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Elke Hahn-DeinstropApplied Thin-LayerChromatography18072007 Knowledge for GenerationsEach generation has its unique needs and aspirations.When Charles Wiley firstopened his small printing shop in lower Manhattan in 1807,it was a generation ofboundless potential searching for an identity.And we were there,helping to define anew American literary tradition.Over half a century later,in the midst of the SecondIndustrial Revolution,it was a generation focused on building the future.Once again,we were there,supplying the critical scientific,technical,and engineering knowledgethat helped frame the world.Throughout the 20th Century,and into the new millen-nium,nations began to reach out beyond their own borders and a new internationalcommunity was born.Wiley was there,expanding its operations around the world toenable a global exchange of ideas,opinions,and know-how.For 200 years,Wiley has been an integral part of each generations journey,en-abling the flow of information and understanding necessary to meet their needs andfulfill their aspirations.Today,bold new technologies are changing the way we live andlearn.Wiley will be there,providing you the must-have knowledge you need to imag-ine new worlds,new possibilities,and new opportunities.Generations come and go,but you can always count on Wiley to provide you theknowledge you need,when and where you need it!William J.PescePresident and Chief Executive OfficerPeter Booth WileyChairman of the BoardElke Hahn-DeinstropApplied Thin-LayerChromatographyBest Practice andAvoidance of MistakesSecond,Revised and Enlarged EditionTranslated by R.G.LeachElke Hahn-DeinstropKleingeschaidter Str.2390542 EckentalGermanyelke.hahndeinstroparcor.deAll books published by Wiley-VCH are carefullyproduced.Nevertheless,authors,editor,andpublisher do not warrant the information containedin these books,including this book,to be freeof errors.Readers are advised to keep in mind thatstatements,data,illustrations,procedural detailsor other items may inadvertently be inaccurate.Library of Congress Card No.:Applied forBritish Library Cataloging-in-Publication DataA catalogue record for this book is availablefrom the British LibraryBibliographic information published by theDeutsche NationalbibliothekDie Deutsche Nationalbibliothek lists thispublication in the Deutsche Nationalbibliografie;detailed bibliographic data are available in theInternet athttp:/dnb.d-nb.de.2007 WILEY-VCH Verlag GmbH&Co.KGaA,WeinheimAll rights reserved(including those of translationinto other languages).No part of this book may bereproduced in any form nor transmitted or trans-lated into machine language without writtenpermission from the publishers.Registered names,trademarks,etc.used in this book,even when notspecifically marked as such,are not to be consideredunprotected by law.TypesettingMitterweger&Partner,PlankstadtPrintingbetz-druck GmbH,DarmstadtBookbindingLitges&Dopf Buchbinderei GmbH,HeppenheimPrinted in the Federal Republic of GermanyPrinted on acid-free paperISBN:978-3-527-31553-6Preface to the Second English EditionIt has been almost seven years since the publication of the first English Edition of mybook on TLC.The following improvements in technology over the years have made itnecessary for me to update the first edition:new precoated layers for both existing andnew fields of applications,a new generation of equipment for safe operations and re-producible results,new devices such as the Diode Array Detector and Biolumines-cence Analyzer,new methods of interface between TLC and analysis methods,espe-cially the use of digital cameras for the documentation of thin layer chromatograms.For the readers benefit,I have updated my description of available products on themarket.I had a wealth of assistance and support,including many telephone exchangeswithin Germany to Hamburg,Berlin,Stuttgart,Darmstadt and Offenburg as well asthe exchanging of many files via e-mail to and from Muttenz(Switzerland)and Hous-ton(Texas,USA).During the last few years I held a series of lectures on chromatography and partookin TLC workshops at high schools and universities within Germany.In attending thoseevents,it was reinforced to me how important sound and comprehensive knowledge ofTLC is,in particular for recognizing and avoiding errors.If this book can contribute to confer my 40 years long enthusiasm for thin layerchromatography to the reader,then the energy expended was worthwhile and I takeleave in my retirement.Eckental,September 2006Elke Hahn-DeinstropPreface to the First English EditionShortly after the announcements in the scientific press in early 1998 of the publicationof the German edition of my book on TLC,I received many enquiries from outsideGermany asking when the English version would be available.The decision by Wiley-VCH to publish an English edition in 1999 was the start ofmany hectic months for me.To produce the present book,not only had the text,refer-ences and market overview to be updated,but also