EP1395821A2 - Procede et dispositif pour effectuer des analyses chromatographiques de fa on automatique et optimale - Google Patents

Procede et dispositif pour effectuer des analyses chromatographiques de fa on automatique et optimale

Info

Publication number
EP1395821A2
EP1395821A2 EP02758210A EP02758210A EP1395821A2 EP 1395821 A2 EP1395821 A2 EP 1395821A2 EP 02758210 A EP02758210 A EP 02758210A EP 02758210 A EP02758210 A EP 02758210A EP 1395821 A2 EP1395821 A2 EP 1395821A2
Authority
EP
European Patent Office
Prior art keywords
retention times
parameters
data
run
chromatography
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.)
Withdrawn
Application number
EP02758210A
Other languages
German (de)
English (en)
Inventor
Sergey Golushko
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.)
VWR International BVBA
Original Assignee
Merck Patent 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 Merck Patent GmbH filed Critical Merck Patent GmbH
Publication of EP1395821A2 publication Critical patent/EP1395821A2/fr
Withdrawn legal-status Critical Current

Links

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
    • G01N30/8693—Models, e.g. prediction of retention times, method development and validation
    • 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
    • G01N30/8658—Optimising operation parameters
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T436/00—Chemistry: analytical and immunological testing
    • Y10T436/11—Automated chemical analysis

Definitions

  • the present invention relates to a method and a device for automatically carrying out and optimizing chromatographic examinations with the aid of an electronic data processing device, the method comprising the steps
  • the corresponding device has a chromatographic column or separation column, an inlet chamber for the mixture of substances, an eluent supply, a measuring unit at the exit of the chromatography column, and a data acquisition unit for the automatic and / or manual input of data.
  • the known systems work reliably and quickly if the analytes, that is to say the individual components of the mixture of substances, are sufficiently known. If, for example, it is important to confirm a concrete composition of a mixture of substances, such as a medicament, and / or to rule out that, for example, a certain undesired by-product, which can easily arise in the manufacturing process, is contained in the mixture, one can standardize on this Set certain chromatography conditions based on empirical values and at least partially let them run automatically. Since the components sought, as well as any undesired components, are known, the individual bands can be clearly assigned to the components on the basis of the chromatogram, which was created on the basis of corresponding empirical values.
  • the concentration of the organic modifier is selected in many cases. varies during the chromatography run (so-called gradient chromatography). This generally begins with a low concentration of the organic modifier, which, for example, is increased continuously until the end of the chromatography run. However, it is often advisable not to leave the concentration gradient constant, but to vary it more strongly, and for example to change the concentration step by step or to change it continuously only for a limited time, and otherwise to proceed at constant concentrations.
  • step iv) performing at least one further chromatography run with the parameters of the retention times optimized according to step iii) and comparison of the actual retention times with the theoretically calculated, optimized retention times,
  • a second test run with a second concentration of the organic modifier is preferably carried out. At least some bands usually appear in the respective chromatogram at both concentrations.
  • the process runs completely automatically and the corresponding device is designed for such an automatic process sequence, that is to say that in addition to the basic components of a chromatography column with an inlet chamber the mixture of substances, an eluent supply and the measuring unit at the exit of the chromatography column, a data acquisition device for the automatic and / or manual entry of data, an associated optimization unit, which, based on the last recorded data of a system, optimizes parameters for a (further) chromatography run calculated and a control device and parameter sensors, which are provided to automatically set the parameters determined in the optimization unit and the parameters according to the automatically determined process flow to control.
  • the number of peaks or bands of the chromatogram measured overall is also recorded.
  • the parameters are only changed to the extent that the number of peaks recorded does not decrease as a result. This also imposes considerable restrictions on the available parameter space and thus a significant acceleration of the optimization.
  • the optimization times for the second column material and / or the second eluent can likewise be shortened considerably. It is therefore expedient for such transitions to other chromatography columns or other eluents to take place initially only theoretically on the basis of the model mentioned, and a switchover is preferably only carried out if the optimizations carried out on this theoretical basis show a significant improvement compared to the chromatography columns or eluents initially used promise.
  • the parameters that is to say the concentration of the organic modifier as a function of time or the temperature, are set automatically in the various chromatography runs which may have to be carried out in the course of the optimization. A user therefore only needs to monitor the system or a corresponding chromatography system at certain time intervals, the stored data expediently being recorded in the form of logs and being displayed on a screen or also on another display medium.

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)
  • Treatment Of Liquids With Adsorbents In General (AREA)

