supply, and the output current of the three-phase power supply is symmetrical three-phase sinusoidal alternating current;
the base is of a hollow structure, the inner wall of the base is provided with a plastic cylinder, and the inner wall of the plastic cylinder is provided with a spiral groove for embedding the microtube; a separation channel in the form of a micro-pipe is embedded in the spiral groove, and the length of the micro-pipe is meter-level, and the inner diameter of the micro-pipe is micron-level and is spiral; the input end of the separation channel is respectively communicated with the sample injection syringe and the infusion pump through a three-way valve;
the magnitude and the frequency of three-phase voltage applied to the three-phase winding are adjusted through a frequency converter; controlling the frequency of the magnetic particles under the action of the rotating magnetic field, and changing the magnetic induction intensity of the separation channel to realize the field flow separation of the magnetic particles with different particle sizes or the same particle size and different magnetic susceptibilities;
the three-phase power supply is obtained by the following method:
rectifying the three-phase alternating-current voltage or the single-phase alternating-current voltage by a rectifier in a frequency converter to form direct-current voltage, and converting the direct-current voltage into three-phase alternating current with certain frequency and voltage by an inverter in the frequency converter;
the currents input into the first phase winding, the second phase winding and the third phase winding by the three-phase power supply are i respectivelyU、iV、iWAnd i isU、iV、iWThe following formula is satisfied:
2. the rotating magnetic field-based magnetic particle field flow separating device according to claim 1, wherein: the output end of the separation channel is communicated with a waste liquid collecting bottle through an ultraviolet-visible light detector.
3. A method for magnetic particle field separation by the rotating magnetic field-based magnetic particle field separation device according to claim 1, characterized by comprising the following steps:
s1, inputting current i to the first phase winding, the second phase winding and the third phase winding respectively by the three-phase power supplyU、iV、iWA rotating magnetic field is formed in a space surrounded by the base, and the frequency of the rotating magnetic field and the voltage of the three-phase winding are adjusted through the frequency converter;
s2, under the condition that the thickness of the plastic cylinder is not changed, the radial position of the microtube is adjusted by changing the diameter of the inner wall and the diameter of the outer wall of the plastic cylinder, and the magnetic induction intensity at the position of the separation channel is changed;
s3, the magnetic particles with different magnetic susceptibilities injected by the sample injection injector and the mobile phase pumped by the infusion pump enter the separation channel from the input end of the separation channel through the three-way valve to perform magnetic particle field flow separation.
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