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Comprehensive Sampling and Sample Preparation
 
 

Comprehensive Sampling and Sample Preparation, 1st Edition

Analytical Techniques for Scientists

 
Comprehensive Sampling and Sample Preparation, 1st Edition,Janusz Pawliszyn,ISBN9780123813732
 
 
 

J Pawliszyn   

Academic Press

9780123813732

9780123813749

3200

281 X 222

Contains a complete treatment of the theory and methodology of sampling in all physical phases and the theory of sample preparation for all major extraction techniques. 

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Key Features

  • Sampling and Sample preparation is a large and well-defined field in Analytical Chemistry, relevant for many application areas such as medicine, environmental science, biochemistry, pharmacology, geology, and food science. This work covers all these aspects and will be extremely useful to researchers and students, who can use it as a starting point to design and implement their experiments and for quality-reviewed background information.
  • There are limited resources that Educators can use to effectively teach the fundamental aspects of modern sample preparation technology. Comprehensive Sampling and Sample Preparation addresses this need, but focuses on the common principles of new developments in extraction technologies rather than the differences between techniques thus facilitating a more thorough understanding.
  • Provides a complete overview of the field. Not only will help to save time, it will also help to make correct assessments and avoid costly mistakes in sampling in the process.
  • Sample and sample preparation are integral parts of the analytical process but are often less considered and sometimes even completely disregarded in the available literature. To fill this gap, leading scientists have contributed 130 chapters, organized in 4 volumes, covering all modern aspects of sampling and liquid, solid phase and membrane extractions, as well as the challenges associated with different types of matrices in relevant application areas.

Description

Comprehensive Sampling and Sample Preparation is a complete treatment of the theory and methodology of sampling in all physical phases and the theory of sample preparation for all major extraction techniques. It is the perfect starting point for researchers and students to design and implement their experiments and support those experiments with quality-reviewed background information.

In its four volumes, fundamentals of sampling and sample preparation are reinforced through broad and detailed sections dealing with Biological and Medical, Environmental and Forensic, and Food and Beverage applications. The contributions are organized to reflect the way in which analytical chemists approach a problem. It is intended for a broad audience of analytical chemists, both educators and practitioners of the art and can assist in the preparation of courses as well in the selection of sampling and sample preparation techniques to address the challenges at hand. Above all, it is designed to be helpful in learning more about these topics, as well as to encourage an interest in sampling and sample preparation by outlining the present practice of the technology and by indicating research opportunities.

Readership

Educators and practitioners of analytical chemistry as well as researchers and graduate students of analytical chemistry, medicine, environmental science, biochemistry, pharmacology, geology, and food science.

Janusz Pawliszyn

The primary focus of Professor Pawliszyn's research program is the design of highly automated and integrated instrumentation for the isolation of analytes from complex matrices and the subsequent separation, identification and determination of these species. The primary separation tools used by his group are Gas Chromatography, Liquid Chromatography and Capillary Electrophoresis coupled to variety of detections systems, including range of mass spectrometry techniques. Currently his research is focusing on elimination of organic solvents from the sample preparation step to facilitate on-site monitoring and in-vivo analysis. Several alternative techniques to solvent extraction are investigated including use of coated fibers, packed needles, membranes and supercritical fluids. Dr. Pawliszyn is exploring application of the computational and modeling techniques to enhance performance of sample preparation, chromatographic separations and detection. The major area of his interest involves the development and application of imaging detection techniques for microcolumn chromatography, capillary electrophoresis and micro chip separation devices. He is an author of over 400 scientific publications and a book on Solid Phase Microextraction. His Hirsch Index (H-index) is 69. He is a Fellow of Royal Society of Canada and Chemical Institute of Canada, editor of Analytica Chimica Acta, Trends in Analytical Chemistry and a member of the Editorial Board of Journal of Separation Science. He initiated a conference, "ExTech", focusing on new advances in sample preparation and disseminates new scientific developments in the area, which meets every year in different part of the world. He received the 1995 McBryde Medal, the 1996 Tswett Medal, the 1996 Hyphenated Techniques in Chromatography Award, the 1996 Caledon Award, the Jubilee Medal 1998 from the Chromatographic Society, U.K., the 2000 Maxxam Award from Canadian Society for Chemistry, the 2000 Varian Lecture Award from Carleton University, the Alumni Achievement Award for 2000 from Southern Illinois University, the Humboldt Research Award for 2001, 2002 COLACRO Medal, 2003 Canada Research Chair, in 2006 he has been elected to the most cited chemists by ISI, in 2008 he received A.A. Benedetti-Pichler Award from Eastern Analytical Symposium, 2008 Andrzej Waksmundzki Medal from Polish Academy of Sciences, 2008 Manning Principal Award, 2010 Torbern Bergman Medal from the Swedish Chemical Society, 2010 Ontario Premier's Innovation Award, 2010 Marcel Golay Award, 2010 ACS Award in Separation Science and Technology and 2011 PittCon Dal Nogare Award. He presently holds the Canada Research Chair and Natural Sciences and Engineering Research Council of Canada Industrial Research Chair in New Analytical Methods and Technologies. He presently holds the University Professor title, the Canada Research Chair and NSERC Industrial Research Chair in New Analytical Methods and Technologies. His Hirsh Index ("H" Index) is 70.

