|
|
|||
|
||||
OverviewThe first book devoted exclusively to a highly popular, relatively new detection technique Charged Aerosol Detection for Liquid Chromatography and Related Separation Techniques presents a comprehensive review of CAD theory, describes its advantages and limitations, and offers extremely well-informed recommendations for its practical use. Using numerous real-world examples based on contributors’ professional experiences, it provides priceless insights into the actual and potential applications of CAD across a wide range of industries. Charged aerosol detection can be combined with a variety of separation techniques and in numerous configurations. While it has been widely adapted for an array of industrial and research applications with great success, it is still a relatively new technique, and its fundamental performance characteristics are not yet fully understood. This book is intended as a tool for scientists seeking to identify the most effective and efficient uses of charged aerosol detection for a given application. Moving naturally from basic to advanced topics, the author relates fundamental principles, practical uses, and applications across a range of industrial settings, including pharmaceuticals, petrochemicals, biotech, and more. Offers timely, authoritative coverage of the theory, experimental techniques, and end-user applications of charged aerosol detection Includes contributions from experts from various fields of applications who explore CAD’s advantages over traditional HPLC techniques, as well its limitations Provides a current theoretical and practical understanding of CAD, derived from authorities on aerosol technology and separation sciences Features numerous real-world examples that help relate fundamental properties and general operational variables of CAD to its performance in a variety of conditions Charged Aerosol Detection for Liquid Chromatography and Related Separation Techniques is a valuable resource for scientists who use chromatographic techniques in academic research and across an array of industrial settings, including the biopharmaceutical, biotechnology, biofuel, chemical, environmental, and food and beverage industries, among others. Full Product DetailsAuthor: Paul H. Gamache (Thermo Fisher Scientific)Publisher: John Wiley & Sons Inc Imprint: John Wiley & Sons Inc Dimensions: Width: 15.90cm , Height: 3.60cm , Length: 22.60cm Weight: 0.885kg ISBN: 9780470937785ISBN 10: 0470937785 Pages: 544 Publication Date: 21 July 2017 Audience: Professional and scholarly , Professional & Vocational Replaced By: 9781394300600 Format: Hardback Publisher's Status: Active Availability: Out of stock The supplier is temporarily out of stock of this item. It will be ordered for you on backorder and shipped when it becomes available. Table of ContentsList of Contributors xvii Preface xxi Acknowledgment xxv Section 1 Fundamentals of Charged Aerosol Detection 1 1 Principles of Charged Aerosol Detection 3 Paul H. Gamache and Stanley L. Kaufman 1.1 Summary 3 1.2 History and Introduction to the Technology 4 1.3 Charged Aerosol Detection Process 9 1.3.1 Nebulization 9 1.3.2 Aerosol Conditioning 13 1.3.2.1 Solvent Load Reduction 13 1.3.2.2 Secondary Processes 13 1.3.2.3 Summary: Aerosol Transport 16 1.3.3 Evaporation 16 1.3.3.1 Aerosol Evaporation Process 