Solid Phase Microextraction: Theory and Practice Janusz Pawliszyn Solid phase microextraction (SPME) is a recently proposed solvent-free sampling and sample preparation technique. SPME represents a quick, sensitive, and economical approach that can be adopted for field work and can be easily integrated with present analytical instrumentation into an automation process. Written by the inventor of the technique, Solid Phase Microextraction: Theory and Practice describes the theoretical and practical aspects of this new technology, which received an "R&D 100" Award in 1994 recognizing its invention as a major advancement in the analytical sciences. Solid Phase Microextraction: Theory and Practice, the first book on SPME, offers the reader: * An overview of SPME technique, theory, method development, and applications; * Experiments for beginners; * A summary of the practical applications of SPME in environmental, food, pharmaceutical, and forensic settings; * Material suitable for SPME courses or self-guided study.

Janusz Pawliszyn is Professor of Chemistry at the University of Waterloo, Ontario, Canada. The primary focus of his research program is the design of highly automated and integrated instrumentation for the isolation of organic materials from complex matrices and the subsequent separation, identification, and determination of these species. For his pioneering work, Professor Pawliszyn received the 1995 McBryde Medal, the 1996 Tswett Medal, the 1996 Hyphenated Techniques in Chromatography Award, and the 1996 Caledon Award. He is a member of the Editorial Boards of the Journal of Microcolumn Separations. The Analyst, and Field Analytical Chemistry and Technology. He presently holds the Supelco-Varian-NSERC Industrial Research Chair in New Analytical Methods and Technologies.

1. SOLID PHASE MICROEXTRACTION IN PERSPECTIVE

1

(10)

1.1 Overview

1

(2)

1.2 Solvent-Free Sample Preparation Techniques

3

(5)

References

8

(3)

2. OPERATING PRINCIPLES AND CONSTRUCTION OF SPME DEVICES

11

(32)

2.1 Historical Perspective on the Early Work

11

(4)

2.2 Basic Principle of Solid Phase Microextraction

15

(1)

2.3 Extraction Modes

16

(6)

2.4 Coatings

22

(2)

2.5 Experimental Parameters that Affect Extraction Efficiency

24

(3)

2.6 Derivatization

27

(4)

2.7 Interfaces to Analytical Instrumentation

31

(7)

2.8 Commercial Devices

38

(3)

References

41

(2)

3. THEORY OF SOLID PHASE MICROEXTRACTION

43

(54)

3.1 Introduction

43

(1)

3.2 Thermodynamics

44

(13)

3.3 Kinetics

57

(32)

3.4 Experimental Verification

89

(6)

References

95

(2)

4. SPME METHOD DEVELOPMENT

97

(44)

4.1 Coating Selection

97

(4)

4.2 Derivatization Reagent Selection

101

(3)

4.3 Extraction Mode Selection

104

(3)

4.4 Agitation Technique Selection

107

(3)

4.5 Selection of a Manual vs Automated System

110

(1)

4.6 Selection of Separation and/or Detection Technique

110

(1)

4.7 Optimization of Desorption Conditions

111

(6)

4.8 Optimization of Sample Volume

117

(5)

4.9 Determination of Extraction Time Profile in Pure Matrix

122

(1)

4.10 Determination of Extraction Time

123

(2)

4.11 Calculation of the Distribution Constant

125

(3)

4.12 Optimization of Extraction Conditions

128

(3)

4.13 Determination of Linear Dynamic Range of the Method for a Pure Matrix at Optimum Extraction Conditions

131

(2)

4.14 Selection of the Calibration Method

133

(1)

4.15 Optimization of Extraction Conditions for Heterogeneous Samples

133

(1)

4.16 Verification of the Equilibration Time, Sensitivity, and Linear Dynamic Range for a Complex Sample Matrices

134

(1)

4.17 Method Precision

135

(2)

4.18 Method Detection Limits

137

(1)

4.19 Validation

137

(2)

4.20 Automation

139

(1)

References

139

(2)

5. APPLICATIONS

141

(52)

5.1 Gaseous Matrix

142

(11)

5.2 Liquid Matrix

153

(5)

5.3 Solid Matrix

158

(3)

5.4 Environmental

161

(9)

5.5 Food and Pharmaceutical

170

(4)

5.6 Clinical and Forensic

174

(3)

5.7 Future Analytical Applications

177

(3)

5.8 Physicochemical Applications

180

(9)

References

189

(4)

6. EXPERIMENTS

193

(16)

6.1 Determination of BTEX in Water

193

(7)

6.2 Determination of Pesticides in Water

200

(4)

6.3 Determination of Caffeine in Beverages

204

(5)

A. THEORETICAL ANALYZES

209

(20)

A.1 Estimation of the Distribution Constant for an Internally Cooled Fiber

209

(3)

A.2 Analysis of Diffusion in and Near the Fiber Coating, without or with "In-Fibre" Derivatization

212

(9)

A.3 One-Dimensional Analysis of Diffusion in a Headspace SPME System

221

(6)

References

227

(2)

B. LIST OF ARTICLES PUBLISHED ON SPME APPLICATIONS

229

(14)

Glossary

243

(2)

Index

245

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