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WO2017125374A1 - Dispositif de détection et de caractérisation de molécules organiques dans un volume d'échantillon liquide - Google Patents

Dispositif de détection et de caractérisation de molécules organiques dans un volume d'échantillon liquide Download PDF

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Publication number
WO2017125374A1
WO2017125374A1 PCT/EP2017/050864 EP2017050864W WO2017125374A1 WO 2017125374 A1 WO2017125374 A1 WO 2017125374A1 EP 2017050864 W EP2017050864 W EP 2017050864W WO 2017125374 A1 WO2017125374 A1 WO 2017125374A1
Authority
WO
WIPO (PCT)
Prior art keywords
plate
metal
sample volume
microfluidic channel
raman
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/EP2017/050864
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German (de)
English (en)
Inventor
Christoph KRATZ
Karsten Hinrichs
Thomas OATES
Dirk Janasek
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.)
Leibniz - Institut fur Analytische Wissenschaften -Isas- EV
Original Assignee
Leibniz - Institut fur Analytische Wissenschaften -Isas- EV
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 Leibniz - Institut fur Analytische Wissenschaften -Isas- EV filed Critical Leibniz - Institut fur Analytische Wissenschaften -Isas- EV
Publication of WO2017125374A1 publication Critical patent/WO2017125374A1/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
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/65—Raman scattering
    • G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
    • B01L3/50—Containers for the purpose of retaining a material to be analysed, e.g. test tubes
    • B01L3/502—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
    • B01L3/5027—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip
    • B01L3/502715—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip characterised by interfacing components, e.g. fluidic, electrical, optical or mechanical interfaces
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/55—Specular reflectivity
    • G01N21/552—Attenuated total reflection
    • G01N21/553—Attenuated total reflection and using surface plasmons
    • G01N21/554—Attenuated total reflection and using surface plasmons detecting the surface plasmon resonance of nanostructured metals, e.g. localised surface plasmon resonance
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00—Additional constructional details
    • B01L2300/16—Surface properties and coatings
    • B01L2300/168—Specific optical properties, e.g. reflective coatings
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01—Arrangements or apparatus for facilitating the optical investigation
    • G01N21/03—Cuvette constructions
    • G01N2021/0346—Capillary cells; Microcells
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01—Arrangements or apparatus for facilitating the optical investigation
    • G01N21/03—Cuvette constructions
    • G01N21/05—Flow-through cuvettes
    • G01N2021/058—Flat flow cell