Affiliations and Expertise

University Professor and Canada Research Chair, Department of Chemistry, University of Waterloo, Ontario

Comprehensive Sampling and Sample Preparation, 1st Edition

Editor-in-Chief

Section Editors

Contributors

Preface

VOLUME 1. Sampling Theory and Methodology

Sampling Theory

1.01. Theoretical Approaches

1.01.1 Introduction

1.01.2 Obtaining the Variance of an Estimator: Taylor Series Method

1.01.3 Simple Random Sampling

1.01.4 Stratified Random Sampling

1.01.5 Systematic Sampling

1.01.6 Cluster Sampling

1.01.7 Conclusion

See also

REFERENCES

Relevant Websites

Quality Assurance and Quality Control

1.02. Methodologies for Sample Preservation and Stabilization

1.02.1 Introduction

1.02.2 Analyte Lost Processes

1.02.3 Methodologies Applied to Aqueous Matrices

1.02.4 Methodologies Applied to Solid Matrices

1.02.5 Methodologies Applied to Biological Matrices

1.02.6 Concluding Remarks

See also

REFERENCES

Relevant Websites

1.03. Assessing and Controlling Sample Contamination

1.03.1 Introduction

1.03.2 Sources of Contamination and their Control

1.03.3 Control of Contamination

See also

REFERENCES

Relevant Websites

1.04. Sample Homogenization

1.04.1 Requirements for Sample Homogenization in Environmental and Food Analysis

1.04.2 Homogenization Theory

1.04.3 Standardized Methods for Sample Homogenization

1.04.4 Validation Procedures

1.04.5 Homogenization Techniques

1.04.6 Application to Food Matrices

1.04.7 Application to Environmental Matrices

1.04.8 Conclusions

Acknowledgments

See also

REFERENCES

Relevant Websites

Emerging Techniques

1.05. Sampling Strategy for Process Control

1.05.1 Introduction to Sampling Approaches for Process Analyzers

1.05.2 A Home for the Analytical System

1.05.3 System Design Consideration Process Analysis

1.05.4 A Home for the Analytical System Revisited

1.05.5 Fast-Loop Filter Technology

1.05.6 What Material Should be Used for Sample Lines?

1.05.7 Extractive Sampling Valves

1.05.8 Ancillary Uses of Real-Time Analyzer Systems in Production

1.05.9 Detection Limit Determination and Calibration

1.05.10 The Future of Process Sampling

1.05.11 New Sampling/Sensor Initiative (NeSSI™)

See also

REFERENCES

Relevant Websites

1.06. Integrated Total Analysis Systems

1.06.1 Introduction

1.06.2 Methods of Environmental Analysis

1.06.3 Optical Measuring Techniques

1.06.4 Integrated Sensor Systems for Continuous Monitoring

1.06.5 Conclusion

See also

REFERENCES

Relevant Websites

1.07. Nanomaterials

1.07.1 Introduction

1.07.2 Types of ENPs

1.07.3 Specificities of ENPs Relevant to Sampling

1.07.4 Sampling of ‘Pure’ ENPs

1.07.5 Sampling of ENPs Contained in ‘Real’ Matrices

1.07.6 Conclusions

See also

REFERENCES

Gaseous Samples

1.08. Indoor Air Sampling

1.08.1 Occurrence of Organic Pollutants in Indoor Environments

1.08.2 Sampling Techniques

1.08.3 Sampling and Sample Treatment Procedures for the Determination of Indoor Pollutants

1.08.4 Conclusions and Future Trends

See also

REFERENCES

Relevant Websites

1.09. Exposure Assessment in the Workplace

1.09.1 Introduction

1.09.2 Inhalatory Exposure Assessment for Health-Related Aerosols in Workplaces

1.09.3 Inhalatory Exposure Assessment for Gas and Vapor in Workplaces

1.09.4 Dermal Exposure Assessment in Workplaces

1.09.5 Occupational Sampling Strategy for Comprehensive Exposure Assessment

See also

REFERENCES

Relevant Websites

1.10. Aerosols PM and PM

1.10.1 Introduction

1.10.2 Sampling of PM10 and PM2.5

1.10.3 Chemical and Biological Composition of PM10 and PM2.5 and the Influence of Air Mass Origin

1.10.4 Real-Time Atmospheric Particle Measurements

1.10.5 Conclusion

See also

REFERENCES

Relevant Websites

