ChromSword® publications
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Rapid Method for the Optimization of Separation
Conditions on Mixed-Mode Stationary Phases Using
Automated Method Development SoftwareRomain Dabr, Achim Schwämmle,Merck KGaA, Darmstadt, Germany Adeline René, ENSICAEN, Caen, France Michael Lämmerhofer, Wolfgang Lindner, Institute of Analytical Chemistry and Food Chemistry, Vienna, Austri Poster Presentation MDA06_th, HPLC 2009, Dresden, Germany Silica-based mixed-mode chromatography materials developed in our laboratories combine both reversed phase (RP) and weak anion exchange (WAX) characteristics, which offers a wide range of applicability for the separation of neutral, acidic, basic, or amphoteric compounds. Chromatographic runs can be performed in many different interaction modes such as reversed phase, hydrophilic and hydrophobic interaction, ion exclusion, ion exchange, or a combination of several of those modes. Due to this high flexibility in usage it could be difficult and time consuming especially for less experienced users to identify the appropriate separation mode and to optimize the chromatographic conditions on such columns.As a case study for such method development, we optimized the separation of three fluoroquinolone-based antibiotics containing both acidic and basic functionalities –ciprofloxacin, danofloxacin and norfloxacin– as well as the separation of norfloxacin from the three main impurities described in the European Pharmacopoeia. Quantitation of Trace Betamethasone or Dexamethasone in Dexamethasone or Betamethasone Active Pharmaceutical Ingredients by Reversed-Phase High-Performance Liquid Chromatography Kang Ping Xiaoa, Yuan Xionga, and Abu M. Rustum Schering-Plough Corporation, Global Quality Services – Analytical Sciences, Union, NJ 07083, USA Journal of Chromatographic Science, ISSN 0021-9665 Volume 46, Number 1, January 2008, pp. 15-22 |
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Efficient
method development
strategy for challenging separation of
pharmaceutical molecules using advanced
chromatographic technologies
Kang Ping Xiaoa, Yuan Xionga, Fang Zhu Liua and Abu M. Rustum Schering-Plough Corporation, Global Quality Services – Analytical Sciences, Union, NJ 07083, USA Journal of Chromatography A, June 2007, pp. 145-156 In this paper, we describe a strategy that can be used to efficiently develop a high-performance liquid chromatography (HPLC) separation of challenging pharmaceutical molecules. This strategy involves use of advanced chromatographic technologies, such as a computer-assisted chromatographic method development tool (ChromSword) and an automated column switching system (LC Spiderling). This process significantly enhances the probability of achieving adequate separations and can be a large time saver for bench analytical scientists. In our study, the ChromSword was used for mobile phase screening and separation optimization, and the LC Spiderling was used to identify the most appropriate HPLC columns. For proof of concept, the analytes employed in this study are the structural epimers betamethylepoxide and alphamethylepoxide (also known as 16-beta methyl epoxide and 16-alpha methyl epoxide). Both of these compounds are used in the synthesis of various active pharmaceutical ingredients that are part of the steroid pharmaceutical products. While these molecules are relatively large in size and contain various polar functional groups and non-polar cyclic carbon chains, their structures differ only in the orientation of one methyl group. To our knowledge, there is no reported HPLC separation of these two molecules. A simple gradient method was quickly developed on a 5 cm YMC Hydrosphere C18 column that separated betamethylepoxide and alphamethylepoxide in 10 min with a resolution factor of 3.0. This high resolution provided a true baseline separation even when the concentration ratio between these two epimers was 10,000:1. Although outside of the scope of this paper, stability-indicating assay and impurity profile methods for betamethylepoxide and for alphamethylepoxide have also been developed by our group based on a similar method development strategy.