Abstract

La présente invention concerne un procédé pour effectuer de façon automatique des analyses chromatographiques à l'aide d'un dispositif électronique de traitement de données. Ce procédé consiste à i) acquérir des données comprenant au moins une des informations suivantes : a) temps de rétention d'au moins un composant du mélange de substances, de préférence pour au moins deux concentrations différentes d'un modificateur organique, b) température à laquelle les temps de rétention ont été déterminés, c) formules développées d'un ou de plusieurs des composants du mélange de substances, d) type d'agent d'élution et concentration d'un modificateur organique dans celui-ci, e) paramètres ou type de la colonne de séparation. L'objectif de l'invention est de mettre au point un procédé et un dispositif d'analyse chromatographique nécessitant un nombre limité de personnes tout en garantissant une acquisition complète, en un temps relativement réduit, de la totalité ou de la majeure partie des composants du mélange de substances. A cet effet, les données acquises peuvent être, en totalité ou en partie, également transférées et/ou complétées à partir d'un dispositif de stockage de données et, si les données ne sont pas disponibles pour les informations selon a), b) ou c), au moins un premier cycle d'essai est effectué dans des conditions isocratiques pour acquérir des temps de rétention selon a) et, de préférence, un autre cycle d'essai isocratique est effectué avec une autre concentration du modificateur organique. Le procédé consiste ensuite à ii) évaluer des temps de rétention en fonction de paramètres d'optimisation sur la base d'un modèle reproduisant une relation fonctionnelle d'au moins une partie des données acquises lors de l'étape i), les données acquises étant reproductibles par réglage de paramètres de modèle, iii) optimiser les temps de rétention dans le modèle par modification des paramètres d'optimisation, iv) réaliser au moins un autre cycle de chromatographie avec les paramètres des temps de rétention optimisés conformément à l'étape iii) et comparer les temps de rétention réels avec les temps de rétention optimisés et évalués de façon théorique, v) éventuellement répéter une ou plusieurs fois les étapes i) à iv) si les écarts entre les temps de rétention évalués et les temps de rétention mesurés dépassent une valeur limite prédéterminée ou si les différences entre les temps de rétention de deux cycles de chromatographie successifs sont inférieures à une valeur limite prédéterminée, la décision de paramètres à régler concrètement pour un cycle suivant étant prise de préférence par un module d'intelligence artificielle.
EP02758210A 2001-06-13 2002-05-31 Procede et dispositif pour effectuer des analyses chromatographiques de fa on automatique et optimale Withdrawn EP1395821A2 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE10128546A DE10128546A1 (de) 2001-06-13 2001-06-13 Verfahren und Vorrichtung zur automatischen, optimierten Durchführung chromatographischer Analysen
DE10128546 2001-06-13
PCT/EP2002/006014 WO2002101384A2 (fr) 2001-06-13 2002-05-31 Procede et dispositif pour effectuer des analyses chromatographiques de façon automatique et optimale

Publications (1)

Publication Number Publication Date
EP1395821A2 true EP1395821A2 (fr) 2004-03-10

Family

ID=7688076

Family Applications (1)

Application Number Title Priority Date Filing Date
EP02758210A Withdrawn EP1395821A2 (fr) 2001-06-13 2002-05-31 Procede et dispositif pour effectuer des analyses chromatographiques de fa on automatique et optimale

Country Status (6)

Country Link
US (1) US7216039B2 (fr)
EP (1) EP1395821A2 (fr)
JP (1) JP2004529369A (fr)
AU (1) AU2002325224A1 (fr)
DE (1) DE10128546A1 (fr)
WO (1) WO2002101384A2 (fr)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10345958A1 (de) 2003-10-02 2005-04-21 Magna Steyr Fahrzeugtechnik Ag Mobiler Tank für kryogene Flüssigkeiten
US9424398B1 (en) * 2009-01-24 2016-08-23 Dionex Corporation Workflows for defining a sequence for an analytical instrument
US8631057B2 (en) * 2009-08-25 2014-01-14 International Business Machines Corporation Alignment of multiple liquid chromatography-mass spectrometry runs
US20120166098A1 (en) * 2010-01-26 2012-06-28 Mccreary Dennis Methods for Optimizing Gradients in Liquid Chromatography Systems
US8716025B2 (en) * 2011-07-08 2014-05-06 Agilent Technologies, Inc. Drifting two-dimensional separation with adaption of second dimension gradient to actual first dimension condition
CN102879508B (zh) * 2011-07-15 2014-12-03 株式会社岛津制作所 用于液相色谱仪的控制设备
US11835501B2 (en) 2015-07-13 2023-12-05 Sartorius Stedim Chromatography Systems Ltd. Optimizing operating binding capacity for a multiple column chromatography process
CN108875284B (zh) * 2018-08-13 2022-07-19 辽宁大学 一种基于随机扩散理论的气相色谱分离仿真方法
DE102019111782A1 (de) * 2019-05-07 2020-11-12 Dionex Softron Gmbh Leistungsüberwachung eines Analysesystems
DE102019111783A1 (de) * 2019-05-07 2020-11-12 Dionex Softron Gmbh Verfahren, System und Verwendung zur Änderung eines Analysevorgangs
JP7131699B2 (ja) * 2019-05-08 2022-09-06 株式会社島津製作所 質量分析装置及び質量分析方法
GB2593686B (en) * 2020-03-30 2022-12-21 Agilent Technologies Inc Adjusting separation method using sensor data and numerical analysis
CN115933803B (zh) * 2023-01-09 2023-06-13 江苏东成工具科技有限公司 一种设备控制方法、设备及计算机可读介质

Family Cites Families (6)

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JP2800509B2 (ja) * 1990-11-30 1998-09-21 株式会社日立製作所 液体クロマトグラフ装置
US5305232A (en) * 1992-05-13 1994-04-19 The University Of Rochester Chromatography system
IT1277749B1 (it) 1995-12-29 1997-11-12 Fisons Instr Spa Dispositivo e metodo per effettuare la separazione di un campione in singoli componenti in un condotto capillare di un apparecchio per la
DE19860354B4 (de) 1998-12-24 2006-11-23 Universität Dortmund Eine Methode zur modellbasierten on-line Optimierung und Parameterschätzung von Batch-Chromatographieprozessen
US20020010566A1 (en) * 2000-04-11 2002-01-24 Chester Thomas Lee Methods for modeling, predicting, and optimizing high performance liquid chromatography parameters
DE10049079A1 (de) 2000-10-02 2002-04-18 Merck Patent Gmbh Verfahren und System zur Methodenoptimierung in der Chromatographie

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO02101384A2 *

Also Published As

Publication number Publication date
DE10128546A1 (de) 2002-12-19
AU2002325224A1 (en) 2002-12-23
US7216039B2 (en) 2007-05-08
JP2004529369A (ja) 2004-09-24
US20040253147A1 (en) 2004-12-16
WO2002101384A2 (fr) 2002-12-19
WO2002101384A3 (fr) 2003-09-12

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