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WO2015028365A1 - Méthode d'analyse pour déterminer les types et les concentrations de bioparticules - Google Patents

Méthode d'analyse pour déterminer les types et les concentrations de bioparticules Download PDF

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Publication number
WO2015028365A1
WO2015028365A1 PCT/EP2014/067726 EP2014067726W WO2015028365A1 WO 2015028365 A1 WO2015028365 A1 WO 2015028365A1 EP 2014067726 W EP2014067726 W EP 2014067726W WO 2015028365 A1 WO2015028365 A1 WO 2015028365A1
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WO
WIPO (PCT)
Prior art keywords
analysis method
sample
particles
scattering angle
light beam
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/EP2014/067726
Other languages
German (de)
English (en)
Inventor
Miroslav Kocifaj
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.)
Siemens Healthcare Diagnostics Products GmbH
Siemens Healthcare Diagnostics Inc
Original Assignee
Siemens Healthcare Diagnostics Products GmbH
Siemens Healthcare Diagnostics Inc
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 Siemens Healthcare Diagnostics Products GmbH, Siemens Healthcare Diagnostics Inc filed Critical Siemens Healthcare Diagnostics Products GmbH
Publication of WO2015028365A1 publication Critical patent/WO2015028365A1/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
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/02—Investigating particle size or size distribution
    • G01N15/0205—Investigating particle size or size distribution by optical means
    • G01N15/0211—Investigating a scatter or diffraction pattern
    • 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
    • G01N21/47—Scattering, i.e. diffuse reflection
    • G01N21/49—Scattering, i.e. diffuse reflection within a body or fluid
    • G01N21/51—Scattering, i.e. diffuse reflection within a body or fluid inside a container, e.g. in an ampoule
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/01—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials specially adapted for biological cells, e.g. blood cells
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N2015/0042—Investigating dispersion of solids
    • G01N2015/0053—Investigating dispersion of solids in liquids, e.g. trouble
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N2015/0042—Investigating dispersion of solids
    • G01N2015/0061—Investigating dispersion of solids in solids, e.g. petrography
    • 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
    • G01N21/47—Scattering, i.e. diffuse reflection
    • G01N2021/4704—Angular selective
    • G01N2021/4711—Multiangle measurement
    • 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
    • G01N21/47—Scattering, i.e. diffuse reflection
    • G01N2021/4792—Polarisation of scatter light