17 1.3.3.2 Evaporation Rate (Re) 17 1.3.3.3 Dried Particle Size 19 1.3.3.4 Volatility and Detector Response 20 1.3.3.5 Particle Size Dependency 20 1.3.3.6 Ionizable Solutes 21 1.3.3.7 Background Solutes: Impurities 22 1.3.3.8 Summary 24 1.3.4 Aerosol Charging 24 1.3.4.1 Mechanisms 24 1.3.4.2 Diffusion Charging Overview 25 1.3.4.3 Unipolar Diffusion Charging Theory 26 1.3.4.4 CAD “Corona Jet” Charger Design 27 1.3.4.5 Corona Ion Jet and Aerosol Particle Jet 28 1.3.5 Summary of Aerosol Charging 29 1.3.6 Summary of CAD Process 29 1.4 CAD Response Model 31 1.4.1 Primary Droplet Size Distribution 32 1.4.2 Impactor 32 1.4.3 Drying and Residue Formation 33 1.4.3.1 Residue Particle Parameters 33 1.4.4 Charging of Residue Particles 33 1.4.5 Ion Removal 34 1.4.5.1 Attenuation of Particle Signal by Ion Trap 36 1.4.6 Signal Current 37 1.4.7 Signal from an Eluting Peak: Peak Shape 38 1.4.8 Peak Area Versus Injected Mass 39 1.4.9 Summary 39 1.5 Performance Characteristics 40 1.5.1 Response Curve: Shape and Dynamic Range 40 1.5.1.1 Semivolatile Analytes 44 1.5.1.2 Calibration 45 1.5.2 Peak Shape 48 1.5.3 Mass Versus Concentration Sensitivity 49 1.5.4 Sensitivity Limits 51 1.5.5 Response Uniformity 52 1.5.5.1 Solvent Gradient Effects 53 1.5.5.2 Analyte Volatility and Salt Formation 53 1.5.5.3 Analyte Density 54 1.5.5.4 Dependence of Aerosol Measurement Technique on Residue Particle Material 54 1.5.6 CAD Versus Formation of Gaseous Ions for MS 56 1.5.6.1 Pneumatically Assisted ESI 57 1.5.6.2 APCI 57 1.5.6.3 Main Differences between CAD and MS 58 References 59 2 Charged Aerosol Detection: A Literature Review 67 Ian N. Acworth and William Kopaciewicz 2.1 Introduction 67 2.2 CAD History and Background 74 2.3 Application Areas 79 2.3.1 Carbohydrates 79 2.3.2 Lipids 79 2.3.3 Natural Products 86 2.3.4 Pharmaceutical and Biopharmaceutical Analysis 86 2.3.5 Other Application Areas 131 2.4 Conclusions 131 Acknowledgements 131 References 141 3 Practical Use of CAD: Achieving Optimal Performance 163 Bruce Bailey, Marc Plante, David Thomas, Chris Crafts, and Paul H. Gamache 3.1 Summary 163 3.2 Introduction 164 3.2.1 First‐ and Second‐Generation Instrument Designs 165 3.2.2 Liquid Flow Range 165 3.2.3 Excess Liquid Removal 167 3.2.4 Temperature Control 167 3.2.5 Aerosol Creation and Transport 167 3.3 Factors Influencing CAD Performance 168 3.3.1 Analyte Properties 168 3.3.1.1 Formation of Aerosol Residue Particles 168 3.3.1.2 Inherent Response of Downstream Aerosol Detector 169 3.3.1.3 Summary of Analyte Properties 169 3.3.2 Eluent Properties and Composition 169 3.3.2.1 Mass Transport 169 3.3.2.2 Eluent Purity 170 3.3.2.3 Mobile Phase Additives 171 3.3.2.4 Additional Sources of Eluent Impurities 173 3.3.2.5 Column Bleed 174 3.3.2.6 Basic Eluents 174 3.3.2.7 System Components and Laboratory Equipment 175 3.3.2.8 Summary 176 3.4 System Configurations 177 3.4.1 Microscale LC 177 3.4.2 Post‐column Addition 177 3.4.3 Multi‐detector Configurations 178 3.5 Method Transfer 180 3.6 Calibration and Sensitivity Limits 182 3.6.1 Power Function 185 3.6.2 Summary of Calibration and Sensitivity Limits 186 References 186 4 Aerosol‐Based Detectors in Liquid Chromatography: Approaches Toward Universal Detection and to Global Analysis 191 Joseph P. Hutchinson, Greg W. Dicinoski, and Paul R. Haddad 4.1 Summary 191 4.2 Introduction 192 