Michael
Pfeffer, Bayer Schering Pharma, Berlin, Germany,
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Elizabeth F. Hewitt , Noramco, Inc., Chemical Services, 1440 Olympic Drive, Athens, GA 30601, USA Patrick Lukulay, Pfizer Global Research and Development, Michigan Pharmaceutical Sciences, 2800 Plymouth Road, Ann Arbor, MI 48105, USA Sergey Galushko, Galushko Software Entwicklung, Im Wiesengrund 49-b, Muehtal 64367, Germany Journal of Chromatography A , Volume 1107, Issues 1-2 , 24 February 2006, Pages 79-87 A comprehensive, fully automated strategy is demonstrated for HPLC-UV chromatographic method development using ChromSword® optimization software. The strategy involves: (1) the automated screening of various column and mobile phase combinations, (2) rational selection of the best starting conditions; and (3) subsequent automated method development to generate optimized separation methods. Pharmaceutical compounds were applied to solve problematic drug impurity separations. ChromSword® software automates the screening, optimization, and documentation steps thus reducing the method development time. The strategy was compared to a manual method development approach showing the automated method strategy affords better selectivity in a shorter time. |
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ChromSword®
Software for Automated and Computer-Assisted Development of HPLC Methods S. Galushko, V. Tanchuk, I. Shishkina, O. Pylypchenko, and W. D. Beinert HPLC Made to Measure: A Practical Handbook for Optimization. Edited by Stavros Kromidas Copyright © 2006 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim ISBN: 3-527-31377-X Chapter 4.2, page 557-570 ChromSword®-Software
für die automatische und Computer-unterstützte HPLC-Methodenentwicklung S. Galushko, V. Tanchuk, I. Shishkina, O. Pylypchenko und W. D. Beinert HPLC richtig optimiert: Ein Handbuch für Praktiker. Herausgegeben von Stavros Kromidas Copyright © 2006 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim ISBN: 3-527-31470-9 Kapitel 4.2, Seiten 583-598 |
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Automating
the validation of chromatographic methods using
the novel tools AUTOVAL and ChromSword
AutoRobust M. Pfeffer, R. Golejewski, N. Harwardt, H. Windt, B. Wykhoff, Schering, Global Chemical Development - In-Process Control, DE-13342 Berlin, Germany Analytica 2006 For checking the ruggedness of HPLC methods ChromSword®AutoRobust, a novel software tool can be used. For a common HPLC methods, it can be tested whether the analytical results are influenced by small changes in chromatographic variables, e.g. column temperature, flow rate, injection volume, concentration of an organic modifier, gradient slopes and break point positions, column batches (up to 6), equilibration time, buffer pH or concentration (up to 12) and stability in solution as well as the absorption wavelength in combination with a PDA. The aim was to get a simple tool for preparing methods for slight systematic changes in chromatographic parameters. Phenolcarbonsaeuren
und Flavonoide in HonigHPLC-Methodenentwicklung mit ChromSword® AUTO S. Trautvetter, I. Koelling-Speer, K. Speer Technische Universitaet Dresden Institut fuer Lebensmittelchemie, D-01062 Dresden, Germany Deutscher Lebenmittelchemikertag 2006, Dresden, Germany Mit der Software ChromSword® AUTO war es moeglich eine HPLC-Trennmethode fuer 35 Phenolcarbonsaeuren und Flavonoide zu entwickeln. Trotz der strukturellen Aehnlichkeiten zahlreicher Verbindungen, die insbesondere im mittleren Bereich des urspruenglichen Chromatogramms zu Ueberlagerungen fuehrten, konnte durch die gleichzeitige Optimierung von Gradient und Temperatur eine bereits vorab optimierte Trennung erzielt und somit Loesungsmittel und Zeit eingespart werden. Durch zusaetzlich vorgenommene manuelle Veraenderungen am Gradienten konnte die Trennung anschliessend noch verfeinert werden. |
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automatic HPLC method development for complex
mixtures with ChromSword Auto
Sergey Galushko, Galushko Software Entwicklung, Im Wiesengrund 49-b, Muehtal 64367, Germany Ahmed Aced  ,IRIS
Technologies International, Ltd., 3 Manse Brae,Longridge, EH47 8NZ, West-Lothian, UK LCGC Europe, 02DEC06 The chromatographic separation of unknown sample mixtures can be challenging for the HPLC method developer if impurities or degradation products are present in the sample. Peaks of these compounds must be resolved from the peaks of interest, thereby increasing the complexity of the method development. ChromSwordAuto method development software integrated with HPLC instruments enables a rapid and unattended separation of complex mixtures. Analysis
of advanced liquid crystals using method
development tools and modern separation
materialsB. Meyer, Merck KGaA, 64293 Darmstadt, Germany Poster Presentation, HPLC2005 To perform automated method development the solution of the single substances (Boronic Acid, Phenyl Bromide, reaction product) as well as the mixture of all three compound were placed in the autosampler and CHROMSWORD AUTO is started. We normally run the method development during night. CHROMSWORD AUTO starts a series of injection of the single compound determining their separation characteristics on the column material used. It predicts a theoretical retention model for each component. Using the retention model simulated chromatograms can be obtained. The corresponding “real” chromatogram of the mixture is shown. The automated method development process was completed after 280 minutes. The time for manual method development would have been 2-3 working days. |
