The HPLC-MS handbook for practitioners

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Weitere Verfasser: Kromidas, Stavros 1954- (HerausgeberIn)
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Veröffentlicht: Weinheim Wiley-VCH Verlag GmbH & Co. KGaA [2017]
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Datensatz im Suchindex

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adam_text CONTENTS PREFACE XI THE STRUCTU RE OF HPLC-MS FOR PRACTITIONERS XIII LIST OF CONTRIBUTORS X V PART I OVERVIEW, PITFALLS, HARDWARE-REQUIREMENTS 1 1 STATE OF THE ART IN THE LC/MS 3 O. SCHMITZ 1.1 INTRODUCTION 3 1.2 IONIZATION METHODS AT ATMOSPHERIC PRESSURE 5 1.2.1 OVERVIEW OF API METHODS 6 1.2.2 ESI 6 1.2.3 APCI 8 1.2.4 APPI 9 1.2.5 APLI 10 1.2.6 DETERMINATION OF ION SUPPRESSION 11 1.2.7 BEST IONIZATION FOR EACH QUESTION 11 1.3 MASS ANALYZER 12 1.4 FUTURE DEVELOPMENTS 13 1.5 WHAT SHOULD YOU LOOK FOR WHEN BUYING A MASS SPECTROMETER? 14 REFERENCES 15 2 TECHNICAL ASPECTS AND PITFALLS OF LC/MS HYPHENATION 19 M,M. MARTIN 2.1 INSTRUMENTAL REQUIREMENTS FOR LC/MS ANALYSIS - CONFIGURING THE RIGHT SYSTEM FOR YOUR ANALYTICAL CHALLENGE 20 2.1.1 (U)HPLC AND MASS SPECTROMETRY - NOT JUST A MERE FRONT-END 20 2.1.2 UHPLC SYSTEM OPTIMIZATION - GRADIENT DELAY AND EXTRA-COLUMN VOLUMES 21 2.1.3 DOES YOUR MASS SPECTROMETER FIT YOUR PURPOSE? 33 2.1.4 DATA RATES AND CYCLE TIMES OF MODERN MASS SPECTROMETERS 38 2.1.5 COMPLEMENTARY INFORMATION BY ADDITIONAL DETECTORS OR MASS SPECTROMETRY WON*T SAVE THE WORLD 39 2.2 LC/MS METHOD DEVELOPMENT AND HPLC METHOD ADAPTATION - HOW TO MAKE MY LC FIT FOR MS? 43 2.2.1 METHOD DEVELOPMENT LC/MS - LC FITS THE MS PURPOSES 44 2.2.2 CONVERTING CLASSICAL HPLC METHODS INTO LC/MS 53 2.3 PITFALLS AND ERROR SOURCES - SOMETIMES THINGS DO GO WRONG 54 2.3.1 NOTSIGNAL AT ALL 54 2.3.2 INAPPROPRIATE ION SOURCE SETTINGS AND THEIR IMPACT ON THE CHROMATOGRAM 56 2.3.3 ION SUPPRESSION 58 2.3.4 UNKNOWN MASS SIGNALS IN THE MASS SPECTRUM 59 2.3.5 INSTRUMENTAL REASONS FOR THE MISINTERPRETATION OF MASS SPECTRA 65 2.4 CONCLUSION 68 2.5 ABBREVIATIONS 69 REFERENCES 70 3 ASPECTS OF THE DEVELOPMENT OF METHODS IN LC/MS COUPLING 73 T TEUTENBERG, T HETZEL, C. PORTNER, S. WIESE, C. VOM EYSER, AND /. TUERK 3.1 INTRODUCTION 73 3.2 FROM TARGET TO SCREENING ANALYSIS 74 3.2.1 TARGET ANALYSIS 74 3.2.2 SUSPECTED-TARGET SCREENING 74 3.2.3 NON-TARGET SCREENING 74 3.2.4 COMPARABLE OVERVIEW OF THE DIFFERENT ACQUISITION MODES 75 3.3 THE OPTIMIZATION OF PARAMETERS IN CHROMATOGRAPHY AND MASS SPECTROMETRY 75 