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WO2013071910A1 - Détecteur de particules magnétiques contenues dans un liquide - Google Patents

Détecteur de particules magnétiques contenues dans un liquide Download PDF

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Publication number
WO2013071910A1
WO2013071910A1 PCT/DE2012/001077 DE2012001077W WO2013071910A1 WO 2013071910 A1 WO2013071910 A1 WO 2013071910A1 DE 2012001077 W DE2012001077 W DE 2012001077W WO 2013071910 A1 WO2013071910 A1 WO 2013071910A1
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WO
WIPO (PCT)
Prior art keywords
magnetic field
field sensor
substrate
drive source
channel
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/DE2012/001077
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German (de)
English (en)
Inventor
Klaus Seemann
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Forschungszentrum Juelich GmbH
Original Assignee
Forschungszentrum Juelich GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Forschungszentrum Juelich GmbH filed Critical Forschungszentrum Juelich GmbH
Publication of WO2013071910A1 publication Critical patent/WO2013071910A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/72—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating magnetic variables
    • G01N27/74—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating magnetic variables of fluids
    • G01N27/745—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating magnetic variables of fluids for detecting magnetic beads used in biochemical assays
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
    • A61B5/00—Measuring for diagnostic purposes; Identification of persons
    • A61B5/05—Detecting, measuring or recording for diagnosis by means of electric currents or magnetic fields; Measuring using microwaves or radio waves
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
    • A61B5/00—Measuring for diagnostic purposes; Identification of persons
    • A61B5/145—Measuring characteristics of blood in vivo, e.g. gas concentration or pH-value ; Measuring characteristics of body fluids or tissues, e.g. interstitial fluid or cerebral tissue
    • A61B5/14546—Measuring characteristics of blood in vivo, e.g. gas concentration or pH-value ; Measuring characteristics of body fluids or tissues, e.g. interstitial fluid or cerebral tissue for measuring analytes not otherwise provided for, e.g. ions, cytochromes
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
    • G01R33/00—Arrangements or instruments for measuring magnetic variables
    • G01R33/12—Measuring magnetic properties of articles or specimens of solids or fluids
    • G01R33/1269—Measuring magnetic properties of articles or specimens of solids or fluids of molecules labeled with magnetic beads
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
    • A61B2560/00—Constructional details of operational features of apparatus; Accessories for medical measuring apparatus
    • A61B2560/02—Operational features
    • A61B2560/0266—Operational features for monitoring or limiting apparatus function
    • A61B2560/0276—Determining malfunction
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
    • A61B2562/00—Details of sensors; Constructional details of sensor housings or probes; Accessories for sensors
    • A61B2562/02—Details of sensors specially adapted for in-vivo measurements
    • A61B2562/0223—Magnetic field sensors
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F10/00—Thin magnetic films, e.g. of one-domain structure
    • H01F10/32—Spin-exchange-coupled multilayers, e.g. nanostructured superlattices
    • H01F10/324—Exchange coupling of magnetic film pairs via a very thin non-magnetic spacer, e.g. by exchange with conduction electrons of the spacer