4.3 Universal Detection Methods 194 4.4 Factors Affecting the Response in Charged Aerosol Detection 198 4.5 Gradient Compensation 204 4.6 Response Models 205 4.7 Green Chemistry 206 4.8 Temperature Gradient Separations 209 4.9 Supercritical CO 2 Separations 210 4.10 Capillary Separations 211 4.11 Global Analysis and Multidimensional Separations 212 4.12 Conclusions 215 References 216 Section 2 Charged Aerosol Detection of Specific Analyte Classes 221 5 Lipid Analysis with the Corona CAD 223 Danielle Libong, Sylvie Héron, Alain Tchapla, and Pierre Chaminade 5.1 Introduction 223 5.2 Principles of Chromatographic Separation of Lipids 227 5.2.1 Theory of Retention Mechanism in Reversed‐Phase Liquid Chromatography 227 5.2.2 Optimizing Selectivity 231 5.2.3 Note on Using pH Modifiers for Selectivity Optimization 235 5.3 Application: Strategy of Lipid Separation 235 5.3.1 Separation of Individual Lipid Classes 236 5.3.2 Separation of Subclasses of Lipids 240 5.3.2.1 Size Exclusion Chromatography 240 5.3.2.2 Argentation Chromatography 241 5.3.3 Separation of Congeners Belonging to Specific Classes of Lipids 242 5.3.4 Behavior of Lipid Separation in Reversed‐Phase Chromatography 246 5.3.5 Behavior of Lipid Separation in Reversed‐Phase Sub‐ and Supercritical Fluid Chromatography 250 5.3.6 Multimodal Chromatographic Systems 252 5.3.7 Identification of the Molecular Species 252 5.3.7.1 Methodology for Identification of Congeners 256 5.4 Literature Review: Early Use of Corona CAD in Lipid Analysis 257 5.4.1 Biosciences 257 5.4.2 Food Chemistry 258 5.4.3 Pharmaceutical Sciences 260 5.4.3.1 Emulsions 260 5.4.3.2 Liposomes 261 5.4.3.3 Surfactants 262 5.4.3.4 Contrast Agents 263 5.4.3.5 Determination of Degradation Product and Impurities 263 5.5 Calibration Strategies 264 5.5.1 Calibration Strategies in Quantitative Analysis of Lipids 264 5.5.2 Classical Calibration (External Calibration, Normalization) 266 5.5.3 Calibration in Absence of Standards 268 References 272 6 Inorganic and Organic Ions 289 Xiaodong Liu, Christopher A. Pohl, and Ke Zhang 6.1 Introduction 289 6.2 Technical Considerations 291 6.2.1 Instrumentation Platform 291 6.2.2 Separation Column 292 6.2.3 Mobile Phase 295 6.2.4 CAD Parameter Setting 297 6.2.5 Sensitivity 297 6.2.6 Calibration Curve, Dynamic Range, Accuracy, and Precision 298 6.3 Applications 300 6.3.1 Pharmaceutical Counterions and Salts 301 6.3.2 Bisphosphonate 303 6.3.3 Phosphorylated Carbohydrates 304 6.3.4 Ionic Liquids 304 6.3.5 Pesticides 305 6.3.6 Other Applications 305 6.4 Concluding Remarks 306 References 306 7 Determination of Carbohydrates Using Liquid Chromatography with Charged Aerosol Detection 311 Jeffrey S. Rohrer and Shinichi Kitamura 7.1 Summary 311 7.2 Liquid Chromatography of Carbohydrates 312 7.3 Charged Aerosol Detection 314 7.4 Why LC‐CAD for Carbohydrate Analysis? 