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Automated
HPLC method development: A step forward
with innovative software technology Wolf-Dieter Beinert, Volker Eckert, Sergej Galushko, Vsevolod Tanchuk and Irina Shishkina, LC GC Europe Supplement, p 34 Existing HPLC method development software has been added to and combined with an HPLC system to perform method optimizations automatically. The additional software modules and the optimization process, based on the theory of reversed-phase chromatography or on an empirical approach, are explained. Test and real application examples demonstrate the systems ability to rapidly optimize chromatographic conditions for reversed-phase separations. A column and solvent switching function enables selection of the most suitable column/organic modifier combination. High-quality separation methods with maximum resolution over minimum run times result. |
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method development using Agilent 1100 Series
HPLC systems, Agilent ChemStation and ChromSword®
software Sergey Galushko, Ralf Honsberg Angelika Gratzfeld-Huesgen, Bernd Hoffmann Agilent Technologies Application, Publication number 5988-8927EN, Published March 1, 2003 The development of an HPLC method is invariably a repetitive and time-consuming process of method planning, development, execution and interpretation. Analysts are often forced to spend a good portion of their effort on these routine tasks rather than concentrating on more valuable work in the laboratory. Today, many tools are available to help automate the method development process. This Application Note demonstrates the use of ChromSword Auto software with Agilent 1100 Series HPLC systems and Agilent ChemStation software. |
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Hitachi LaChrom Elite
HPLC and fast LC pharmaceutical applications:
OTC analgesics & steroids
John K. Lim, Michael C. Riley, Stephen T. Watts Hitachi High Technologies America LCGC North America, February 2003 Routine development of multi-component "Fast Liquid Chromatograhy" (Fast LC) applications are rapidly and easily accomplished by integrating (a) the new Hitachi LaChrom® Elite HPLC system, (b) Automated Method Development Tool (ChromSword Auto), and (c) Hitchi Chromolith™ monolithic reversed-phase columns. The fast LC applications allow for high throughput analysis leading to a significant reduction in run times contrasted to conventional C18 particulate column run times by several-fold. Examples presented herein demonstrate an integrated approach to fast LC applications development of Over-the-Counter (OTC) analgesics and steroids. The
Hitachi LaChrom Elite HPLC Automated Method
Devlopment System: Polar Reversed Phase
SeparationsJohn K. Lim, Hitachi High Technologies America LCGC North America, September 2003 Traditional HPLC method development involves highly skillful, experienced, knowledgeable, and intuitive operators to generate efficient separation methods. This is often a time-consuming endeavor that does not always produce the best possible separation results, in spite of the best efforts. Automated method development (AMD) with the Hitachi LaChrom® Elite (LCE) HPLC system in conjunction with ChromSword Auto (CSA) provides a unique AMD system that will separate multi-component systems effortlessly, accurately, and with significant savings in both time and cost for the method development. Un logiciel de développement assisté par ordinateur en chromatographie liquide haute performance C. Delaurent Institut Méditerranéen de la recherche en nutrition C. Brenier-Maurel Laboratoire de Chimie appliquée UMR 6516 Faculté des Sciences et Techniques de St. Jérôme 13397 Marseille Cedex 20 - France S.V. Galushko, V. Tanchuk, L. Shishkina, O. Pylypchenko Galushko Software Entwicklung, Am Wiesengrund 49B, 64367 Muehltal -Germany Techniques Instrumetales Spectra Analyse, Vol. 21, No. 224, Janvier-Fevrier 2002 Le développement de méthodes de séparation est l'objectif le plus important, mais aussi le plus difficile à atteindre en Chromatographie Liquide haute Performance (CLHP). L'utilisation de programmes informatiques spécialisés peut aider l'analyste à mener à bien cette tache. De tels programmes permettent en effet, de piloter <intelligemment> une chaine de CHLP dans le cadre du développement de méthodes séparatives, et en ce mode automatique. Les paragraphes qui suivent sont consacrés a l' utilisation du logiciel ChromSword® pour la mise au point et le développement de méthodes en CLHP. Ce logiciel est capable de fonctionner automatiquement, comme un assistant virtuel, pour gérer en mode continu le procédé de développement de méthodes. Il peut également fonctionner en mode discontinu comme un expert impartial dans le cadre de l'optimisation de méthodes en CHLP. 
Press Release:
Agilent and IRIS are co-marketing ChromSword® Auto with Agilent HPLC and ChemStation solutions in the U.S. and Canada |