Definitions

  • the invention relates to a detector for magnetic particles in a liquid.
  • Bioanalytics is about converting the presence of an analyte in a liquid into an electrical signal and making it detectable. For this purpose it is known to add to the liquid a fluorescence marker which binds specifically to the analyte sought. The higher the concentration of analyte in the fluid, the more tags are bound and fluoresce upon excitation with light of the appropriate wavelength. This is optically read out.
  • the optical equipment required for this purpose are difficult to miniaturize, in contrast to the magnetic field sensors known, for example, from hard disk read heads.
  • the liquid magnetic particles (markers) which specifically bind to the analyte sought.
  • the liquid is conducted to a sensitive magnetic field sensor. The higher the concentration of the analyte in the liquid, the more markers are bound and the larger the field registered at the magnetic field sensor.
  • a detector for magnetic particles in a liquid comprises a substrate on which at least one magnetic field sensor is arranged.
  • magnetic particles are also understood to mean objects to which magnetic particles are attached and / or embedded in the magnetic particles.
  • a channel guided past the magnetic field sensor or guided directly over the magnetic field sensor is arranged on the substrate for guiding the liquid, and a drive source for generating a relative movement between the liquid and the channel is provided.
  • a channel is understood to mean a structure which allows an essentially one-dimensional movement of the liquid past the magnetic field sensor.
  • the shape and dimensions of the channel depend on the size and shape of the magnetic particles to be detected.
  • the channel is preferably open on both sides, so that the liquid, after it has passed through the magnetic field sensor through it, can leave the vicinity of the magnetic field sensor through it again. Otherwise, the course of the channel is not limited. In particular, it does not have to be straightforward.
  • the combination of channel and drive source allows the liquid to be conveyed in the direction of the magnetic field sensor so that it flows past it at a defined maximum distance. Ideally, this distance is less than the distance to which the magnetic field sensor can still register a magnetic particle.
  • the channel is advantageously guided past the magnetic field sensor at a distance of 50 ⁇ or less. According to the prior art, there was no precise control over the course of the liquid flow in the vicinity of the magnetic field sensor, so that existing particles passed too far past the magnetic field sensor. It was recognized that this was a limiting factor for the achievable measurement accuracy and the inventive combination of channel and drive source increases this measurement accuracy.
  • the magnetic field sensor can be operated alternately with the drive source. Then, a magnetic field sensor can be used, the measurement result by the of the Drive source excited movement of the substrate is affected.
  • the magnetic field sensor only has to be mechanically robust so that it is not destroyed by the forces exerted by the drive source.
  • the magnetic field sensor can also be operated simultaneously with the drive source. Then only a magnetic field sensor can be used whose measurement result is not influenced by the movement of the substrate excited by the drive source.
  • a plurality of magnetic field sensors are arranged on the substrate, in particular as a row or field, the trajectories and transport properties of individual magnetic objects, such as magnetic particles or objects marked with magnetic particles, can be studied in fluidic media of various kinds.
  • the magnetic field sensors do not all have to be of the same type. Certain areas of the substrate will be exposed to greater mechanical accelerating forces than other areas in the movement excited by the drive source. This is especially true when a surface acoustic wave is driven through the substrate.
  • Robust magnetic field sensors such as Hall sensors, can then be arranged in the mechanically heavily loaded areas, and mechanically sensitive sensors, such as tunnel magnetoresistance sensors, in the less stressed areas.
  • the drive source and the magnetic field sensor are accommodated on one and the same surface of one and the same substrate, this reduces the space requirement which the detector and drive source as a whole occupy.
  • Many similar detectors can be arranged on one and the same substrate surface.
  • a detector with a plurality of magnetic field sensors can be realized on a common substrate with only one or a few drive sources.
  • the detector is particularly suitable for "lab-on-a-chip" bioanalysis
  • the detector is generally so far miniaturized that it can be implanted and used in vivo For example, blood levels can be measured continuously without having to remove samples from a vein over and over again.
  • the drive source is able to generate a periodic relative movement between the liquid and the channel. Such movement causes the liquid to be successively conveyed through the channel without permanently changing the central position of the substrate.
  • the liquid is influenced as little as possible on its way through the channel. This is particularly advantageous when it is a sensitive biological fluid, such as blood. Its properties change when it is mechanically stressed too much.
  • the drive source is able to move the substrate as a whole through the liquid.
  • the substrate may be adhered to a stirrer which is introduced into the liquid.
  • a larger volume of the liquid can be searched for the magnetic particles, if it is not known at what depth within the liquid they are.
  • the drive source is arranged on a first substrate, or it is a part of this substrate.
  • the magnetic field sensor is arranged on a second substrate separate from the first substrate. Both substrate surfaces are advantageously facing each other and at the same time limit the channel. To form a very small channel, it is sufficient to place the nominally planar first substrate with the drive source and the nominally planar second substrate with the magnetic field sensor to each other and to fix them at a distance of the previously defined channel height.
  • the channel can also be structured, for example, in a surface of one of the two substrates.
  • the magnetic field sensor is mechanically decoupled from the movement of the first substrate with the drive source, so it is neither moved nor stretched or compressed. Then also magnetic field sensors that respond to such influence with a falsification of their measurement signal can be operated simultaneously with the drive source. At the same time, the heat generated during operation of the drive source can be better dissipated, for example via the side of the first substrate facing away from the channel.
  • the first substrate may be, for example, piezo-electric and functionalized by an applied electrical contact to the drive source.
  • the second substrate with the Magnetic field sensor is then subject to the drive, no special requirements more. It can be made of the material that best suits the realization of the magnetic field sensor and the channel.
  • a drive source is provided, which is able to stretch and / or compress at least one substrate in the direction of the channel.
  • the drive source is able to drive surface acoustic waves through at least one substrate.
  • An expansion and / or compression of at least one substrate can be realized particularly easily if this substrate is piezoelectric.
