• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    Sensor, apparatus and procedure for the determination of solute concentration in solutions. This document describes a sensor, an apparatus and method that allows a direct analysis of fluids to determine quantities of solutes in solutions. For this purpose, it is possible to use transducers with monolayer or multilayer structures (such as a planar photonic structure in the form of a bragg microcavity) porous birefringent. The method of the invention presents two possible configurations; a first configuration in which there is a sensor that is photonic crystal in a microfluidic structure comprising two transparent windows, taking the data capture in transmission mode, and a second configuration in which the photonic crystal that acts as a sensor it is located at one end of an optical fiber, proceeding to the data collection in the reflection mode. (Machine-translation by Google Translate, not legally binding)
    公开号:ES2612340A1
    申请号:ES201531540
    申请日:2015-10-27
    公开日:2017-05-16
    发明作者:Manuel OLIVA RAMÍREZ；Francisco Yubero Valencia；Ángel BARRANCO QUERO；Agustín RODRÍGUEZ GONZÁLEZ-ELIPE；Luis José Fernández Ledesma；Miguel Holgado Bolaños
    申请人:Consejo Superior de Investigaciones Cientificas CSIC；Universidad Politecnica de Madrid；Universidad de Zaragoza；
    IPC主号:
    专利说明:

    OBJECT OF THE INVENTION
    The object of the invention is framed in the field of analytics. More specifically, the object of the invention is directed to the determination of the concentration of a solute within a solution, said determination being carried out by optical means using photonic transducers in the form of a porous thin layer. BACKGROUND OF THE INVENTION
    There are many analytical methodologies that allow to determine concentrations of different solutes in solutions. Thus, in industries such as the brewery and others related to the manufacture of similar beverages, a fermentation process is controlled by means of measurements with a pycnometer, which measures the density of the solution, which is then correlated with the concentration of dissolved solute. In this way, for example, it is possible to identify the amount of sugar in a solution in a fermentation process.
    Likewise, there are many optical methods for the determination of solutes in solutions among which those based on optical absorption, colorimetry, fluorescence or change of refractive index of liquids are widely used. Specifically, for the determination of glucose or sugars in general in aqueous solutions, so-called refractometers are used, devices that identify the refractive index of liquids, since this parameter depends on the degree of concentration of the solution. In order for the refractive index analysis to be effective, these devices require a minimum sample volume (liquid to be analyzed) of the order of 0.1-1.0 ml, and also that the sample be relatively transparent and without turbidity. On the other hand, their operation is “ex-situ” and requires a sampling and analysis in an external system.
    In the field of analysis of solutions and fluids, there is generally a growing trend towards the use of microfluidic devices. These generally have an input and output between which one or more section channels with micrometric dimensions (tens / hundreds of microns in size) run and where different analytical determinations can be performed continuously. These devices have advantages such as the consumption of small volumes of solution for diagnosis, rapid analysis, compact systems due to the integration of several functionalities in small volumes, lower manufacturing costs to make the development of disposable chips profitable through their mass production, etc.
    In the field of microfluidics, different means of determining the characteristics of the fluid circulating through the microchannels are used, with the possibility of developing methods based on optical measurements with systems or components integrated in the microchannels that, acting as transducers, present a change in optical response when the corresponding liquid passes through them. A well-known and widely used example for a wide variety of applications is the determination of changes in the plasmonic response of nanoparticles or very thin layers of metals such as gold or silver.
    The optical detection in microfluidics is especially interesting due to its non-invasive character, rapid response and, in general, high sensitivity. In this sense there are configurations in which optical detection transducers based on absorption effects, fluorescence or optical interferences using photonic structures, exalted surface Raman or the aforementioned based on surface plasmon resonance are used.
    Regarding the development of analyte sensors in solutions based on the monitoring of optical interferences using photonic structures, it is worth mentioning document US9007593 in which a method for assessing amounts of solute in solution vapors is described. The method consists of exposing porous layers that form structures of Bragg mirrors, microcavities or “rugate” filters to the vapors to be analyzed and to follow the variation of the optical response of this porous layer after thermal cycles. The magnitude and shape of the hysteresis processes in the optical response after thermal cycles correlates with the presence and quantity of solutes present in the analyzed vapors. In spite of this, this method requires high temperatures to be able to measure solutes, reaching 200ºC as low temperature, and requires heating and cooling the solution, resulting in an important energy expenditure.