3.3.1 REQUIREMENTS AND RECOMMENDATIONS FOR HPLC/MS ANALYSIS TAKING DIN 38407-47 AS AN EXAMPLE 75 3.3.2 THE DEFINITION OF CRITICAL PEAK PAIRS IN THE CONTEXT OF HPLC/MS COUPLING 77 3.3.3 THE SEPARATION OF POLAR COMPONENTS FROM THE COLUMN VOID TIME 79 3.3.4 DETERMINING THE HPLC METHOD PARAMETERS USING THE EXAMPLE OF THE SEPARATION OF SELECTED PHARMACEUTICALS 80 3.3.5 CARRYING OUT SCREENING EXPERIMENTS 84 3.3.6 EVALUATION OF THE DATA AND DISCUSSION OF THE INFLUENCING PARAMETERS 86 3.3.7 USING SIMULATION SOFTWARE FOR FINE OPTIMIZATION 98 3.3.8 CHOOSING THE STATIONARY PHASE SUPPORT 99 3.3.9 THE INFLUENCE OF THE INNER COLUMN DIAMETER AND THE MOBILE PHASE FLOW RATE 103 3.3.10 THE INFLUENCE OF THE INJECTION VOLUME 104 3.3.11 ESTABLISHING THE MASS SPECTROMETRIC PARAMETERS 115 3.3.12 OPTIMIZATION OF THE MASS SPECTROMETRIC PARAMETERS 117 3.3.13 QUANTIFICATION USING LC/MS 122 3.3.14 SCREENING USING LC/MS 128 3.3.15 MINIATURIZATION - LC/MS QUO VADIS? 132 REFERENCES 135 PART II TIPS, EXAMPLES, TRENDS 139 4 LC/MS FOR EVERYBODY/FOR EVERYTHING? - LC/MS TIPS 141 E MANDEL 4.1 INTRODUCTION 141 4.2 TIP NUMBER 1 142 4.2.1 CHOOSING THE RIGHT LC/MS INTERFACE 142 4.3 TIP NUMBER 2 748 4.3.1 WHICH MOBILE PHASES ARE COMPATIBLE WITH LC/MS? 148 4.4 TIP NUMBER 3 149 4.4.1 PHOSPHATE BUFFER - THE EXCEPTION 149 4.5 TIP NUMBER 4 150 4.5.1 PAIRED IONS 150 4.5.2 WHICH ANTIDOTE* IS AVAILABLE? 151 4.5.3 SUMMARY 152 4.6 TIP NUMBER 5 152 4.6.1 USING ADDITIVES TO ENHANCE ELECTROSPRAY IONIZATION 152 4.6.2 ADDITIVES FOR APCI 153 4.6.3 SUMMARY 154 4.7 TIP NUMBER 6 154 4.7.1 HOW CAN I ENHANCE SENSITIVITY OF DETECTION? 154 4.8 TIP NUMBER 7 155 4.8.1 NO LINEAR RESPONSE AND POOR DYNAMIC RANGE? 155 4.8.2 THE REASONS 156 4.8.3 POSSIBLE SOLUTIONS 156 4.8.4 SUMMARY 157 4.9 TIP NUMBER 8 157 4.9.1 HOW MUCH MS DO I NEED? 157 4.9.2 SOLUTIONS 158 4.9.3 SUMMARY 158 4.10 NEED MORE HELP? 166 REFERENCES 167 PART III USER REPORTS 169 5 LC COUPLED TO MS - A USER REPORT 171 A. MULLER AND A. HOFMANN REFERENCES 176 6 PROBLEM SOLVING WITH HPLC/MS-A PRACTICAL VIEW FROM PRACTITIONERS 177 E. FLEISCHER 6.1 INTRODUCTION AND SCOPE 177 6.2 CASE EXAMPLE 1 181 6.2.1 INVESTIGATION OF METHOHEXITAL IMPURITIES AND DECOMPOSITION PRODUCTS 181 6.2.2 SAMPLE PREPARATION 181 6.3 CASE EXAMPLE 2 183 6.3.1 SEPARATION OF OLIGOMERS FROM CAPROLACTAM, MULTICOMPONENT SEPARATION OF IMPURITIES ON A GRAM SCALE 183 6.4 CASE EXAMPLE 3 184 6.4.1 PREPARATION AND ISOLATION OF BIS-NALBUPHINE FROM NALBUPHINE 184 6.5 CASE EXAMPLE 4 186 6.5.1 ISOLATION AND ELUCIDATION OF DOPAMINE