Advances In Chromatography: Volume 43

Featuring reliable, up-to-the-minute reviews of major developments in chromatography, Advances in Chromatography, Volume 43 discusses the utilization and application of new analytical methodologies. It covers subjects such as gradient elution in liquid column chromatography, solid phase microextraction, and polyelectrolytes. It also examines supercritical fluids for off-line sample preparation in food analysis and assess technologies for the analysis of biologically important compounds. Each chapter includes an abundance of bibliographic citations.

Phyllis R. Brown is Professor of Chemistry at the University of Rhode Island in Kingston, where she has taught since 1973 Eli Grushka is Professor of Analytical Chemistry at the Hebrew University of Jerusalem in Israel Susan Lunte is the Courtesy Professor of Chemistry, University of Kansas, Lawrence

Contributors

vii

Contents of Other Volumes

ix

1. Gradient Elution in Liquid Column Chromatography-Prediction of Retention and Optimization of Separation

1

(108)

Pavel Jandera

I. Introduction

3

(6)

II. Theory of Retention in Analytical Gradient-Elution Chromatography

9

(10)

A. Calculation of retention times and of retention volumes

9

(8)

B. Bandwidths and resolution in gradient-elution LC

17

(2)

III. Reversed-Phase Chromatography with Binary Gradients

19

(6)

IV. Normal-Phase Chromatography with Binary Gradients

25

(9)

V. Ion-Exchange Gradient Elution Chromatography

34

(2)

VI. Effects of the Instrumentation and of the Nonideal Retention Behavior on the Retention in Gradient Elution

36

(19)

A. Effects of the dwell volume on retention in gradient elution LC. Retention data in gradient elution with an initial hold-up period. Gradient preelution and postelution

37

(11)

B. Effects of the adsorption of strong solvents on retention

48

(7)

VII. Gradient Elution Method Development

55

(23)

A. Transfer of gradient methods and effects of changing operating conditions on separation

56

(13)

1. Changing flow rate of the mobile phase in gradient elution chromatography

58

(1)

2. Changing column diameter in gradient elution chromatography

59

(2)

3. Changing column length in gradient elution chromatography

61

(1)

4. Rapid prediction of the effects of changing gradient steepness (gradient range) and initial mobile phase composition on the separation

62

(7)

B. Optimization of gradient elution separations

69

(43)

1. Peak capacity and fast gradients

69

(2)

2. Optimization of gradients for specific separation problems

71

(7)

VIII. Chromatography with Ternary Gradients

78

(3)

IX. Peculiarities of Gradient Elution Separation of High-Molecular Compounds

81

(9)

X. Conclusion

90

(1)

Acknowledgments

90

(2)

Symbols

92

(4)

References

96

(8)

Appendix A Correction of the retention volume in normal-phase HLPC for the column uptake of polar solvents during elution (solvent-demixing effect)

104

(3)

Appendix B Schematics of a spreadsheet program for optimization of gradient elution

107

(2)

2. Supercritical Fluids for Off-Line Sample Preparation in Food Analysis Prior to Chromatography

109

(70)

Jerry W. King

I. Supercritical Fluids for Sample Preparation

110

(2)

II. Supercritical Fluid Extraction (SFE)

112

(19)

A. Basic Principles of SFE

112

(5)

B. Types of Extraction and Instrumentation

117

(5)

C. The Sample Matrix and Its Preparation for SFE

122

(3)

D. The Problem with Coextractives and Water

125

(3)

E. Collection of the Extracted Analyte

128

(3)

III. Integration of Cleanup Step with SFE

131

(11)

A. Fluid Density-Based Fractionation

132

(3)

B. Use of Adsorbents with SFE

135

(4)

C. Inverse SFE

139

(1)

D. Variation in Extraction Fluid Type or Composition

140

(2)

IV. Coupling Reaction Chemistry (Derivatization) with SFE

142

(7)

A. Reactions in Supercritical Fluid Media (SFR)

142

(2)

B. Types of Derivatizations Used in SFE

144

(2)

C. Utilization of Catalysts with SFR

146

(3)

V. Applications of Critical Fluids for Sample Preparation

149

(17)

A. Analysis of Trace Components

150

(3)

B. Proximate Fat Analysis

153

(3)

C. SFE Prior to Gas Chromatography (GC)

156

(2)

D. SFE with HPLC or SFC

158

(6)

E. SFE Integrated with Selected Chromatographic/Spectroscopic Techniques (IR,MS)

164

(2)

VI. Status of the Technique-Conclusions

166

(1)

References

167

(7)

Appendix A

174

(5)

3. Correspondence Between Chromatography, Single-Molecule Dynamics, and Equilibrium: A Stochastic Approach

179

(52)

Francesco Dondi, Alberto Cavazzini, and Michel Martin

I. Summary

180

(1)

II. Introduction

181

(2)

III. The Stochastic Approach of Chromatography

183

(6)

A. General Aspects

183

(2)

B. Basic Stochastic Model

185

(4)

IV. Peak Shape Features and Experimental Errors in the Determination of the Retention Factor

189

(6)

A. Peak Splitting Effect

190

(1)

B. Peak Tailing Effect

191

(1)

C. Stochastic Bias Effect

192

(2)

D. Injection Effect

194

(1)

E. Unretained Tracer Selection Effect

195

(1)

V. Equilibrium Conditions in Chromatography

195

(2)

VI. Discussion

197

(9)

A. Peak Splitting

198

(1)

B. Peak Tailing

199

(2)

C. Stochastic Bias

201

(1)

D. Injection

201

(1)

E. Number of Analyte Molecules

202

(4)

F. Selection of the Holdup Time Marker

206

(1)

VII. Conclusion

206

(2)

Acknowledgments

208

(1)

Glossary

208

(2)

References

210

(3)

Appendix A

213

(8)

Appendix B

221

(5)

Appendix C

226

(2)

Appendix D

228

(2)

Appendix E

230

(1)

4. Solid-Phase Microextraction: A New Tool in Contemporary Bioanalysis

231

(42)

Georgios Theodoridis and Gerhardus J. de Jong

I. Introduction

232

(2)

II Extraction Mode and Coupling

234

(8)

A. Novel Devices

238

(4)

III. Sorption Principles and Parameters

242

(4)

IV. Coatings

246

(9)

A. Absorptive Coatings

247

(2)

B. Solid Coatings

249

(1)

C. Special Coatings

250

(5)

V. Derivatization

255

(3)

VI. Bioanalytical Applications

258

(6)

VII. Possibilities and Limitations of SPME

264

(4)

References

268

(5)

5. Polyelectrolytes as Stationary Phases in Liquid Chromatography

273

(32)

Lilach Yishai-Aviram and Eli Grushka

I. Introduction

274

(2)

II The Principle of Dynamic Coating

276

(3)

III. Column Characterization

279

(3)

IV. Positively Charged Polyelectrolytes as Stationary Phases

282

(7)

A. Coating Procedures

282

(12)

B. Properties of the Phases and Retention Mechanism

294

C. Applications

289

(1)

V. Negatively Charged Polyelectrolytes as Stationary Phases

289

(9)

A. Coating Procedures

289

(2)

B. Properties of the Phases and Retention Mechanism

291

(6)

C. Applications

297

(1)

VI. Complex Polyelectrolyte Layering

298

(1)

References

298

(7)

Index

305

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Advances In Chromatography: Volume 43

Summary

Author Biography

Table of Contents

Supplemental Materials