    WO2010 / 026269A1 describes an optical detection system for high sensitivity bioassays without marking, which is based on the monitoring of the optical response (spectral response of the interference profile, measured in reflection / transmission following its angular dependence on function of the wavelength) of three-dimensional nanostructures that incorporate molecular markers anchored thereon (nanopillars, Fabry Perot structures or other equivalents) after exposure to solutions, in this case integrated into fluidic devices. That is, this system requires a plurality of sensitive bio-photonic cells deposited on a substrate, resulting in a configuration that, although not requiring microfluidic elements, is complex. This complexity is reflected in the manufacturing process comprising at least two stages plus an additional stage of anchoring specific bioreceptors. Also, this detection system requires the spectral detection (depending on the wavelength) of optical interference phenomena.
    Alternatively, the present invention is a novel simple layer or optically active planar photonic structure, wherein the detection is based on the generation and monitoring of the offset between the components of the electric field of the incident polarized light, as it is reflected or transmitted by the sensor part (transducer) of the device (optically active planar photonic porous structure). The photonic structure can be part of the microfluidic chip through which the problem solution circulates, or it can be integrated into the end of an optical fiber by introducing it into the solution to be analyzed. In no case does it require the incorporation of molecular markers for its operation. DESCRIPTION OF THE INVENTION
    In a first aspect of the invention there is a sensor for the determination of solute concentration in solutions defined by a transducer formed by a porous planar photonic structure.
    In a second aspect of the invention there is an apparatus that integrates in a microfluidic device the planar photonic transducer or sensor of the first aspect of the invention, which is in contact with the solution to be analyzed. To proceed with the measurement, the solution is circulated through the microfluidic device where the sensor is located, putting it in contact with the solution flowing through the interior of the microfluidic device. Said apparatus is integrated with an optoelectric detection system, coupling a polarized light source and a light ellipticity analysis system. As a whole, the system allows you to interrogate and have information about the optical properties, basically the refractive index, of the liquid or solution that circulates through the microfluidic device.
    In a third aspect of the invention there is a method for determining the concentration of solutes in solutions that makes use of the sensor of the first aspect of the invention, where the apparatus of the second aspect of the invention is in whose microfluidic device the problem solution circulates , also making use of the aforementioned optoelectric detection system.
    The invention, in all its aspects, is based on the use of a sensor that acts as a transducer of the optical properties of liquids and which comprises an optically active planar photonic structure composed of one or more porous thin layers, preferably prepared by techniques. of physical deposition in vapor phase (evaporation or sputtering) in a geometric configuration of material contribution according to a flush angle between the source of deposited material and the surface of the substrate on which the thin layer is deposited. These types of thin layers have a columnar structure in cross section with an anisotropic porosity. The final transducer can be defined by a single layer of a single material or a stack of several layers that make up a multilayer structure with alternating layers of different index of refraction. In both cases a basic condition is that all the components of the transducer have birefringence (different index of refraction in two perpendicular directions) in the plane and a high porosity.
    By affecting linearly polarized light on the sensor, which has infiltrated the solution whose solute concentration is to be determined, with the polarized vector misaligned with respect to its optical axes, the ellipticity of the reflected and / or transmitted light by the photonic structure it depends on the refractive index of the liquid that infiltrates the sensor and is therefore characteristic of the concentration of the solute in the solution. Specifically, the sensor acts as an optical retarder, so that the analysis of the induced delay between the two components of the polarization of light is a measure of the concentration of a given solute in a solution.