1.11. Passive Sampling of Atmospheric Organic Contaminants

1.11.1 Evolution of Passive Sampling of Atmospheric Contaminants

1.11.2 Types of Passive Samplers

1.11.3 Atmospheric Compounds Sampled

1.11.4 Analysis of Passive Samplers

1.11.5 Calibration of Passive Samplers

1.11.6 Applications

1.11.7 Future Trends and Challenges

See also

REFERENCES

Relevant Websites

Liquid Samples

1.12. Surface Microlayer

1.12.1 Introduction

1.12.2 Techniques for Sampling the Microlayer

1.12.3 Sampling Efficiency

1.12.4 Chemicals in SML

1.12.5 Sampling and Assessment of Inorganic Compounds in SMLs

1.12.6 Biology of Microlayers and Biological Implications

1.12.7 Developments in SML Sampler Techniques: Robotics in SML Sampling

1.12.8 SML Sampling in Oceans and Extreme Environments

1.12.9 Significance of Microlayer Studies in Water Quality Assessments and Oil Spill Episodes

1.12.10 Concluding Remarks

Acknowledgments

See also

REFERENCES

Relevant Websites

1.13. Equipment for Water Sampling Including Sensors

1.13.1 Introduction

1.13.2 Types of Samples

1.13.3 General Considerations

1.13.4 Water Sampling Equipment

1.13.5 Surface Water Sampling Equipment

1.13.6 Groundwater Sampling Equipment

1.13.7 Rainwater Samplers

1.13.8 Sensors and Actuators

1.13.9 Integrated Control Systems in Sampling

1.13.10 Concluding Remarks

See also

REFERENCES

Relevant Websites

1.14. Passive Sampling of Organic Contaminants in Waters

1.14.1 Introduction

1.14.2 Theory and Modeling

1.14.3 Types of Samplers and Example Applications

1.14.4 Comparisons With Biomonitoring and Use With Bioassays

See also

REFERENCES

Relevant Websites

1.15. Passive Sampling for Inorganic Contaminants in Water

1.15.1 Introduction

1.15.2 Principles of Passive Sampling

1.15.3 Passive Sampler Devices

1.15.4 Applications of Samplers

1.15.5 Future Trends

See also

REFERENCES

1.16. Seawater Organic Contaminants

1.16.1 Introduction

1.16.2 Seawater Sampling

1.16.3 Collection Methods

1.16.4 Sampling Devices for Seawater

Acknowledgments

REFERENCES

Relevant Websites

1.17. Sampling Approaches for Trace Element Determination in Seawater

1.17.1 Introduction

1.17.2 Clean Techniques

1.17.3 Sampling Approaches

Appendix 1: Symbols and Abbreviations

Annex 1

Annex 2

Annex 3

See also

REFERENCES

Relevant Website

1.18. Sampling of Humic and Colloidal Phases in Liquid Samples

1.18.1 Introduction

1.18.2 What is Humic and Colloidal Phase?

1.18.3 Distribution and Sources of COM in the Aquatic Environment

1.18.4 Colloidal Scavenging in Aquatic Environments

1.18.5 Determination of DOM and COM

1.18.6 The Characterization of Humic and Colloidal Matter

1.18.7 Separation of Humic and Colloidal Phases from Aqueous Samples

1.18.8 Conclusions

See also

REFERENCES

Relevant Website

Solid Samples

1.19. Sampling of Fish, Benthic Species, and Seabird Eggs in Pollution Assessment

1.19.1 Introduction

1.19.2 Types of Sampling Studies

1.19.3 Marine Conventions and Other International Programs Related to Contaminants and Their Effects

1.19.4 Environmental Matrices: Advantages and Disadvantages of Biota

1.19.5 Substances Relevant to Biota Monitoring

1.19.6 Basic Concepts in Biomonitoring

1.19.7 Purposes of Sampling Marine Biota

1.19.8 Selection of Species

1.19.9 Sampling Period

1.19.10 Sampling Frequency

1.19.11 Field Sampling and Sampling Equipment: Storage and Pretreatment of Samples

1.19.12 Banking

1.19.13 Summary and Conclusions

See also

REFERENCES

Relevant Websites

1.20. Collection and Preparation of Human Biological Specimens for Contaminant Analysis

1.20.1 Introduction

1.20.2 Sampling of Biomatrices

1.20.3 Sample Preparation Techniques Used with Biomatrices

1.20.4 Alternative Matrices

1.20.5 Conclusions

See also

REFERENCES

