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Multidimensional Chromatography

Edited by Luigi Mondello, Alastair C. Lewis and Keith D. Bartle

Copyright © 2002 John Wiley & Sons Ltd

ISBNs: 0-471-98869-3 (Hardback); 0-470-84577-5 (Electronic)

Multidimensional Chromatography

Multidimensional

Chromatography

LUIGI MONDELLO

Dipartimento Farmaco-chimico, Università degli Studi di Messina, Italy

ALASTAIR C. LEWIS

School of Chemistry and School of the Environment, University of Leeds, UK

KEITH D. BARTLE

School of Chemistry, University of Leeds, UK

JOHN WILEY & SONS, LTD

Copyright © 2002 by John Wiley & Sons Ltd,

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Library of Congress Cataloging-in-Publication Data

Mondello Luigi.

Multidimensional chromatography / Luigi Mondello, Alastair C. Lewis, Keith D. Bartle. p. cm

Includes bibliographical references and index. ISBN 0-471-98869-3

1. Chromatographic analysis. I. Lewis, Alastair C. II. Bartle, Keith D. III. Title.

QD79.C4 M65 2001 543 .089—dc21

2001046684

British Library Cataloguing in Publication Data

A catalogue record for this book is available from the British Library

ISBN 0 471 98869 3

Typeset in 10/12pt Times by Thomson Press (India) Limited, New Delhi Printed and bound in Great Britain by Biddles Ltd, Guildford and King’s Lynn.

This book is printed on acid-free paper responsibly manufactured from sustainable forestry, in which at least two trees are planted for each one used for paper production.

CONTENTS

List of Contributors

xi

Preface

 

xiii

PART 1: GENERAL

1

1

Introduction

3

 

K.D. Bartle

 

 

1.1

Preamble

3

 

1.2

Packed Capillary Column and Unified Chromatography

4

 

1.3

Resolving Power of Chromatographic Systems

6

 

1.4

Two-Dimensional Separations

9

 

1.5

The Origins of Multidimensional Chromatography

12

 

Acknowledgements

13

 

References

13

2 Coupled High Performance Liquid Chromatography with High

 

 

Resolution Gas Chromatography

17

 

L. Mondello

 

 

2.1

Introduction

17

 

2.2

Transfer Techniques

18

 

2.3

Vaporization with Hot Injectors

25

 

2.4

Transfer of Water-Containing Solvent Mixtures

28

 

2.5

Indirect Introduction of Water

31

 

2.6

Conclusions

38

 

References

42

3 Multidimensional High Resolution Gas Chromatography

47

 

A. C. Lewis

 

 

3.1

Introduction

47

 

3.2

Practical Two-Dimensional Gas Chromatography

48

 

3.3

Practical Examples of Two-Dimensional Chromatography

57

 

3.4

Conclusions

72

 

References

72

4

Orthogonal GC – GC

77

 

P. J. Marriott

 

 

4.1

Introduction to Multidimensional Gas Chromatography

77

 

4.2

Introduction to GC GC Separation

80

vi

Contents

4.3

Introduction to Modulation Technology

82

4.4

Orthogonality of Analysis

94

4.5

Quantitative Aspects

101

4.6

Future Opportunities and Challenges of GC GC Technology

104

Acknowledgements

106

References

106

5 Coupled-Column Liquid Chromatography

109

Claudio Corradini

 

5.1

Introduction

109

5.2

Theoretical Aspects

111

5.3

LC – LC Techniques

116

5.4

Conclusions

129

References

130

6 Supercritical Fluid Techniques Coupled with Chromatographic

 

Techniques

135

F. M. Lanças

 

6.1

Introduction

135

6.2

On-Line Coupling of SFE with Chromatographic Techniques

138

6.3

SFE – GC

138

6.4

SPE – SFE – GC

139

6.5

SFE – SFC

141

6.6

SFE – LC

141

6.7

On-Line Coupling of Supercritical Fluid Extraction with

 

 

Capillary Electrodriven Separation Techniques (SFE – CESTs)

143

6.8

From Multidimensional to Unified Chromatography

 

 

Passing through Supercritical Fluids

147

References

147

7 Unified Chromatography: Concepts and Considerations for

 

Multidimensional Chromatography

151

T.L. Chester

 

7.1

Introduction

151

7.2

The Phase Diagram View of Chromatography

153

7.3

Instrumentation

159

7.4

Advantages of and Challenges for Unified Chromatography

 

 

Techniques in Multidimensional Systems

162

7.5Column Efficiency and Plate Heights in

 

Unified Chromatography

164

References

167

8 Multidimensional Planar Chromatography

171

Sz. Nyiredy

 

8.1

Introduction

171

8.2

Two-Dimensional or Multidimensional

 

 

Planar Chromatography?