    A first possible configuration of the sensor is to consider a single microstructured porous thin layer (for example of TiO2) that has a high birefringence, preferably above 0.15 (i.e. high optical activity), in the sample plane. When the polarized light strikes this layer with the polarization axis forming a certain angle (preferably 45 °) with respect to the optical axes of the layer, variations in the magnitude of the ellipticity of the incident light when it is reflected / transmitted by the device (quotient between the components of the electric field of the parallel light and perpendicular to the polarization vector of the incident light beam) constitutes a measure of the variation in the refractive index of the solution that infiltrates the pores of the optically active layer. The intensity of these variations depends on the magnitude of the birefringence of the layer, the alignment of the polarization of the incident light with respect to its optical axes and its thickness. One way to follow these variations is to measure the ratio between the intensities of transmitted / reflected light after crossed polarizers and aligned with the polarization vector of the incident light, with the microfluidic device located between them.
    Another possible configuration of the sensor of this invention consists of an optical microcavity separated by two Bragg mirrors (Bragg microcavity), formed by the superposition of two birefringent one-dimensional photonic crystals separated by another porous layer, also birefringent, which acts as an optical defect. In order to obtain the desired optical interference pattern, some optical contrast is necessary between the materials of the constituent layers of the device. Thus, it is preferably proposed, but not restrictive, the use of SiO2 and TiO2 as constituent materials of the layers alternately. As an example, if two Bragg mirrors consisting of 7 porous layers (50% pore volume) alternated with TiO2 and SiO2 of approx. 85 nm each and a layer that acts as an optical SiO2 defect of approx. 200 nm, a pattern of transmitted light interference is achieved consisting of a window of reflected light between 500 and 700 nm, in which a narrow resonant peak of transmission around 600 nm is appreciated. By making polarized light strike on this Bragg microcavity, with the polarization axis forming a certain angle (preferably 45 °) with respect to the optical axes of the layer in which the problem solution has infiltrated, variations in the magnitude of the ellipticity of the incident light in the light reflected / transmitted in the device are a measure of the variation in the refractive index of the solution that infiltrates the pores of the birefringent multilayer structure. If the analysis is done by filtering the light around wavelengths at which the resonant peak of the Bragg structure appears, the sensitivity in the analysis is maximized.
    The manufacturing with a zig-zag columnar topology of the porous structure of these multilayers using the flush angle deposition technology confers an increase in optical activity (birefingency) to the individual layers, this being consequently a preferred mode of manufacturing the layers. same. This increase in birefringence results in a greater sensitivity to solute concentrations in the solutions. Another topology that also confers optical activity to this planar structure in the form of multilayers is that in which the inclined columns of the different constituent layers are oriented in the same direction.
    In a first variant of the apparatus of the second aspect of the invention, the sensor formed by the optically active porous layer can be included in a microfluidic circuit with two transparent windows, data being taken in transmission or reflection mode. In a second variant of the apparatus of the second aspect of the invention, the sensor located within the microfluidic device can be interrogated directly with an optical fiber, data being taken in the reflection mode. This detection mode can also be used by placing the sensor directly on the tip of an optical fiber that is introduced directly into the solution, thus dispensing with the microfluidic system. DESCRIPTION OF THE DRAWINGS
    To complement the description that is being made and in order to help a better understanding of the characteristics of the invention, according to some preferred examples of practical implementation thereof, a set of drawings is attached as an integral part of said description. where, for illustrative and non-limiting purposes, the following has been represented:
    Figure 1. Shows an operation scheme of the apparatus for the determination of glucose or other solutes in aqueous solutions working in the transmission mode. This scheme shows: the microfluidic device (1), the sensor (2), the light polarization analyzer (3), the polarized light beam (4), optical filter (5), the polarized transmitted light parallel (6) to the initial of the incident beam, with intensity I2, light transmitted with perpendicular polarization (7) to the initial of the incident beam, with intensity I1, the photodiode (8).
    Figure 2.- Shows an operation scheme of the apparatus for the determination of glucose or other solutes in aqueous solutions working in the reflection mode. This scheme shows: the sensor (2) as an optically active planar photonic transducer, the light polarization analyzer (3), the polarized light beam (4), the optical filter (5), the reflected light with intensity I2 and parallel polarization (6) with respect to the initial of the incident beam, the light reflected with intensity I1 and perpendicular polarization (7) with respect to the initial of the incident beam, the photodiode (8), the polarizer (9) and the fiber optics (10).