  • monocrystalline lithium niobate, lithium tantalate, quartz or gallium arsenide are suitable as piezoelectric substrates.
  • electrode structures for example interdigital structures, on the substrate. If these are subjected to alternating voltage, the region functionalized with the electrode structures is excited to periodically change the length.
  • the drive source is able to drive surface acoustic waves through at least one substrate by exciting this substrate sinusoidally, these waves can be excited by means of momentum transfer, a continuous relative movement between the liquid and the channel, as opposed to very discontinuous, such as sawtooth Movement that drives the fluid by utilizing its inertia alone through the channel.
  • Sinusoidal excitation of the substrate resulting in a continuous flow of liquid through the channel, loads the detector with significantly lower accelerating forces and reduces the risk of, for example, tearing the tunnel barrier, which is only a few nanometers thick, in a magnetic field sensor.
  • the liquid is spared. For example, when a biological fluid, such as blood, is moved very strongly discontinuously against the canal, cells can be destroyed. The fragments can then clog the channel, so that the detector is no longer usable.
  • the window of the maximum power which can be coupled into the drive becomes larger.
  • the use of surface acoustic waves opens up the possibility of intentionally imparting a movement direction even to the smallest quantities of fluidic media and, for example, of moving individual magnetic particles or objects marked with magnetic particles over a plurality of magnetic detectors or a field of detectors. It was recognized that the surface acoustic wave is in the incompressible liquid spreads and attacks on each one of its particles. Especially with small amounts of liquid that do not fill the channel completely, in this way the surface tension, which holds smallest droplets in the channel, can be overcome much better than for example with an inertial drive, which tries to tear the droplets in the discontinuous phase of the movement.
  • the wave-wave of the surface acoustic wave is typically parallel to the surface of the substrate that defines the channel.
  • the refractive index changes, so that the surface acoustic wave is reflected there in part. This can lead to the formation of a standing wave, a beating or even a destructive interference.
  • the drive source is arranged or interconnected such that the wave vector of the surface acoustic wave does not include a right angle with at least one boundary of the substrate on which the surface acoustic wave impinges.
  • the wave vector with the boundary encloses an angle between 30 ° and 60 °. Then, the portion of the surface acoustic wave reflected at the interface is directed away from the channel by reflection at this oblique edge, so that only a traveling wave drives the liquid through the channel and the formation of standing waves is avoided.
  • Diamond shaped piezoelectric elements with matching bevelled edges are commercially available. However, it is also possible, for example, for only a part of the substrate to be piezoelectric and thus to perform the fluidic drive by means of surface acoustic waves, while the magnetic detection takes place on a non-piezoelectric sub-substrate.
  • the detector has deflector or absorption structures for deflecting or attenuating surface acoustic waves which run from the drive source in the direction away from the magnetic field sensor or else run out from the drive source via the magnetic field sensor. This prevents these two portions of the surface acoustic waves produced by the drive source from interfering with the shaft driven by the channel after reflection at the interface of the substrate and interfering with the propulsion of the liquid through the channel.
  • At least one substrate is mechanically coupled to a piezoelectric element as a drive source. This is set into vibration upon application of an alternating voltage, which are coupled into the substrate. In this way, a substrate can be vibrated, which is not piezoelectric itself. When the vibrations are generated, the piezoelectric material is constantly periodically deformed, producing Joule 's heat.
  • this heat source is spatially separated from the substrate and in particular from the channel and / or the magnetic field sensor, the heat effect on the substrate, the magnetic field sensor and / or the liquid in the channel can be advantageously reduced. If, for example, 5 watts of power is coupled into a piezoelectric element with 5 mm edge length, this corresponds to a higher heat load per unit area than on a stove top.
  • the drive source such as the piezoelectric element, disposed on one surface and the magnetic field sensor on the other surface of one and the same substrate.
  • the drive source first couples bulk acoustic waves into the one surface of the substrate. These bulk waves pass through the substrate and are converted on its other surface into acoustic surfaces which drive the liquid through the channel.
  • the channel and the liquid are protected by the substrate against the heat effect of the drive source and also electrically separated.
  • the magnetic field sensor is at least partially decoupled from the movement of the drive source. Since the drive source in this embodiment is no longer within the channel, it can no longer be electrically short-circuited by the liquid in the channel.
  • the channel is guided past a magnetic field source.
  • this magnetic field source is advantageous in the flow direction of the liquid behind the magnetic field sensor.
  • the magnetic field source may be a permanent magnetic region or an electrical coil. Magnetic particles registered by the magnetic field sensor attach to the magnetic field source. This can be used to permanently remove them from the liquid flow through the channel so that they are not re-fed into the channel at a later time and are registered by the magnetic field sensor. The particles or other objects to which the particles are bound can also be obtained as valuable substances from the liquid. If the magnetic field source is a coil, then a strong current pulse through this coil can be used to free the area of the magnetic field sensor of magnetic particles and to reset the detector as it were.
  • the magnetic field sensor is designed as a stack of functional layers whose magnetostrictions and / or magnetoacoustic coupling constants cancel each other out.
  • This is advantageous at least in the frequency range between 0.5 MHz and 5 GHz, preferably between 10 MHz and 1 GHz and very particularly preferably between 150 and 250 MHz, for periodic movements, strains and / or compressions of the substrate in the frequency range relevant for microfluidic applications.
  • A, in particular periodic, movement of the substrate as a whole acts on the functional layers of the sensor by way of magnetoacoustic coupling. If the related coupling constants are mutually exclusive, the sensor's measurement result will not be affected.
  • A, in particular periodic, elongation or compression of the substrate acts by way of magnetostriction on the functional layers.
  • the penetration of the measurement result of the sensor is in turn minimized when the magnetostrictions of the functional layers cancel each other out.
  • Particularly advantageous in this context is a planar Hall sensor.
  • other spintronic sensors based on tunneling magnetoresistance (TMR), anisotropic magnetoresistance (AMR), giant magnetoresistance (GMR), anomalous Hall effect (AHE), and Planar Hall are also suitable Effect (PHE), Spin Hall Effect (SHE), Domain Wall Resistance (DWR), and Spin Torque Transfer (STT).