315 7.5 Early Applications of CAD to Carbohydrate Analysis 316 7.6 Additional Applications of CAD to Carbohydrate Analysis 317 References 322 8 Polymers and Surfactants 327 Dawen Kou, Gerald Manius, Hung Tian, and Hitesh P. Chokshi 8.1 Summary 327 8.2 Introduction 328 8.3 Polymer Analysis 328 8.4 Polyethylene Glycol 329 8.4.1 PEG Reagents 330 8.4.2 Low Molecular Weight PEGs 333 8.4.3 PEGylated Molecules 335 8.5 Surfactants 336 References 339 9 Application of Charged Aerosol Detection in Traditional Herbal Medicines 341 Lijuan Liang, Yong Jiang, and Pengfei Tu 9.1 Summary 341 9.2 Introduction 342 9.3 Factors that Affect the Sensitivity of CAD 343 9.3.1 Mobile Phase Composition 343 9.3.2 Effects of Nitrogen Gas Purity on the Sensitivity of CAD 344 9.3.3 The Effect of Mobile Phase Modifiers 344 9.3.4 Comparison of Flow Rate Effect on the Sensitivity of CAD 345 9.4 Application of CAD in Quality Analysis of Traditional Herbal Medicines 345 9.4.1 Determination of Saponins in Radix et Rhizoma Notoginseng by CAD Coupled with HPLC 345 9.4.2 Determination of Ginsenosides by LC‐CAD 346 9.4.3 Other Applications of CAD 349 9.5 Conclusion 353 References 353 Section 3 Industrial Applications of Charged Aerosol Detection 355 10 Charged Aerosol Detection in Pharmaceutical Analysis: An Overview 357 Michael Swartz, Mark Emanuele, and Amber Awad 10.1 Summary 357 10.2 Introduction 358 10.3 Analytical Method Development 359 10.4 Analytical Method Validation 361 10.5 CAD in Analytical Method Transfer 363 10.6 CAD in Formulation Development and Ion Analysis 364 10.7 Carbohydrate Analysis by CAD 368 10.8 CAD in Stability Analyses 371 10.9 Conclusion 373 References 374 11 Impurity Control in Topiramate with High Performance Liquid Chromatography: Validation and Comparison of the Performance of Evaporative Light Scattering Detection and Charged Aerosol Detection 379 David Ilko, Robert C. Neugebauer, Sophie Brossard, Stefan Almeling, Michael Türck, and Ulrike Holzgrabe 11.1 Summary 379 11.2 Introduction 380 11.3 Material and Methods 382 11.3.1 Reagents and Material 382 11.3.2 HPLC–ELSD/CAD 382 11.3.3 TLC and HPTLC Limit Test for Impurity A 383 11.4 Results and Discussion 383 11.4.1 Method Validation: Impurity Control 383 11.4.2 Method Validation: Assay 388 11.4.3 TLC and HPTLC Limit Test for Impurity A 390 11.5 Conclusion 390 Acknowledgment 390 References 391 12 Applying Charged Aerosol Detection to Aminoglycosides: Development and Validation of an RP‐HPLC Method for Gentamicin and Netilmicin 393 Arul Joseph and Abu Rustum 12.1 Introduction 393 12.1.1 Background 394 12.2 Development and Validation of an RP‐HPLC Method for Gentamicin Using Charged Aerosol Detection 395 12.2.1 Method Development 395 12.2.1.1 Selection of Detector 395 12.2.1.2 Related Substances 395 12.2.1.3 Mobile Phase Composition and Column Selection 398 12.2.1.4 Sample Preparation 400 12.2.2 Method Validation 402 12.2.2.1 Experimental 402 12.2.2.2 Specificity 403 12.2.2.3 Linearity 403 12.2.2.4 Accuracy 404 12.2.2.5 Limit of Detection and Limit of Quantitation 405 12.2.2.6 Reproducibility and Precision 406 12.2.2.7 Robustness 406 12.2.2.8 Alternate Column Validation 406 12.2.2.9 Calculation 407 12.2.2.10 Chromatographic Conditions of the Final Method 409 12.2.3 Discussion 409 12.3 Application of Strategy to Netilmicin Sulfate 410 12.3.1 Method Development 410 12.3.1.1 Sample Preparation 414 12.3.2 Method Validation 415 12.3.2.1 Specificity 415 12.3.2.2 Linearity 415 12.3.2.3 Limit of Detection and Limit of Quantitation 417 12.3.2.4 Robustness 417 12.3.2.5 Calculation 418 12.3.2.6 Chromatographic Conditions of the Final Method 418 12.3.3 Discussion 418 12.4 Conclusion 420 Acknowledgments 420 References 420 13 Determination of Quaternary Ammonium Muscle Relaxants with Their Impurities in Pharmaceutical Preparations by LC‐CAD 425 Agata