    Figure 3. It shows a front view of the microfluidic device (1) that includes the sensor (2) with its optical axes (dashed lines) forming an angle of 45 ° with a polarization vector of the incident light.
    Figure 4. It shows a graph showing the calibration curve in microfluidic device based on a birefringent porous single layer for determination of glucose in aqueous solutions working in the transmission mode. The graph shows the ratio between the intensities of light transmitted by the analyzed device after a crossed polarizer or aligned with the polarization vector of the incident beam.
    Figure 5. Shows a graph showing the calibration curve in microfluidic device based on birefringent porous multilayer (Bragg microcavity) for determination of glucose in aqueous solutions working in the transmission mode. The graph shows the ratio between the intensities of light transmitted by the analyzed device after a crossed polarizer or aligned with the polarization vector of the incident beam. PREFERRED EMBODIMENT OF THE INVENTION
    In the first aspect of the invention referred to a sensor (2) for determining the concentration of solutes in solutions, there is a sensor formed by one or several porous and optically active layers presenting birefringence, which are prepared by physical deposition in phase steam in flush oblique angle geometry.
    Preferably, this porous and optically active layer is manufactured by evaporation by electron bombardment of a blank in a vacuum chamber located at a distance between 20 and 100 cm of a flat substrate (glass, quartz, etc.) oriented with its perpendicular forming an angle of 70 ° or more with respect to the direction of the flow of evaporated atoms from the target. In an alternative embodiment in which the sensor (2) is formed by photonic structures that integrate a multitude of layers, the substrate can be held fixed when it is passed from one layer to the next or rotated 180 ° from one layer to the next. In both embodiments the resulting planar photonic structure is optically active. Other physical vapor deposition techniques such as sputtering can also be used for the manufacture of these optically active layers and structures.
    In a preferred embodiment of the method corresponding to the third aspect of the invention, a sensor-like photonic transducer (2) is used comprising at least one porous birefringent layer of a single material (for example TiO2) with a thickness between 0 , 2 and 3.0 microns and prepared in a flush angle configuration that is placed inside a chip or microfluidic device (1) with its optical axes forming an angle of 45º with respect to the polarization vector of the incident light, as presented in Figure 3. To maximize the sensitivity of the method it is convenient, although not limiting, that the birefringence value be 0.15 or higher. As Figure 1 illustrates, the light transmitted through the microfluidic device (1), which includes the photonic transducer that acts as a sensor (2), is analyzed with a light polarization analyzer (3), which separates the parallel (6) and perpendicular (7) contributions of the electric field of the transmitted light beam (with respect to the polarization state of the incident light beam). The respective intensities I1 / I2 of these light beams are measured by photodiodes (8) and the ratio between the same I1 / I2 is evaluated. Variations in the solute concentration in the solution that fills the pores of the birefringent porous photonic transducer will become apparent as variations in the I1 / I2 ratio values, as shown in Figure 4.
    In a second aspect of the invention there is an apparatus that integrates in the microfluidic device (1) the planar photonic transducer or sensor (2), which is in contact with the solution to be analyzed. To proceed with the measurement, the solution is circulated through the microfluidic device (1) where the sensor (2) is located, putting it in contact with the solution flowing through the interior of the microfluidic device (1), to interrogate and have information on the optical properties, basically the refractive index, of the liquid or solution that circulates through the microfluidic device (1).
    Preferably, the microfluidic device (1) comprises at least two transparent windows in the ranges of the visible and near infrared spectra, the sensor (2) being included in the microfluidic circuit (1) disposed between said transparent windows.
    Optionally, the sensor (2) is located at the end of an optical fiber insertable in the microfluidic device (1).