  • the magnetic field sensor is a spintronic sensor with an antiferromagnetically netting pinned ferromagnet, wherein the direction of the antiferromagnetic coupling between the ferromagnet and the pinning layer with the wave vector of the coupled into the magnetic field sensor oscillations an angle of 45 ° or less, preferably of 10 ° or less, and most preferably is parallel. Then, the vibrations do not generate oscillating magnetization in the system of ferromagnet and pinning layer. Only when an external magnetic field is applied, this can set a magnetization direction above a certain strength, which can possibly be deflected periodically by the vibrations of the substrate.
  • the continuous or pulsed operation of interdigital structures by means of a high-frequency sinusoidal voltage has been proven in practice.
  • the substrate can be excited in particular with frequencies between 10 MHz and 5 GHz.
  • surface waves are formed in Rayleigh or Love mode. Both modes are suitable for exciting a fluidic phase, in which the liquid is mixed in itself. This phase is interesting for exploring chemical reactions initiated on-chip by mixing the reactants. the. Especially love modes preferably cause such a mixing, since they are shear waves. Love fashions contribute less to transporting the fluid as a whole than Rayleigh fashions.
  • the comb structures which are typically lithographically worked out of gold and a metallic adhesive layer on the piezoelectric substrate, are generally operated with a continuous or pulsed sinusoidal voltage signal of an output power between 1 ⁇ W and 5 W, preferably between 1 ⁇ W and 0.5 W.
  • various geometric arrangements of the exciter structures are helpful for generating standing waves or running waves and thus directing or locally accumulating the mass transport of magnetic particles or objects marked with magnetic particles in the fluidic phase.
  • the excitation structures are placed at appropriate angles to the respective generated sound path.
  • two exciter structures on a lithium niobate substrate together with a series of magnetic multi-layer structures located within the sound path were worked out as detectors in various lateral dimensions and at a resonance frequency of about 190 MHz operated with a signal generator for generating a sinusoidal AC voltage.
  • a resonance frequency of about 190 MHz operated with a signal generator for generating a sinusoidal AC voltage.
  • the influence of surface acoustic waves on the magnetic detector structure was tested in the form of a planar-Hall-effect sensor and its mechanical as well as proved the electronic robustness.
  • the applied external magnetic fields were at some oersteds.
  • the coupling efficiency was ensured by simultaneous detection of the incoming wave trains at the end of the sound path.
  • the magnetic detection of magnetic particles or objects marked with magnetic particles can take place by means of a planar Hall effect sensor, but also by means of other magnetic detection mechanisms together with the generation of the surface acoustic waves on one and the same substrate.
  • Suitable markers are, for example, FePt nanoparticles which are functionalized with at least one biotin molecule.
  • a streptavidin molecule is bound to the biotin molecule at one of its two ends. The other end is available for binding to the analyte.
  • pathologically altered cells have a receptor for a specific protein (such as HER2)
  • streptavidin can either bind directly to this receptor or via an antibody (such as anti-HER2), which has entered into a very stable binding to the receptor and quasi acts as an adapter. If a fluid with pathologically altered cells flows through the channel, the signal registered by the magnetic field sensor is proportional to both the concentration of the cells in the fluid and the number of receptors per cell, which in turn is a measure of the pathological change in the cell.
  • antibody-receptor binding is accomplished without mediation by the streptavidin-biotin complex. Then the diameter of the magnetic marker together with the biological functionalization surrounding it is in a favorable ratio to the radial drop of its magnetic stray field.
  • Another application may be, for example, in the magnetic measurement of the characteristic of leukemia excess number of B-leukocytes.
  • an antibody binding of the magnetic markers to the leukocytes via immunoglobulin B IgB and the respective antibody anti-lgB could take place.
  • Figure 1 embodiment of the detector according to the invention in supervision.
  • FIG. 2 side view of the embodiment from FIG. 1.
  • Figure 3 embodiment of the detector according to the invention with drive source
  • Figure 5 embodiment of the detector according to the invention with two drive sources, which selectively drive the liquid through the channel or objects in the region of
  • FIG. 1 shows an embodiment of the detector according to the invention in a plan view.
  • a piezoelectric substrate (not numbered) is in a partial area by metallic Interdigital structures (a), which are acted upon by AC voltage, functionalized as a drive source.
  • This substrate accommodates at the same time several magnetic field sensors (c) within a channel, of which only the lateral boundaries (f) are drawn.
  • the drive source (a) drives acoustic surface waves through the substrate. As symbolized by the arrows, these waves travel in both directions away from the drive source (a). Only the portion (b) ensures the propulsion of the liquid.
  • the other part is deflected by a deflector (d) so that this part does not interfere with the part (b) and hinder the transport.
  • Figure 2 shows a side view of the detector.
  • the deflector (d) is not drawn.
  • the upper limit (f) of the channel is visible.
  • the channel contains a liquid with several objects, each marked by magnetic particles (e). By passing these particles (e) from the shaft (b) past the magnetic field sensors (c), they generate electrical signals there.
  • FIG. 3 shows another embodiment of the detector according to the invention in side view.
  • the area (a) functionalized as a drive source is here arranged on the one surface and the magnetic field sensors are arranged on the other surface of one and the same substrate.
  • the drive source (a) first drives a bulk acoustic wave through the substrate. This is converted to a surface wave (b) on the other surface and drives the liquid through the channel.
  • FIG. 4 shows a further exemplary embodiment of the detector according to the invention in side view.
  • the drive source (a) is arranged on a first substrate.
  • the magnetic field sensors (c) are arranged on a separate second substrate. Both substrates together limit the channel.
  • the magnetic field sensors (c) are decoupled from the movement of the drive source (a).
  • FIG. 5 shows a further embodiment of the detector according to the invention in a top view.
  • two drive sources (a) are provided. If only one of the drive sources (a) is in operation or if both drive sources (a) are operated in exactly opposite phase, the fluid is driven in one direction through the channel whose lateral boundaries (f) are drawn. If both drive sources (a) are operated in phase, the objects marked with magnetic particles (e) accumulate in the wave taps of the surface acoustic wave. In one of these pressure nodes are the magnetic field sensors (c). If the magnetic particles (e) are only present in a low concentration in the liquid, their local concentration in the region of the magnetic field sensors (c) can be raised above the detection limit in this way.