two more Sections describing newequipment had to be included.Documents 413 were revised and Tables 21a and 26were added.The Sections on video documentation were also extensively revised totake account of technical advances in this area.Numerousdiscussionsbytelephoneandfaxhavehelpedthetranslator,Mr.R.G.Leach,to import a flavor of my personal writing style into the English edi-tion.The main aim is to prevent fatigue and to inspire the reader to read on.Also,asa small“extra”,my ideas for two new cartoons have been excellently translated intoactual drawings by Norbert Barth.I dedicate the second of these new cartoons to Dr.Angelika Koch,with whom Ipublished several papers last year on the subject of the ancient remedy frankincense(olibanum),and who,in the course many conversations,gave me the strength to com-plete all the work for this book.I hope that all my friends and colleagues,in nearby Europe and also in distantJapan,China,India and Australia,and all other TLC users worldwide will derivepleasure from reading my book and will have great success in their work with TLC!Eckental,September 1999Elke Hahn-DeinstropPreface to the First German EditionDuring twenty-five years of practical experience with thin-layer chromatography(TLC),I have learned to appreciate the advantages of this method of analysis,espe-cially its power,flexibility and cost-effectiveness.The aim of this book is to pass on toa new generation of analysts any useful knowledge and practical tips that I have accu-mulated during this time.It includes some descriptions,illustrated by cartoons,ofamusing incidents in the everyday laboratory life of a second-year apprentice and atrainee pharmacist.I have already found these anecdotes to be useful teaching aids.If the cartoons seem to suggest that a new university graduate is likely to be lessknowledgeable about TLC than a young girl trained in an industrial laboratory,this isquite deliberate.However,I hope that established practitioners will also be able topick up some tips that may be useful in their everyday work.Formalism is nowadays unavoidable even in the field of TLC,and this book conse-quently contains a great many descriptions of practical procedures.The author hasnevertheless taken great care to describe these accurately and reliably and also to givecopious hints on how to avoid mistakes.The theme of TLC as an art form is also discussed in a short section in the Appen-dix.A writer starts the day with a blank sheet of paper and is happy with any prose orpoetry successfully written on it.In TLC we start with a white plate.If the chromato-grams we eventually obtain fulfill their intended purpose,we have had a successfulday.Eckental,October 1997Elke Hahn-DeinstropTothe Man by my SideContents1Introduction.11.1What Does TLC Mean?.11.2When Is TLC Used?.21.3Where Is TLC Used?.31.4How Is the Result of a TLC Represented?.41.4.1Retardation Factor.41.4.2Flow Constant.61.4.3Other TLC Parameters.71.5What Kinds of Reference Substances Are Used in TLC?.81.6The Literature on TLC.91.6.1General Literature.91.6.1.1Books and Information Sheets in German.91.6.1.2Books in English.111.6.1.3Book in Another Language.111.6.2Journals.121.6.2.1German Language Journals Containing Articles on TLC(Selection).121.6.2.2English Language Journals on TLC.121.6.2.3English Language Journals Containing General Articleson Chromatography(Selection).121.6.3Abstracts.131.6.4Pharmacopoeias.132Precoated Layers.152.1Precoated Layers Why?.152.2What Are Precoated Layers Produced?.162.2.1Sorbents.162.2.2Supports for Stationary Phases.192.2.3Additives.202.3What Types of Precoated Layers Are There?.212.4What Are the Uses of Precoated Layers?.27XIIContents2.5Criteria for the Selection of Stationary Phases in TLC.272.5.1How Can the Choice of the Stationary Phase be Made?.282.5.2How Can the Recommendations for Stationary PhasesFound in Pharmacopoeias be Applied to Precoated Layers?.282.6Effect of the Stationary Phase When Mobile Phases Are Identical.302.7Advice on the Ordering and Storage of Precoated Layers.312.8Problems in the Naming and Arrangement of Precoated Layers.333Before the TLC Development Process.353.1Handling of Precoated Layers.353.1.1Film and Foil.353.1.2Glass Plates.363.2Prewashing.413.3Activation.433.4Conditioning.443.5Impregnation.463.5.1Impregnation by Dipping.463.5.2Impregnation by Spraying.463.5.3Impregnation by Predevelopment.473.6Application of Samples.503.6.1Manual Application of Samples.513.6.2Semiautomatic Application.563.6.3Fully Automatic Application.613.7Positioning of the Samples.653.8Drying Before the Development.674Solvent Systems,Developing Chambers and Development.694.1Solvent Systems.694.1.1Choice of Solvent Systems.704.1.2Preparation and Storage of Solvent Systems.794.1.3Problematical Solvent System Compositions.824.2TLC Developing Chambers.874.2.1What Types of TLC Developing Chambers Are There?.874.2.1.1TLC Chambers for Vertical Development.884.2.1.2TLC Developing Chambers for Horizontal Development.904.2.2Influence of the Chamber Atmosphere.914.2.2.1The