    In a more preferred embodiment of the method of the invention, a sensor (2) is used that acts as a transducer formed by a Bragg microcavity in turn formed by a series of stacked birefringent layers and of different refractive index (for example TiO2 and SiO2 of thicknesses around 80 nm with a central SiO2 defect approximately 200 nm thick) prepared in a flush angle configuration. This planar photonic structure is placed with its optical axes at an angle of 45 ° with respect to the polarization vector of the incident light, as presented in Figure 3. In this case the incident polarized light is passed through an optical filter ( 5) whose transmission window is centered on the transmission peak of the Bragg microcavity used. The light transmitted through the microfluidic device (1), which includes the photonic sensor (2) is analyzed with a light polarization analyzer (3), which separates the parallel (6) and perpendicular (7) contributions from the field electrical of the transmitted light beam (with respect to the polarization state of the incident light beam). The intensities of these light beams are measured with photodiodes (8) and the ratio between the same I1 / I2 is evaluated. Variations in the solute concentration in the solution that fills the pores of the birefringent porous photonic transducer will become apparent as variations in the I1 / I2 ratio values. For example, the ratio of transmitted light intensities with an electric field perpendicular and parallel to the polarization vector of the incident light is evaluated and by correlation with a calibration line, this ratio is a measure of the solute concentration in the solution. The results of this calibration process are presented in Figure 5.
    In an alternative embodiment of the invention in which the sensor is facing one end of an optical fiber at a given distance, the reflection spectra are recorded with aligned and crossed polarizers, giving rise to a series of spectra in function of the concentration of solute that infiltrates the pores of the layer.
    From an optical point of view, the reflection measurement is also compatible with the arrangement of the system in the microfluidic circuit, although it can also be used by direct immersion of the end of the fiber-sensor system in the liquid to be analyzed. An example of the embodiment of the invention in the first case is illustrated in Figure 2, according to which the light transmitted by an optical fiber (10) is filtered (5) and polarized (9) before reaching the sensor (2 ) in contact with the liquid to be analyzed. The reflected light is divided into its components according to its polarization plane (3) and the intensity of the parallel (6) and perpendicular polarized lights (7) with respect to the initial beam, measuring their intensities I1 and I2 by means of two photodiodes .
    As an example of the calibration process between the variation of intensities I1 / I2 when varying the concentration of solute in a glucose water solution, Figure 4 shows the calibration curve in a microfluidic device based on a birefringent porous single layer for glucose determination in aqueous solutions working in the transmission mode. The graph shows the ratio between the intensities of light transmitted by the analyzed device after a crossed polarizer or aligned with the polarization vector of the incident beam.
    Finally, Figure 5 shows the calibration curve in microfluidic device based on birefringent porous multilayer (Bragg microcavity) for determination of glucose in aqueous solutions working in the transmission mode. The graph shows the ratio between the intensities of light transmitted by the analyzed device after a crossed polarizer or aligned with the incident beam polarization vector
    It is possible to functionalize the internal surfaces of the pores of the photonic crystal layers to make it selective to certain solvents, for example so that it is not sensitive to polar solvents (water), preventing such solvents from infiltrating into said pores. This functionalization can be done by anchoring apolar molecules by chemical methods on the exposed oxidic surfaces of the pores so that only apolar solvents have a tendency to infiltrate inside them. This sensor configuration is especially recommended for testing mixtures of two solvents so that the optical response is exclusively a function of the characteristics of the apolar solvent, which would selectively infiltrate the pores of the sensor.
    权利要求:
    Claims (10)
    [1]
     R E I V I N D I C A C I O N E S
    one.  Sensor (2) for determining the concentration of solutes in solutions, wherein the sensor (2) is characterized in that it comprises at least one porous and optically active layer presenting birefringence.
    [2]
    2.  Sensor (2) according to claim 1 characterized in that it additionally comprises two porous one-dimensional photonic crystals formed by birefringent layers of different refractive index separated by a central porous layer, defining a Bragg microcavity.
    [3]
    3.  Sensor (2) according to claims 1 or 2 characterized in that the photonic crystals comprise alternating layers of SiO2 and TiO2.
    [4]
    Four.  Sensor (2) according to any one of claims 1 to 3 characterized in that the internal surfaces of the pores of the porous layer are functionalized.
    [5]
    5.  Apparatus for determining the concentration of solutes in solutions comprising a microfluidic device (1), characterized in that:
    x the microfluidic device (1) in turn comprises a sensor (2) as described in any one of claims 1 to 4 associated with the microfluidic device (1), and
    x The apparatus comprises a polarized light beam source (4), an optical filter (5), a light polarization analyzer (3) and photodiodes (8).