Definitions

  • the invention relates to an analysis method for determining at least one element of a Müller matrix of a sample with biological particles, wherein a light beam is scattered by the sample. Furthermore, the invention relates to an analysis system for carrying out the aforementioned method.
  • a Müller matrix can be used to mathematically translate the operation of almost any optical element. For example, changes in direction, changes in polarization, absorption and the like, with the indication of the Muller matrix 4 * 4, so a total of sixteen elements S U, has ⁇ described.
  • the Stokes vector of a scattered light beam on a sample can be determined by, be applied to the Stokes vector of the incident light beam, the Mueller matrix, which writes be the effect of the sample on the light ⁇ .
  • the Müller matrix contains information about the size, shape and refractive index of the particles contained in the sample. If, for example, be a mixture of different particle types ⁇ , the determined Mueller matrix is characteristic of this speziel- le mixture.
  • mixture of particles of different particle types is comprised of a superposition of several matrices Müller, the latter being characterizedis ⁇ table for the respective particle types.
  • heranzu ⁇ pull spectroscopic methods to analyze particles in a random manner in a sample and to detect.
  • ⁇ eventually leads up to a fingerprint of a sample, wherein both the real and the imaginary part of a spec- trum Resonanzfre- be used for the analysis.
  • This Metho ⁇ de relies primarily on the resolution of the wavelength used, wherein also the problem is ent ⁇ that optionally two very similar particle types are present, which differ slightly in their characteristics. Thus, again the problem is such
  • the invention is based on the object, an analysis method and an analysis system for determining at least one
  • the analysis system is therefore characterized in that at least a discrete scattering angle the scattered radiation over a defined frequency and wavelength range is detected.
  • two concepts for the investigation of biological particles are combined, whereby the amount of data available to the fingerprint is multiplied by the number of wavelengths that can be resolved.
  • this element is determined for a specific scattering angle and for a specific wavelength spectrum.
  • it behaves in such a way that the resonance phenomenon reacts very sensitively to small particle sizes or particle shapes and thus makes them easier to detect.
  • the inventive method has the further advantage that a very fast in-vitro diagnosis of biological see particles, either in liquids or on surfaces is made possible. It is not necessary to evenly align the biological particles in any form. It has been found that resonant scanning in a very precise manner allows the detection of particles that differ only very slightly from their size, shape or chemical properties. For example, it is possible particles, which have a refractive index difference of only 0.01 undoubtedly by their Resonanzsig ⁇ dimensional distinguished. This accuracy is not achievable with standard fingerprint methods.
  • so-called post-processing routines can be used to determine a plurality of biological substances / particles simultaneously, including their concentration. A comparison or fit between the measured and calculated data is performed. The calculated data are based on scattering and resonance behavior known from various biological particles and take into account, if necessary, a weighting.
  • the sample is not damaged by the resonance scattering measurement and is optionally repeated analyzed to rule out possible Feh ⁇ ler or uncertainties that could occur ⁇ during the experiment.
  • the optical approach avoids the use of chemical reagents. The fact that the first fixed scattering angle is chosen for the analysis, this is so selectable that one relies on a better data-related starting basis, to distinguish two or more similar ⁇ similar particle types from each other. This choice must therefore also be made in the wake of an already existing scattering experiment or a measurement with a conventional method.
  • the wavelength is changed in a wavelength interval that at least partially or completely belongs to the visible wavelength range.
  • the wavelength interval By choosing the wavelength interval quite be able ⁇ agreed particle sizes better detected and keep ⁇ tribuge.
  • the wavelength interval between 476 nanometers and 523 nanometers in the visible wavelength range is particularly well suited for particles which have a diameter of approximately 5 micrometers.
  • the element of the Mueller matrix will be ⁇ selected to distinguish between two types of particles from each other.
  • ⁇ selected to distinguish between two types of particles from each other.
  • the reliability of the statement is further increased by selecting, in addition to the first, fixed scattering angle, the second fixed scattering angle, a third fixed scattering angle, which extends the underlying data record once more.
  • the particles are randomly distributed in the sample.
  • no preparation steps are necessary, which affect the preparation of the sample and also represent possible sources of error.
  • the sample does not need to undergo a special procedure either before or after the analysis.
  • the sample is archived in order to be evaluated again, if necessary.
  • the particles are aligned in the same manner. For example, takes place Gleichaus ⁇ direction of the particles by applying an electric field or ispracticgeru fen ⁇ by other influences. This enables the analysis method to be performed with a light beam formed by pulses separated in time. Thus, the resolution or sharpness of the resonance peaks can be better implemented in the analysis data. If the orientations of the particles are random, an analysis based on a continuous (CW) regime is appropriate.
  • CW continuous
  • the light beam from temporally separate light pulses is formed, which are ideally generated by a pulsed laser source play mode coupled with active or passive ⁇ .
  • modulators can be used to generate the light pulses, which act modulating directly on a continuous beam of light.
  • a particle type and optionally a concentration of particles belonging to the particle type are determined.
  • the determined Mueller matrix which is characteristic of the particle mixture, is formed as a superposition of Muller matrices of individual particle types which are each weighted with a weighting parameter from which the concentration of the respective particle type can be determined. In purely mathematical terms, this results in a fit function with the matrices of the identified particle types and their associated weighting parameters.
  • the sample is either a liquid or a solid.
  • the liquid may be at ⁇ game as an emulsion or any other liquid containing chemical particles.