IMPURITIES 186 7 LC/MS FROM THE PERSPECTIVE OF A MAINTENANCE ENGINEER 189 O. ATO/ZER 7.1 INTRODUCTION AND HISTORICAL SUMMARY 189 7.2 SPRAY TECHNIQUES 190 7.3 PASSAGE THROUGH THE ION PATH 191 7.4 THE ANALYZER 191 7.5 MAINTENANCE 193 REFERENCES 198 PART IV VENDOR S REPORTS 201 8 LC/MS - THE PAST, PRESENT, AND FUTURE 203 T.L. SHEEHAN AND E MANDEL 9 VENDOR S REPORT - SCIEX 207 D. SCHLEUDER 10 MANUFACTURER REPORT - THERMO FISHER SCIENTIFIC 213 M M . MARTIN 10.1 LIQUID CHROMATOGRAPHY FOR LC/MS 214 10.2 MASS SPECTROMETRY FOR LC/MS 215 10.3 INTEGRATED LC/MS SOLUTIONS 217 10.4 SOFTWARE 217 REFERENCES 219 ABOUT THE AUTHORS 221 INDEX 227
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spelling The HPLC-MS handbook for practitioners edited by Stavros Kromidas
1. Auflage
Weinheim Wiley-VCH Verlag GmbH & Co. KGaA [2017]
© 2017
XVI, 233 Seiten Illustrationen, Diagramme, Portraits
txt rdacontent
n rdamedia
nc rdacarrier
HPLC-MS (DE-588)4414892-6 gnd rswk-swf
Chemie
Chemistry
Environmental Chemistry
Flüssigkeitschromatographie
HPLC-MS
LC/MS
Mass Spectrometry
Massenspektrometrie
Pharmaceutical & Medicinal Chemistry
Pharmazeutische u. Medizinische Chemie
Umweltchemie
(DE-588)4143413-4 Aufsatzsammlung gnd-content
HPLC-MS (DE-588)4414892-6 s
DE-604
Kromidas, Stavros 1954- (DE-588)122124685 edt
Wiley-VCH (DE-588)16179388-5 pbl
Erscheint auch als Online-Ausgabe, ePDF 978-3-527-80919-6
Erscheint auch als Online-Ausgabe, ePub 978-3-527-80917-2
Erscheint auch als Online-Ausgabe, Mobi 978-3-527-80918-9
Erscheint auch als Online-Ausgabe, oBook 978-3-527-80920-2
DNB Datenaustausch application/pdf http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=029830807&sequence=000001&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA Inhaltsverzeichnis
spellingShingle The HPLC-MS handbook for practitioners
HPLC-MS (DE-588)4414892-6 gnd
subject_GND (DE-588)4414892-6
(DE-588)4143413-4
title The HPLC-MS handbook for practitioners
title_auth The HPLC-MS handbook for practitioners
title_exact_search The HPLC-MS handbook for practitioners
title_full The HPLC-MS handbook for practitioners edited by Stavros Kromidas
title_fullStr The HPLC-MS handbook for practitioners edited by Stavros Kromidas
title_full_unstemmed The HPLC-MS handbook for practitioners edited by Stavros Kromidas
title_short The HPLC-MS handbook for practitioners
title_sort the hplc ms handbook for practitioners
topic HPLC-MS (DE-588)4414892-6 gnd
topic_facet HPLC-MS
Aufsatzsammlung
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