    [6]
    6.  Apparatus according to claim 5 characterized in that the microfluidic device (1) comprises at least two transparent windows in the ranges of the visible and near infrared spectra, the sensor (2) being included in the microfluidic circuit (1) disposed between said transparent windows.
    [7]
    7.  Apparatus according to claim 5 characterized in that the sensor (2) is located at the end of an optical fiber inserted in the microfluidic device (1).
    [8]
    8.  Method for determining the concentration of solutes that makes use of an apparatus as described in claim 5, the method being characterized in that it comprises:
    i. contact the sensor (2) with a solution whose concentration is to be determined,
    ii. illuminate the sensor (2) with linear polarized light once infiltrated with the solution whose concentration is to be determined,
    iii. analyze the light transmitted or reflected through the microfluidic device
    (1) by means of a light polarization analyzer (3), which allows discriminating between parallel (6) and perpendicular components (7) with respect to the polarization vector of the beam of light transmitted or reflected through the microfluidic device (1) .
    iv. determine the respective intensities I1 / I2 of these light beams using photodiodes (8), and
                      v. calculate the quotient between intensities I1 / I2, and
    saw. determine the concentration of solutes from variations in the I1 / I2 quotient values by correlation with a calibration line.
    [9]
    9.  Method according to claim 8, characterized in that the sensor is part of the microfluidic device (1) which in turn comprises two transparent windows in the ranges of the visible and near infrared spectra, the sensor being located between said transparent windows proceeding to the data collection in reflection mode.
    [10]
    10.  Method according to claim 8, characterized in that the sensor (2) is located at one end of an optical fiber that is introduced directly into the solution, data being taken in the reflection mode by means of recording reflection spectra with some aligned and crossed polarizers, giving rise to spectra based on solute concentration.
    7
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    同族专利:
    公开号 | 公开日
    ES2612340B1|2018-03-09|
    WO2017072388A1|2017-05-04|
    BR112018008502A2|2018-10-23|
    US20180328838A1|2018-11-15|
    EP3379233A1|2018-09-26|
    MX2018005253A|2019-07-04|
    引用文献:
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    US8280470B2|2006-11-03|2012-10-02|Volcano Corporation|Analyte sensor method and apparatus|
    ES2334318B2|2008-09-05|2011-11-28|Universidad Politécnica de Madrid|OPTICAL DETECTION SYSTEM FOR BIO-TESTS OF HIGH SENSITIVITY SINMARCADO.|
    WO2012012437A2|2010-07-20|2012-01-26|The Regents Of The University Of California|Temperature response sensing and classification of analytes with porous optical films|
    US9739710B2|2012-10-15|2017-08-22|Nutech Ventures|Optical sensing and separation based on ordered three-dimensional nanostructured surfaces|CN109884063B|2019-04-24|2021-08-20|杭州翔毅科技有限公司|Acquisition structure for liquid sensor|
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    申请号 | 申请日 | 专利标题
    ES201531540A|ES2612340B1|2015-10-27|2015-10-27|SENSOR, DEVICE AND PROCEDURE FOR THE DETERMINATION OF THE CONCENTRATION OF SOLUTIONS IN DISSOLUTIONS|ES201531540A| ES2612340B1|2015-10-27|2015-10-27|SENSOR, DEVICE AND PROCEDURE FOR THE DETERMINATION OF THE CONCENTRATION OF SOLUTIONS IN DISSOLUTIONS|
    PCT/ES2016/070764| WO2017072388A1|2015-10-27|2016-10-27|Sensor, apparatus and method for determining a concentration of a solute in a solution|
    EP16805879.0A| EP3379233A1|2015-10-27|2016-10-27|Sensor, apparatus and method for determining a concentration of a solute in a solution|
    US15/771,854| US20180328838A1|2015-10-27|2016-10-27|Sensor, apparatus and method for determining a concentration of a solute in a solution|
    MX2018005253A| MX2018005253A|2015-10-27|2016-10-27|Sensor, apparatus and method for determining a concentration of a solute in a solution.|
    BR112018008502A| BR112018008502A2|2015-10-27|2016-10-27|sensor, apparatus and method for determining glucose concentration in solutions|
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