172

201
203
204
206
207
208
209
210
211

Contents

 

vii

8.3

Two-Dimensional Development on Single Layers

173

8.4

Methods for the Selection of Appropriate Mobile Phases

175

8.5

Two-Dimensional Development on Bilayers

176

8.6

Multiple Development in One, Two or Three Dimensions

177

8.7

Multiple Development in One Direction

178

8.8

Multiple Development in Two Dimensions

182

8.9

Multiple Development in Three Dimensions

184

8.10

Coupled Layers with Stationary Phases of Decreasing Polarity

186

8.11

Grafted Planar Chromatography

186

8.12

Serially Connected Multilayer Forced-Flow Planar

 

 

Chromatography

188

8.13

Combination of Multidimensional Planar

 

 

Chromatographic Methods

191

8.14

Coupling of Planar Chromatography with other

 

 

Chromatographic Techniques

193

8.15

Further Considerations

193

References

194

9 Multidimensional Electrodriven Separations

197

Martha M. Degen and Vincent T. Remcho

 

9.1

Introduction

197

9.2

Electrophoretic Separations

197

9.3

Comprehensive Separations

199

9.4

Planar Two-Dimensional Separations

200

9.5Chromatography and Electrophoresis Combined in

Non-Comprehensive Manners

9.6Comprehensive Two-Dimensional Separations with

an Electrodriven Component

9.7Microcolumn Reverse Phase High Performance Liquid

Chromatography – Capillary Zone Electrophoresis

9.8Microcolumn Size Exclusion

Chromatography – Capillary Zone Electrophoresis

9.9Packed Capillary Reverse Phase High Performance

Liquid Chromatography – Capillary Zone Electrophoresis

9.10Packed Capillary Reverse Phase High Performance Liquid

Chromatography – Fast Capillary Zone Electrophoresis

9.11Three-Dimensional Size Exclusion Chromatography – Reverse Phase Liquid Chromatography –

Capillary Zone Electrophoresis

9.12Transparent Flow Grating Interface with Packed Capillary

High Performance Liquid Chromatography – Capillary

Zone Electrophoresis

9.13Online Reverse Phase High Performance Liquid Chromatography – Capillary Zone Electrophoresis – Mass

Spectrometry

viii

 

Contents

9.14

The Future of Multidimensional Electrokinetic Separations

212

9.15

Conclusions

213

References

213

PART 2: APPLICATIONS

215

10 Multidimensional Chromatography: Foods, Flavours and

 

Fragrances Applications

217

G. Dugo, P. Dugo and L. Mondello

 

10.1

Introduction

217

10.2

Multidimensional Gas Chromatography (GC–GC or MDGC) 218

10.3

Multidimensional High Performance Liquid

 

 

Chromatography

231

10.4Multidimensional Chromatography using On-Line Coupled High Performance Liquid Chromatography and Capillary

 

(High Resolution) Gas Chromatography (HPLC–HRGC)

235

10.5

Multidimensional Chromatographic Methods which

 

 

Involve the Use of Supercritical Fluids

241

10.6

Multidimensional Planar Chromatography

242

References

245

11 Multidimensional Chromatography: Biomedical and

 

Pharmaceutical Applications

251

G. W. Somsen and G. J. de Jong

 

11.1

Introduction

251

11.2

Liquid Chromatography – Liquid Chromatography

252

11.3

Solid-Phase Extraction – Liquid Chromatography

265

11.4

Liquid Chromatography – Gas Chromatography

273

11.5

Solid-Phase Extraction – Gas Chromatography

278

11.6

Solid-Phase Microextractions Coupled with Gas

 

 

or Liquid Chromatography

280

11.7

Supercritical Fluid Extraction Coupled with Supercritical

 

 

Fluid Chromatography

284

11.8

Coupled Systems Involving Capillary Electrophoresis

285

11.9

Conclusions

290

References

291

12 Industrial and Polymer Applications

303

Y. V. Kazakevich and R. LoBrutto

 

12.1

Introduction

303

12.2

General

304

12.3

LC–GC

304

Contents

 

ix

12.4

LC–GC Applications

305

12.5

SEC–GC Applications

306

12.6

SEC–Reversed Phase LC Applications

315

12.7

GC–GC Applications

317

12.8

SFC–GC and Normal Phase-LC – SFC Applications

324

12.9

Normal Phase-LC – SFC Applications

324

12.10

SFC – GC Applications

325

12.11

SFC – SFC Applications

328

12.12

Conclusions

330

 

