WO2018196958A1 - Procédé et dispositif pour étalonner une analyse chromatographique de mélanges gazeux complexes, en particulier de gaz respirables - Google Patents

Procédé et dispositif pour étalonner une analyse chromatographique de mélanges gazeux complexes, en particulier de gaz respirables Download PDF

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Publication number
WO2018196958A1
WO2018196958A1 PCT/EP2017/059784 EP2017059784W WO2018196958A1 WO 2018196958 A1 WO2018196958 A1 WO 2018196958A1 EP 2017059784 W EP2017059784 W EP 2017059784W WO 2018196958 A1 WO2018196958 A1 WO 2018196958A1
Authority
WO
WIPO (PCT)
Prior art keywords
calibration
substance
substances
chromatographic analysis
retention time
Prior art date
Application number
PCT/EP2017/059784
Other languages
German (de)
English (en)
Inventor
Maximilian Fleischer
Alexander Michael Gigler
Original Assignee
Siemens Aktiengesellschaft
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 Aktiengesellschaft filed Critical Siemens Aktiengesellschaft
Priority to PCT/EP2017/059784 priority Critical patent/WO2018196958A1/fr
Publication of WO2018196958A1 publication Critical patent/WO2018196958A1/fr

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/86—Signal analysis
    • G01N30/8665—Signal analysis for calibrating the measuring apparatus
    • G01N30/8668—Signal analysis for calibrating the measuring apparatus using retention times
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
    • G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
    • G01N2030/8813—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample biological materials

Definitions

  • This invention relates to a method for calibrating a chromatographic analysis according to the preamble of claim 1 and to an arrangement for calibrating a
  • mobile phase is meant the phase in which a mixture of substances (sample) is introduced and moved at the beginning of the separation system (column), which is introduced into a carrier medium or the filling of the columns, while the stationary phase is characterized by a phase which enters with differing ⁇ dangerous ingredients of the substance mixture interactions and does not move.
  • the stationary phase consists of a liquid (also called “spacer fluid”) or gel with which the mecanicsei ⁇ te the running columns, particularly in the case of the embodiment as a capillary coated.
  • spacer fluid also called "spacer fluid”
  • gel with which the mecanicsei ⁇ te the running columns, particularly in the case of the embodiment as a capillary coated.
  • Retention is understood as the delayed flow of individual substances of the substance mixture of the mobile phase by interaction with the stationary phase.
  • Trä ⁇ germedium liquid or gas
  • these are high-purity substances (eg argon as the carrier gas in the GC).
  • the object underlying the invention is to provide a solution which improves the known from the prior art solutions, in particular ensures an application in the medical field.
  • a first retention time of at least one calibration substance is determined during the chromatographic analysis of a sample, wherein the calibration is performed on the basis of an evaluation of the first retention time.
  • the invention further relates to an arrangement for calibrating a chromatographic analysis of complex mixtures of substances, in particular breathing gases, characterized by means for carrying out the method and means for
  • the inventive method is such wei ⁇ ned, and that the calibration substance is mixed with the carrier medium of the chromatographic analysis and / or the sample.
  • the method according to the invention is further developed in such a way that the calibration substance to be admixed is configured according to an assignment to the type of the samples to be examined and / or the chromatography system such that the same calibration substance is always added to the analysis site.
  • the method according to the invention is developed in such a way that a substance is admixed as the calibration substance to substances produced in the human organism and substances produced by metabolic activities, in particular by molecules have non-producible functional groups in the human organism, is disjoint. As a result, an influence of the calibration substance on the sample can be minimized.
  • a calibration substance is designed and admixed in dependence on the type of the samples to be examined and / or the chromatography system such that a first retention time of the calibration sub-dance is disjunctive to respectively second retention times of substances of a sample.
  • This facilitates a differentiation of the two substances, so that the correct retention time can be used for the evaluation for the subsequent calibration.
  • This can be further improved when the fiction, ⁇ modern method is further formed such that the Calib ⁇ r istssubstanz is configured and mixed, that the first retention time significantly, so in he ⁇ considerably recognizable manner differs from the second retention times.
  • the method according to the invention thus uses the Verwen ⁇ tion of a mixture, for example from the classical
  • Purest carrier medium such as helium or argon
  • a precisely known and according to the invention so ausgestalte ⁇ th and admixed calibration substance, which differs from occurring in the samples to be examined substances provided.
  • the retention time can be recorded "online", ie during the sample measurement itself
  • Calibration substances to be chosen or designed so that they differ significantly in their retention time of the retention times of the substances in the samples.
  • the invention provides that the mixture can generally be selected specifically for each experimental design, as well as by the choice of the column and the configuration of the chromatographic system, for example as e.g. GC as GC MS (Mass Spectrometer), GC FTIR (Fourier Transform Infrared Spectrometer), GC MS MS, etc. is currently the case.
  • GC mass Spectrometer
  • GC FTIR Fastier Transform Infrared Spectrometer
  • GC MS MS etc.
  • FIGURE shows a flow chart with a simplified representation of an embodiment of the Ver ⁇ method
  • These may be molecules carrying functional groups which can not be produced by the human organism (and also not by disease) and also, at least typically, can not be delivered by administration, for example, intravenously or orally, etc.
  • isotope-labeled molecules so that the distinction between human and non-human origin can be distinguished.
  • a step S2 the admixture of the calibration substance then takes place in the carrier medium of the GC.
  • a third step S3 which is usually the injection of the sample, that is, their compounds, and their chromatographic analysis jointly associated with calibration ⁇ approximately substance.
  • a fourth step S4 of the determined retention times of the calibration substance and of the sample substances the retention time of the calibration substance was used for the calibration and evaluated.
  • a correction of the retention time axis will then optionally take place as a function of the evaluation, so that in a sixth step S6 an adaptation of the sample data to this corrected retention time axis can take place.
  • the invention is not be limited to the example described ⁇ , so at this point are some characteristic features and advantages of the invention and its developments as