  • a solid ⁇ material whose outer layer is relevant, which is mixed with said particles, and optionally up to a GeWiS ⁇ sen degrees allows the penetration of the light beam.
  • Determining at least one element of a miller matrix of a sample with biological particles with a light source for generating a light beam, wherein the light beam is directed to the sample, at least one detector for detecting scattered light scattered on the sample at a first scattering angle with respect to the light beam wherein said light source to easily see ⁇ is to generate ge light beams with different wavelengths.
  • the light source is a light source, which is intended, for example by the Turn a micrometer screw or knob to change the wavelength of the emitted light beam.
  • This can be realized in different ways, for example by the adjustment of a cavity-internal filter or the like.
  • the light source is also composed of a plurality of light sources, each of which generates a different wavelength range or wavelength individually.
  • FIG. 1 shows an analysis system which, based on scattering and a subsequent analysis of the Stokes vector, is provided with auditory Müller-Matrix particle types and the concentrations of the respective particle types contained in a sample 5,4, analyzed and in particular makes particle types ⁇ divisible, which have very similar properties.
  • the analysis system has a (weilenlien-) tunable light source 12, which is given for example as a laser source, the light beam 6 first passes through a Polarisationsop ⁇ policy 13, then to hit the sample to be examined 5.
  • the sample 5 to be examined, as well as the remaining samples 4, are contained in test tubes, which are sealed off from the outside world with a top-mounted closure. Therefore, the sample 4, which remain to be Analy ⁇ se as well as the current to be examined sample 5 than to handle such archived and easily shown.
  • the light or laser beam 6 is scattered on the specimen 5 to be examined, whereby only three scattering angles 1, 2 , 3, namely 0r - 2 and -3, are taken into account for the analysis method.
  • the deflected in each case in the direction of said scattering angle 1,2,3 light is detected in each case by a separate De ⁇ Tektor and passed the respective detection signal to a controller.
  • the controller 7 is also used to control the light source 12, eg a laser source, by operating during a
  • Scattering measurement is successively tuned to the wavelength of the light source 12.
  • the data determined by the detectors 10 are stored together with the wavelength data on a computer 8 or server, so that this computer 8, possibly by means of an intermediate memory 9, the measured ⁇ nen data with a central database 11 via a communication level 14, such for example an intranet or the In ternet ⁇ , collation.
  • the analysis system is able to measure all Stokes parameters, thus capturing the entire Stokes vector of scattered light. Based on this, the associated Müller Matrix of the scattered light with knowledge of the Stokes vector of the light or laser beam 6 extractable.
  • Stokes parameters include, for example the intensity or the polarization- ⁇ on the scattered light.
  • the polarization optics 13 include, for example, polarizers and / or quarter lambda plates or else a modulator. The same applies to the detectors 10, each of which may also have quarter lambda plates for processing the scattered light.
  • the detectors 10 themselves can be designed, for example, as a photomultiplier.
  • Samples 4.5 are advantageously on a Zu Switzerlandmecha ⁇ mechanism (feeder) is placed, which is designed for test tubes.
  • a Zu Switzerlandmecha ⁇ mechanism feeder
  • Such a system is to be equipped easily with a bar code scanner ⁇ which allows to provide the samples 4.5 with a bar code and identify unambiguously in this way.
  • the light source 12 is controlled by the controller 7 by the computer 8 so that the wavelength is continuously variable over a predefined wavelength interval when the sample 5 is measured in the scattering experiment.
  • Part of the analysis of the measured resonance spectra is to compare these with calculated resonance spectra.
  • the correspondence between all measured and calculated Müller matrix elements is needed to detect the presence of a specific biological particle. It can be used to advantage complement this first analysis step, which determines the identity of the Parti ⁇ keltypen additional computer routines.
  • Ge ⁇ weighting parameters are determined that a synthetic magnetic resonance spectrum for individual biological particles contained combinatorial ⁇ kidney. In this way, both the identity of the particles and their relative concentration are determined by fitting the measured and the calculated spectra. This is a very advantageous method step, because different patent pathogenic consistent can be found without an emergency ⁇ necessity for independent measurements or additional chemical reagents see to have. The better the sensitivity of the
  • Detectors 10 such as a photomultiplier, is made, the better can be extremely low intensity with ⁇ th and therefore very low concentrations of biological particles detected. This is further improved by using a modulator in polarization optics 13 to eliminate background noise in a lock-in arrangement.
  • Measurements can be performed by using for the control or for calibration homogeneous isotropic particles with micro be ⁇ known physical properties. Standardized, calibrated or custom powder samples are available in the market and are easy to test the analysis apparatus are used.
  • a monodisperse sample 4 should be used to ⁇ containing a latex polystyrenes with different sized particles (for example, between 30 nanometers to a few micrometers). Such samples with small size distributions are well known. But there are also a number of pharmaceutical and chemical sources that can provide a wide range of test specimens with specific refractive indices, which also have different sizes and shapes. For example, monodisperse monosols can be generated as needed and used for testing.
  • particles were used as the basis of a spherical shape, their chemical properties, represented by the refractive index ⁇ slightly differ.
  • the same applies to the comparison particle with m 3 l, 3 + 0.01i, the imaginary part of which deviates by the same amount.
  • the comparison particle to the refractive index m 3 differs so significantly with its characteristic behavior of Sn compared to the reference particle that the decision base is not only in the structure but also in the intensity, which is plotted here in arbitrary units.
  • FIG. 3 shows in a corresponding manner in comparison to FIG. 2 an analysis of the Müller matrix element S 34 .
  • the Muller matrix parameter Sn or S 34 could already be sufficient to distinguish very similar particle types from one another.
  • the invention relates to an analysis method for determining at least one element S of a Müller matrix of a sample 4,5 with biological particles, wherein a light beam 6 is scattered by the sample 5.