References

331

13 Multidimensional Chromatography in Environmental Analysis

335

R. M. Marcé

 

13.1

Introduction

335

13.2

Multidimensional Gas Chromatography

336

13.3

Multidimensional Liquid Chromatography

341

13.4

Liquid Chromatography – Gas Chromatography

358

13.5

Conclusions and Trends

370

 

Acknowledgements

370

 

References

370

14 Multidimensional Chromatographic Applications in

 

the Oil Industry

379

J. Beens

 

14.1

Introduction

379

14.2

Gases

381

14.3

Gasolines and Naphthas

387

14.4

Middle Distillates

392

14.5

Residue-Containing Products

401

 

Acknowledgements

403

 

References

403

15 Multidimensional Chromatography: Forensic and

 

Toxicological Applications

407

15.1

Introduction

407

15.2

Liquid Chromatography–Gas Chromatography

408

15.3

Liquid Chromatography –Liquid Chromatography

410

15.4

Gas Chromatography–Gas Chromatography

414

15.5

On-Line Sample Preparation

427

15.6

Conclusions

429

 

Acknowledgements

429

 

References

429

Index

 

433

Multidimensional Chromatography

Edited by Luigi Mondello, Alastair C. Lewis and Keith D. Bartle

Copyright © 2002 John Wiley & Sons Ltd

ISBNs: 0-471-98869-3 (Hardback); 0-470-84577-5 (Electronic)

CONTRIBUTORS

Bartle, Keith D.

School of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK

Beens, Jan

Department of Analytical Chemistry and Applied Spectroscopy, Faculty of Sciences, Free University de Boelelaan 1083, 1081 HV Amsterdam, The Netherlands

Chester, Thomas L.

The Procter & Gamble Company, Miami Valley Laboratories, PO Box 538707, Cincinnati, OH, 45253-8707, USA

Corradini, Claudio

Consiglio Nazionale delle Ricerche, Instituto di Cromatografia, Area della Ricerca di Roma, Via Salaria Km. 29 300, 00016-Monterotondo Scalo, Roma, Italy

Degen, Martha M.

Department of Chemistry, Oregon State University, Gilbert Hall 153, Corvallis, OR, 97331-4003, USA

de Jong, G. J.

Department of Analytical Chemistry and Toxicology, University of Groningen, Antonius Deusinglaan 1, 9713 AV Groningen, The Netherlands

Dugo, Giovanni

Dipartimento Farmaco-chimico, Facoltà di Framacia, Università degli Studi di Messina, Viale Annunziata, 98168-Messina, Italy

Dugo, Paola

Dipartimento di Chimica Organica e Biologica, Facoltà di Scienze, Università degli Studi di Messina, Salita Sperone, 98165-Messina, Italy

Kazakevich, Yuri V.

Department of Chemistry, Seton Hall University, 400 South Orange Avenue, South Orange, NJ, 07079, USA

Contributors

xii

Lanças, Fernando M.

Laboratory of Chromatography, Institute of Chemistry, University of São Carlos, Av. Dr Carlos Botelho 1465, 13560-970 São Carlos (SP), Brasil

Lewis, Alastair C.

School of Chemistry and School of the Environment, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK

LoBrutto, Rosario

Department of Chemistry, Seton Hall University, 400 South Orange Avenue, South Orange, NJ, 07079, USA

Marcé, R. M.

Department of Analytical Chemistry and Organic Chemistry, Universitat Rovira i Virgili, Imperial Tarraco 1, 43005-Tarragona, Spain

Marriott, Philip J.

Chromatography and Molecular Separation Group, Department of Applied Chemistry, Royal Melbourne Institute of Technology, GPO Box 2467V, Melbourne 3001, Victoria, Australia

Mondello, Luigi

Dipartimento Farmaco-chimico, Facoltà di Farmacia, Università degli Studi di Messina, Viale Annunziata, 98168-Messina, Italy

Nyiredy, Sz.

Research Institute for Medical Plants, H-2011 Budakalàsz, PO Box 11, Hungary

Remcho, Vincent T.

Department of Chemistry, Oregon State University, Gilbert Hall 153, Corvallis, OR, 97331-4003, USA

Snow, Nicholas H.

Department of Chemistry, Seton Hall University, 400 South Orange Avenue, South Orange, NJ, 07079, USA

Somsen, G. W.

Department of Analytical Chemistry and Toxicology, University of Groningen, Antonius Deusinglaan 1, 9713 AV Groningen, The Netherlands