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Abstract

L'invention concerne un détecteur de particules magnétiques contenues dans un liquide. Ledit détecteur comprend un substrat sur lequel est agencé au moins un capteur de champ magnétique. Selon l'invention, un canal passant le long du capteur de champ magnétique est agencé sur le substrat pour le guidage du liquide, et une source d'entraînement assure la production d'un mouvement relatif entre le liquide et le canal. La combinaison du canal et de la source d'entraînement permet de refouler le liquide en direction du capteur de champ magnétique de telle manière qu'il passe à une distance maximale définie du capteur. Idéalement, cette distance est inférieure à l'éloignement à partir duquel le capteur de champ magnétique ne peut plus enregistrer une particule magnétique. Si une de ces particules est refoulée dans le canal par la source d'entraînement, on a l'assurance que ladite particule sera elle aussi enregistrée. Il est apparu que la combinaison du canal et de la source d'entraînement selon l'invention augmente la précision de mesure.
PCT/DE2012/001077 2011-11-17 2012-11-07 Détecteur de particules magnétiques contenues dans un liquide Ceased WO2013071910A1 (fr)

Applications Claiming Priority (2)

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DE102011118742.5 2011-11-17
DE201110118742 DE102011118742A1 (de) 2011-11-17 2011-11-17 Detektor für magnetische Partikel in einer Flüssigkeit

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