Definitions

  • the invention relates to an apparatus for detecting and characterizing organic molecules in a liquid sample volume in the micromixer and submicroliter range by means of Raman and infrared spectroscopy, in particular by means of RR (Raman Resonant Spectroscopy), SERS (Surface-Enhanced Raman Spectroscopy), SECARS (US Pat. surface-enhanced coherent anti-Stokes Raman spectroscopy), SEIRA (surface-enhanced infrared absorption) and SPR (surface plasmon resonance).
  • the object of the invention is a simple detection and characterization of organic molecules with a concentration below the ppm range in a liquid sample volume in the micro- and sub-microliter range due to the vibration properties of the molecules by means of the aforementioned methods of Raman spectroscopy and infrared spectroscopy in to achieve a single device.
  • This object is achieved in a device of the type described by a Mikrofluidikchip with at least one upwardly open Mikroflui- dikkanal for flowing through the sample volume and by the at least one microfluidic channel covering, serving as a measuring window transparent plate, which on the at least one microfluidic channel facing Page coated with a metal island film, and by a directed to the plate Detection optics, which emits light on the plate and receives the reflected light rays.
  • the device according to the invention is therefore suitable for evaluating the light radiation reflected at the interface between the metal-island film and the sample volume.
  • the different topologies of the metal-island film by virtue of their optical properties, impart amplification effects for the simultaneous use of Raman spectroscopy and infrared spectroscopy techniques and surface plasmon resonance spectroscopy.
  • the reinforcing effect of the metallic substrate or of the metal-insulator film results essentially from the resonant excitation of surface plasmon in the metal islands, the required resonant wavelength of the electromagnetic radiation being dependent on the diameter of the metal islands.
  • the elliptical shape of the metal islands according to the invention eliminates the rotational symmetry and leads to a splitting of the excitable resonances.
  • two different plasmonic resonances along the major axis and minor axis of the ellipsoid can now be excited.
  • the plasmonic resonance along the minor axis occurs in a region of shorter wavelengths than the resonance along the major axis.
  • the use of such a backside reflection geometry allows the production of the actual microfluidic chip from a cost-effective polymer material, because the microfluidic chip itself is not penetrated by the incident light and thus no evaluation of the transmission takes place.
  • the device is thus an accessory for Raman and IR spectroscopy and surface plasmon resonance spectroscopy with imaging optics, optical fibers and / or the use of brilliant radiation sources (eg gas laser, QCLs). Since the device makes a combined infrared and Raman analysis possible, a higher detection rate for the diagnosis compared to a single measuring method is made possible. In addition, the sample consumption is very low and is z. B. in the submicroliter range.
  • the microfluidic chip and the plate are interchangeable arranged in a common holding device. This facilitates handling, in particular the microfluidic chip can be exchanged in a simple manner.
  • the transparent plate must be chosen from a material that is transparent to both visible light (Raman spectroscopy and surface plasmon resonance spectroscopy) and infrared. It is therefore preferred that the plate consists of calcium fluoride, barium fluoride or zinc selenide.
  • the microfluidic chip may consist of inexpensive materials. Preferably, it consists z. B. plastic (polymer material) or glass.
  • the metal island film can basically consist of different metals. Particular preference is given to using gold or silver. Other metals, e.g. Platinum, are also suitable.
  • the metal island film can basically be applied to the board in a variety of ways. It is preferably provided that the metal island film is applied to the plate by thermal evaporation under high vacuum conditions, i. evaporated. Alternatively, colloidal solutions or etching processes can also be used for the production.
  • the individual metal islands have dimensions of the order of 20 to 100 nm, whereas the at least one microchannel of the microfluidic chip has a width of the order of 50 to 100 ⁇ m.
  • the coverage of the plate in the area of the measuring window with the metal island film is about 80 to 90% compared to the total area in the measuring window for infrared, for Raman is a much lower
  • the metal island film is covered by an ultrathin protective layer. This, some nm thick
  • Protective layer e.g. is made of silicon oxide, allows the multiple usability and cleaning of the microfluidic channel covering plate.
  • an ultrathin organic functional layer is applied to the metal film or the protective layer.
  • a further embodiment provides that the major axes of the metal islands are aligned parallel to one another in order to use the coupling of the plasmonic resonances defined between the individual metal islands along the main axes.
  • a further embodiment provides that the distance between the edges of two directly adjacent metal islands along the direction of their main axes is smaller than the length of the main axis of the respective metal island.
  • an asymmetric distance distribution between the individual metal islands is produced, wherein the distance between the edges of two adjacent metal islands along the major axes is smaller than the distance along the minor axes.
  • the distance between the edges of two adjacent metal islands along the main axes should preferably be less than 10 nm in order to optimally use the SEI RA effect.
  • Another embodiment provides that the main axes of the metal islands are aligned in a preferred direction to allow polarization-dependent measurement, which are optimized for certain applications.
  • FIG. 1 is a schematic representation of a device according to the invention in section
  • Fig. 3 is a schematic representation of an isotropic metal island film on the plate of the device.
  • Fig. 4 is a schematic representation of an isotropic metal island film on
  • a device for the detection and characterization of organic molecules in a liquid sample volume in the micro- and sub-microliter range by means of surface-enhanced Raman and infrared and surface plasmon resonance spectroscopy is generally designated 1.
  • This device 1 is particularly suitable for the following spectroscopy methods:
  • the device 1 initially has a microfluidic chip 2, in whose upper side at least one microfluidic channel 3 is provided.
  • this microfluidic channel 3 is connected at its inlet to an inlet 4 accessible from the underside of the microfluidic chip 2 and at the outlet to an outlet 5 accessible from the underside of the microfluidic chip 2, so that a flow direction for the liquid sample in the microfluidic channel 3 in FIG Meaning of the arrows 6 results.
  • At least the region of the microfluidic channel 3, but preferably the entire microfluidic chip 2 is covered at the top by a transparent plate 7 serving as a measuring window. This at least for infrared light and visible light transparent plate 7 is coated on the side facing the microfluidic channel 3 side with a metal island film, the metal islands are denoted by 8 and indicated schematically.
  • metal islands 8 which are preferably made of gold or silver or also of platinum, can be applied in different ways to the underside of the plate 7, e.g. by vapor deposition from a high vacuum. Alternatively, colloidal solutions or etching methods may also be used.
  • a vane-shaped holding device 9 is provided, on the underside of which an opening 10 is provided in the region of the inlet 4 and an opening 11 in the region of the outlet 5 in order to supply and remove the sample can.
  • an opening 10 is provided in the region of the inlet 4 and an opening 11 in the region of the outlet 5 in order to supply and remove the sample can.
  • one or more height-adjustable clamping plates 13 are provided, which rest with its underside clamping the top of the plate 7 and record both the microfluidic chip 2 and the plate 7 stationary in the holding device 9.
  • the device 1 also has a detection optics 14, which can be configured differently.
  • the detection optics 14 is an imaging optics (for example, lens or mirror objectives), which serves to focus the incident light on the sample, ie on the plate 7.
  • the incident light rays are indicated by 15, with variable incidence and angle of departure are possible.
  • the light reflected on the surface of the microfluidic channel 3 or of the metal-inscribed film can be guided by the same or a separate optic in reflection onto a detector, not shown, the reflected beams are indicated by 16.
  • the detector, not shown is part of a spectrometer, also not shown, for. B. a dispersive or inteferometric spectrometer.
  • the metal island film has a multiplicity of metal islands 8, the order of magnitude of these metal islands 8 being, for example, between 20 and 100 nm, while the width of the microfluidic channel 3 is about 100 ⁇ m.
  • the arrangement of the metal islands 8 is basically arbitrary.
  • the degree of coverage of the underside of the plate 7 is at most about 80 to 90%.
  • the island film is isotropic.
  • the substrate in this case shows both Raman and infrared enhancement.
  • the polarization direction of the light which is indicated in each case by a double arrow for infrared (reference numeral 17) and Raman (reference numeral 18), is irrelevant and can also be unpolarized.
  • FIG. 4 An isotropic arrangement is shown in FIG. In this case, a polarization direction for Raman (reference numeral 18) and a direction for infrared (reference numeral 17) are optimized. In FIG. 4, the two polarization directions are thus perpendicular to one another. But it can also be other, not mutually perpendicular directions, as long as one is designed for infrared and the other optimal for Raman.
  • the sample volume in the micro- or even submicroliter range is conveyed through the microfluidic channel 3. Meanwhile, the single sample volume can be sequentially measured with different Raman and infrared microscopes or in the same setup for Raman and Infrared.
  • the transparent plate 7 must be transparent to infrared and visible light and preferably consists of calcium fluoride (CaF 2 ), barium fluoride (BaF 2 ) or zinc selenide (ZnSe). Of course, other infrared and visible light transparent materials are possible. LIST OF REFERENCE NUMBERS