Unsaturated N-Chamber.934.2.2.2The Saturated N-Chamber.94XIIIContents4.2.3Influence of Temperature in Chromatography.974.2.4Location and Labeling of TLC Developing Chambers.974.3Development of Thin-Layer Chromatograms.994.3.1One-Dimensional Thin-Layer Chromatography.1004.3.1.1Vertical Development.1014.3.1.2Horizontal Development.1064.3.2Two-Dimensional Thin-Layer Chromatography.1084.4Drying After Development.1115Evaluation Without Derivatization.1135.1Direct Visual Evaluation.1135.1.1Detection in Daylight.1135.1.2Detection with 254-nm UV Light.1135.1.3Detection with 365-nm UV Light.1155.2Direct Optical Evaluation Using Instruments.1165.2.1Principle of Operation of a TLC Scanner.1165.2.2Direct Optical Evaluation Above 400 nm.1175.2.3Direct Optical Evaluation Below 400 nm.1175.2.4Direct Optical Evaluation with 365-nm UV Light(Fluorescence Measurement).1175.3Diode-Array Detection.1205.4Coupled Methods for Substance Identification.1225.5Documentation Without or Before Derivatization.1236Derivatization.1256.1Thermochemical Reaction.1266.2Irradiation with High-Energy Light.1276.3Reaction with Reagents.1296.3.1Spraying of TLC Plates.1296.3.1.1Manual Spraying of TLC Plates.1296.3.1.2Fully Automatic Spraying of TLC Plates.1336.3.2Dipping of TLC Plates.1346.3.3Vapor Treatment of TLC Plates.1396.3.4Coating TLC Plates.1406.4Special Cases of Derivatization.1436.4.1Prechromatographic Derivatization.1436.4.1.1Reaction with Reagents.1436.4.1.2Incorporation of Radionuclides.1446.4.2Simultaneous Derivatization and Development.1456.4.3Reaction Sequences.1466.4.4Biological-Physiological Methods of Detection.147XIVContents6.5Further Treatment of Derivatized Chromatograms.1486.5.1Effect of Heat.1486.5.2Stabilization of Colored and Fluorescent Zones.1507Evaluation After Derivatization.1537.1Visual Evaluation.1537.1.1Visual Qualitative Evaluation.1537.1.2Visual Semiquantitative Evaluation.1537.2Evaluation Using a TLC Scanner.1547.2.1Qualitative Evaluation.1547.2.2Quantitative Evaluation.1557.2.2.1Absorption Measurement.1567.2.2.2Fluorescence Measurement.1617.2.2.3Comparison of“Parallel”With“Transverse”Measurement.1667.3Evaluation Using a Video System.1747.3.1Qualitative Video Evaluation.1757.3.2Quantitative Video Evaluation.1767.3.3Comparison of the TLC Scanner With Video Evaluation.1777.4Evaluation by Flat-Bed Scanner.1787.5Evaluation Using a Digital Camera.1788Documentation.1818.1Description of a Thin-Layer Chromatogram.1818.2Documentation by Drawing,Tracing and Photocopying.1828.3Photographic Documentation.1838.3.1Photography Using the Polaroid Camera MP-4.1838.3.2Photography Using 35-mm Cameras.1838.3.2.1Photography in 254-nm UV Light.1848.3.2.2Photographs in 365-nm UV Light.1858.3.2.3Photographs in White Light.1858.3.3Archiving of 35-mm Films.1878.4Video Documentation.1888.5Documentation With Digital Cameras.1988.6TLC Scanner Documentation.1998.7Flat-Bed Scanner Documentation.1998.8Bioluminescence Measurements.2008.8.1Toxicity Screening Using the Bioluminescent Bacteria Vibrio fischeri.2008.8.2Detecting Bioluminescence With the BioLuminizerTM.200XVContents9GMP/GLP-Conforming Operations in TLC.2039.1Validation of TLC Methods.2079.2Use of Qualified/Calibrated Equipment.2119.3GMP/GLP-Conforming Raw Data Sheets.2149.4Examples of GMP/GLP-Conforming Testing Procedures(TPs).2239.4.1Identity and Purity of a Bulk Pharmaceutical Chemical andDetermination of the Limit Values of Related Compounds.2249.4.2Identity and Purity of Various Flavonoid-Containing Plant Extracts.2249.4.3Content of a Pharmaceutical Chemical in a Tablet.22510Effects of Stress.24110.1Controlled Stress on a Substance.24110.2TLC-Sensitive Substances.24210.2.1Interactions With Sorbents.24210.2.2Effect of Elevated Temperature.24210.2.3Effect of Light.24310.2.4Oxidative Effects.24511Special Methods in TLC.24711.1AMD Automated Multiple Development.24711.2OPLC Overpressured Layer Chromatography.24811.3HPPLC High Pressure Planar Liquid Chromatography.24911.4TLC-FID/FTID Combination of TLC and Flame-Ionization Detectoror Flame-Thermionic Ionization Detector.24911.5TLC-NDIR.25011.6RPC Rotation Planar Chromatography.25212Appendix.25312.1CHROMart.25312.2References.25512.3Abbreviations.26312.4Acknowledgements.26712.5Market Overview.268Photograph Section.271Subject Index.309List of TablesTable 1:Types of sorbents and supports for precoated layers.18Table 2:Meanings of code letters and numbers in product designations.19Table 3a:Important commercially available precoated layers andexamples of typical applications.2223Table 3b:New precoated layers.23Table 4:Peppermint oil(Oleum menthae piperitae).24Table 5:Production of constant humidity in closed vessels.44Table 6:Greater Celandine(Chelidonium majus L.).49Table 7:Semiautomatic application using the Linomat IV.59Table 8:Eluotropic Series.71Table 9:Carbamazepine.75Table 10:Birch leaves(Betulae folium).76Table 11:Primula root(Primulae radix).77Table 12:Liquorice root(Liquiritiae radix).78Table 13:Solvent r
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