Landscapes

  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analysing Biological Materials (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

La présente invention concerne un procédé pour étalonner une analyse chromatographique de mélanges gazeux complexes, en particulier de gaz respirables, dans lequel on détermine un premier temps de rétention d'au moins une substance d'étalonnage pendant l'analyse chromatographique d'un échantillon, l'étalonnage étant réalisé à partir d'une évaluation du premier temps de rétention. L'invention concerne par ailleurs un dispositif comprenant des moyens pour la mise en œuvre du procédé.
PCT/EP2017/059784 2017-04-25 2017-04-25 Procédé et dispositif pour étalonner une analyse chromatographique de mélanges gazeux complexes, en particulier de gaz respirables WO2018196958A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PCT/EP2017/059784 WO2018196958A1 (fr) 2017-04-25 2017-04-25 Procédé et dispositif pour étalonner une analyse chromatographique de mélanges gazeux complexes, en particulier de gaz respirables

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/EP2017/059784 WO2018196958A1 (fr) 2017-04-25 2017-04-25 Procédé et dispositif pour étalonner une analyse chromatographique de mélanges gazeux complexes, en particulier de gaz respirables

Publications (1)

Publication Number Publication Date
WO2018196958A1 true WO2018196958A1 (fr) 2018-11-01

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP2017/059784 WO2018196958A1 (fr) 2017-04-25 2017-04-25 Procédé et dispositif pour étalonner une analyse chromatographique de mélanges gazeux complexes, en particulier de gaz respirables

Country Status (1)

Country Link
WO (1) WO2018196958A1 (fr)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2001055714A1 (fr) * 2000-01-25 2001-08-02 The State Of Oregon Acting By And Through The State Board Of Higher Education On Behalf Of Portland State University Procede et appareil de concentration d'echantillons a analyser
WO2006110848A2 (fr) * 2005-04-11 2006-10-19 Cerno Bioscience Llc Analyse de donnees chromatographiques et de spectre de masse
US20090039250A1 (en) * 2007-08-06 2009-02-12 Hitachi Ltd. Mass spectrometer and method of mass spectrometry
US20140260509A1 (en) * 2013-03-15 2014-09-18 Christopher A. Pohl Method of calibrating a chromatography system
EP2998736A1 (fr) * 2014-09-18 2016-03-23 Dionex Corporation Procédé automatisé d'étalonnage d'un système de chromatographie et d'analyse d'un échantillon

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2001055714A1 (fr) * 2000-01-25 2001-08-02 The State Of Oregon Acting By And Through The State Board Of Higher Education On Behalf Of Portland State University Procede et appareil de concentration d'echantillons a analyser
WO2006110848A2 (fr) * 2005-04-11 2006-10-19 Cerno Bioscience Llc Analyse de donnees chromatographiques et de spectre de masse
US20090039250A1 (en) * 2007-08-06 2009-02-12 Hitachi Ltd. Mass spectrometer and method of mass spectrometry
US20140260509A1 (en) * 2013-03-15 2014-09-18 Christopher A. Pohl Method of calibrating a chromatography system
EP2998736A1 (fr) * 2014-09-18 2016-03-23 Dionex Corporation Procédé automatisé d'étalonnage d'un système de chromatographie et d'analyse d'un échantillon

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