Blazewicz, Magdalena Poplawska, Malgorzata Warowna‐Grzeskiewicz, Katarzyna Sarna, and Zbigniew Fijalek 13.1 Summary 425 13.2 Introduction 426 13.3 Experimental 429 13.3.1 Equipment and Conditions 429 13.3.2 Material Studied 430 13.3.3 Standard Solutions 431 13.4 Results and Discussion 431 13.4.1 Selection of Chromatographic Conditions 431 13.4.1.1 LC‐CAD Method for Atracurium, Cisatracurium, and Mivacurium and Their Impurities 431 13.4.1.2 LC‐CAD Method for Pancuronium and Its Impurities 432 13.4.2 Identification of Analytes 434 13.4.3 Validation of the Methods 434 13.4.3.1 Linearity 436 13.4.3.2 Detection and Quantitation Limits 438 13.4.3.3 Precision and Accuracy 441 13.4.3.4 Range 442 13.4.4 Determination of Active Substances and Impurities in Pharmaceutical Preparations 443 13.4.5 Stability 443 13.5 Conclusion 445 Acknowledgments 445 References 446 14 Charged Aerosol Detection of Scale Inhibiting Polymers in Oilfield Chemistry Applications 449 Alan K. Thompson 14.1 Summary 449 14.2 Background to Scale Inhibition in Oilfields 450 14.2.1 General Background 450 14.2.2 Squeeze Programs 452 14.2.3 Polymeric Inhibitors 454 14.3 Historical Methods of Analysis 455 14.4 Charged Aerosol Detection for Polymeric Scale Inhibitors 459 14.4.1 Theoretical Application of CAD 459 14.4.2 Practical Application of CAD 460 14.4.3 Typical Validation of Methodology 461 14.4.3.1 Linearity of Detection 462 14.4.3.2 Precision of Injection 463 14.4.3.3 Assay Accuracy and Precision 464 14.4.3.4 Assay Ruggedness 464 14.4.3.5 Assay Ruggedness 2: Inter‐instrument Variability 465 14.4.3.6 Limit of Detection and Limit of Quantification 466 14.4.3.7 Analysis of Routine Oilfield Brine Samples for Polymeric Scale Inhibitor Using HPLC‐CAD 466 14.4.4 Limits of Methodology 467 14.5 Conclusions and Further Work 468 References 469 15 Applications of Charged Aerosol Detection for Characterization of Industrial Polymers 471 Paul Cools and Ton Brooijmans 15.1 Introduction 471 15.2 Liquid Chromatography of Polymers 472 15.3 Solvents 475 15.4 Quantitative Detection of Polymer Molecules 476 15.4.1 Ultraviolet Detection 476 15.4.2 Differential Refractive Index Detection 476 15.4.3 Evaporative Detection 477 15.4.4 Charged Aerosol Detection 477 15.4.5 Molar Mass Dependent Detection 478 15.4.6 Mass Spectrometry 478 15.5 Size Exclusion Chromatography and Charged Aerosol Detection 479 15.6 Gradient Polymer Elution Chromatography and CAD 486 15.7 Liquid Chromatography Combined with UV, CAD, and MS Detection 490 15.7.1 LC‐ESI‐TOF MS System at DSM Coating Resins 491 15.8 Typical Examples of Industrial Applications Using LC‐MS‐CAD 492 15.8.1 Raw Material Analysis 493 15.8.2 Intermediates 494 15.8.3 End Products 495 15.9 Epilogue 497 Acknowledgments 497 References 497 Index 501ReviewsAuthor InformationPAUL H. GAMACHE is Director of Research and Development at Thermo Fisher Scientific. He has more than thirty years' experience within the analytical instrument industry. His primary area of expertise is in the development of instrumentation and techniques based on liquid chromatography. He has published more than 50 articles and book chapters including the first publication describing commercial CAD technology. In 2005 he was co-awardee of an NIH Metabolomics Roadmap research grant. Tab Content 6Author Website:Countries AvailableAll regions |