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Analytical Chemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Pathology (AREA)
  • Biochemistry (AREA)
  • Physics & Mathematics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Immunology (AREA)
  • Engineering & Computer Science (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Nanotechnology (AREA)
  • Dispersion Chemistry (AREA)
  • Hematology (AREA)
  • Clinical Laboratory Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

L'invention concerne un dispositif (1) de détection et de caractérisation de molécules organiques dans un volume d'échantillon liquide de l'ordre du microlitre ou du submicrolitre au moyen d'une spectroscopie Raman ou infrarouge, en particulier au moyen de la spectroscopie Raman de résonance (RR), de la spectroscopie Raman exaltée en surface (SERS), de la spectroscopie Raman anti-Stokes cohérente exaltée en surface (SE-CARS), de l'absorption infrarouge exaltée en surface (SEIRA) et de la résonance plasmonique de surface (SPR). L'invention vise à obtenir une détection et une caractérisation simples de molécules organiques présentant une concentration inférieure au domaine des ppm dans un volume d'échantillon liquide de l'ordre du microlitre et du submicrolitre en raisons de caractéristiques vibratoires des molécules au moyen dudit procédé de spectroscopie Raman et de spectroscopie infrarouge dans un dispositif unique. Cet objectif est atteint grâce à une puce microfluidique (2) dotée d'au moins un canal microfluidique (3) ouvert vers le haut pour l'écoulement du volume d'échantillon et grâce à une plaque (7) transparente recouvrant ledit au moins un canal microfluidique (3) et servant de de fenêtre de mesure, laquelle plaque est revêtue, sur le côté tourné vers ledit au moins un canal microfluidique (3), d'un film d'îlots métalliques, les îlots métalliques (8) se présentant sous forme d'ellipses, et grâce à un système optique de détection (14) orienté vers la plaque (7), lequel système optique de détection émet de la lumière (15) sur la plaque (7) et reçoit les faisceaux lumineux (16) réfléchis.
PCT/EP2017/050864 2016-01-21 2017-01-17 Dispositif de détection et de caractérisation de molécules organiques dans un volume d'échantillon liquide Ceased WO2017125374A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102016101001.4A DE102016101001B4 (de) 2016-01-21 2016-01-21 Vorrichtung zur Detektion und Charakterisierung von organischen Molekülen in einem flüssigen Probenvolumen
DE102016101001.4 2016-01-21

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Cited By (4)

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EP3586962A1 (fr) * 2018-06-22 2020-01-01 Unchained Labs Germany GmbH Système de support d'échantillon magnétique pour un microscope raman
CN110865066A (zh) * 2019-11-18 2020-03-06 南通大学 一种全反射结构的拉曼光谱样品盒
CN113058668A (zh) * 2021-03-20 2021-07-02 山东大学 一种基于电容性超材料结构的人工表面等离激元的微流控检测芯片结构及其制备、检测方法
CN117686435A (zh) * 2023-12-07 2024-03-12 华中农业大学 用于透明流体类食品检测的微流控芯片及制造方法

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3586962A1 (fr) * 2018-06-22 2020-01-01 Unchained Labs Germany GmbH Système de support d'échantillon magnétique pour un microscope raman
CN110865066A (zh) * 2019-11-18 2020-03-06 南通大学 一种全反射结构的拉曼光谱样品盒
CN113058668A (zh) * 2021-03-20 2021-07-02 山东大学 一种基于电容性超材料结构的人工表面等离激元的微流控检测芯片结构及其制备、检测方法
CN113058668B (zh) * 2021-03-20 2022-05-27 山东大学 一种基于电容性超材料结构的人工表面等离激元的微流控检测芯片结构及其制备、检测方法
CN117686435A (zh) * 2023-12-07 2024-03-12 华中农业大学 用于透明流体类食品检测的微流控芯片及制造方法

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