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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Dispersion Chemistry (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

L'invention concerne une méthode d'analyse permettant de déterminer au moins un élément S d'une matrice de Mueller d'un échantillon (4, 5) contenant des bioparticules grâce à la dispersion d'un faisceau lumineux (6) par l'échantillon (5). Selon l'invention, pour augmenter la précision, en particulier l'identification de particules qui se ressemblent, on effectue également, en complément de l'expérience de dispersion, une analyse par spectroscopie de résonance en mesurant au moins une résonance optique ou plusieurs résonances optiques selon un premier angle solide de dispersion ϑ. L'invention concerne en outre un système permettant de mettre en œuvre la méthode d'analyse.
PCT/EP2014/067726 2013-08-28 2014-08-20 Méthode d'analyse pour déterminer les types et les concentrations de bioparticules Ceased WO2015028365A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE201310217157 DE102013217157A1 (de) 2013-08-28 2013-08-28 Analyseverfahren zur Ermittlung der Typen und Konzentrationen biologischer Partikel
DE102013217157.9 2013-08-28

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WO2015028365A1 true WO2015028365A1 (fr) 2015-03-05

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113176185A (zh) * 2021-04-23 2021-07-27 长春理工大学 一种烟雾粒子穆勒矩阵的偏振测量系统

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US10502700B2 (en) 2016-07-12 2019-12-10 United States Gypsum Company Methods for analyzing respirable particles in bulk materials
CN112924421A (zh) * 2021-01-28 2021-06-08 重庆邮电大学 一种核酸适配体传感器的共振光散射检测分析方法及检测装置

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US4884886A (en) * 1985-02-08 1989-12-05 The United States Of America As Represented By The Department Of Energy Biological particle identification apparatus
US6060710A (en) * 1998-12-21 2000-05-09 The United States Of America As Represented By The Secretary Of The Army Infrared Mueller matrix detection and ranging system
WO2002025247A2 (fr) * 2000-09-20 2002-03-28 Menguc M Pinar Procede et appareil non intrusifs permettant de caracteriser des particules par diffusion d'elements matriciels au moyen d'une radiation polarisee elliptiquement
DE60308864T2 (de) 2003-09-12 2007-05-24 Bruker Biospin Gmbh Verfahren der Resonanz-Spektroskopie für die Analyse von statistischen Eigenschaften von Proben
WO2007120181A2 (fr) * 2005-10-03 2007-10-25 Henry M. Jackson Foundation For The Advancement Of Military Medicine, Inc. Procédé et appareil permettant de mesurer des paramètres de la matrice de mueller relatifs à la diffusion d'une lumière polarisée

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US6060710A (en) * 1998-12-21 2000-05-09 The United States Of America As Represented By The Secretary Of The Army Infrared Mueller matrix detection and ranging system
WO2002025247A2 (fr) * 2000-09-20 2002-03-28 Menguc M Pinar Procede et appareil non intrusifs permettant de caracteriser des particules par diffusion d'elements matriciels au moyen d'une radiation polarisee elliptiquement
DE60308864T2 (de) 2003-09-12 2007-05-24 Bruker Biospin Gmbh Verfahren der Resonanz-Spektroskopie für die Analyse von statistischen Eigenschaften von Proben
WO2007120181A2 (fr) * 2005-10-03 2007-10-25 Henry M. Jackson Foundation For The Advancement Of Military Medicine, Inc. Procédé et appareil permettant de mesurer des paramètres de la matrice de mueller relatifs à la diffusion d'une lumière polarisée

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113176185A (zh) * 2021-04-23 2021-07-27 长春理工大学 一种烟雾粒子穆勒矩阵的偏振测量系统
CN113176185B (zh) * 2021-04-23 2022-10-11 长春理工大学 一种烟雾粒子穆勒矩阵的偏振测量系统

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