Food Safety

1.21. Food Contaminanants

1.21.1 Introduction

1.21.2 Sampling Plans: Basic Concepts

1.21.3 Sampling Plans for Chemical Hazards

1.21.4 Sampling Plans for Microbial Hazards

1.21.5 Rules for Sampling and Preparation of Samples for Analysis

1.21.6 European Legislation on Sampling Methods for Foodstuff Control

1.21.7 Evaluation of Microbiological Quality in Food Environments

1.21.8 Concept of FSO

See also

REFERENCES

Relevant Websites

Forensic Applications

1.22. Biopsic Sampling (Cancer)

1.22.1 Principles of Histologic Sampling

1.22.2 Principles of Gross Specimen Handling and Histologic Techniques

1.22.3 Cytologic Specimens

See also

REFERENCES

Relevant Websites

1.23. Legal and Forensic Sampling

1.23.1 Introduction and Scope

1.23.2 Role of Statistics as Sampling Strategy

1.23.3 Analysis of Ignitable Liquid Residues from Fire Debris

1.23.4 Detection and Analysis of Explosives

1.23.5 Gunshot Residue Analysis

1.23.6 Analysis of Controlled Substances and Toxicants from Different Matrices

1.23.7 Forensic Examination of Trace Evidence

1.23.8 Forensic Environmental Analysis

1.23.9 Analysis of Human Odor Profile

1.23.10 Analysis of Human Decomposition Products

1.23.11 Nuclear Forensics

1.23.12 Field Sampling Methods for Analytes of Forensic Interests

1.23.13 Conclusion

See also

REFERENCES

Relevant Websites

VOLUME 2. Theory of Extraction Techniques

Extraction Techniques

2.01. Theory of Extraction

2.01.1 Perspective on Sample Preparation

2.01.2 Fundamentals

2.01.3 Optimization of the Extraction Process

2.01.4 Summary: Significance of Fundamental Developments

Frequently used Symbols and Abbreviations

See also

REFERENCES

2.02. Headspace Analysis

2.02.1 Introduction

2.02.2 Static Headspace

2.02.3 Dynamic Headspace

2.02.4 Headspace Sensitivity

2.02.5 Sample Handling

2.02.6 GC Column

2.02.7 Headspace Hardware

2.02.8 Enrichment Techniques to Enhance Sensitivity

2.02.9 Quantitative Analysis

2.02.10 Qualitative Analysis

2.02.11 Conclusions

Acknowledgments

See also

REFERENCES

2.03. Liquid–Liquid Extraction: Basic Principles and Automation

2.03.1 Introduction and Scope of Coverage

2.03.2 Operation Optimization Strategies

2.03.3 Batch Liquid–Liquid Extraction

2.03.4 Countercurrent Liquid–Liquid Extraction

2.03.5 Extraction Apparatus and Techniques

2.03.6 LLE Techniques

2.03.7 LLE Applications for Environmental Analysis

2.03.8 Automation and Future Perspective

See also

REFERENCES

Relevant Websites

2.04. Soxhlet Extraction and New Developments Such as Soxtec

2.04.1 Historical Outline of Conventional Soxhlet Extraction

2.04.3 Focused Microwave-Assisted Soxhlet Extraction (FMASE)

2.04.4 High-Pressure Soxhlet Extraction

2.04.5 Ultrasound-Assisted Soxhlet Extraction

2.04.6 Turbulent Solid-Liquid Extraction Techniques – Promising Soxhlet-Related Extraction Techniques

2.04.7 Summary

See also

REFERENCES

2.05. Soxhlet Extraction Versus Accelerated Solvent Extraction

2.05.1 Introduction

2.05.2 Soxhlet Extraction

2.05.3 Accelerated Solvent Extraction

2.05.4 Comparing Soxhlet Extraction and ASE

2.05.5 Future Perspectives

See also

REFERENCES

2.06. Accelerated Solvent Extraction (ASE) and High-Temperature Water Extraction

2.06.1 Introduction

2.06.2 Operation

2.06.3 Method Optimization

2.06.4 Method Development

2.06.5 Selectivity in ASE

2.06.6 High-Temperature Water Extraction

2.06.7 Conclusions

See also

REFERENCES

2.07. Fundamentals of Supercritical Fluid Extraction

2.07.1 Introduction

2.07.2 Theoretical Fundamentals

2.07.3 Material and Devices

2.07.4 Implementations and Applications of Supercritical Fluid Extraction

See also

REFERENCES

Relevant Websites

2.08. Microwave Extraction

2.08.1 Introduction

2.08.2 Principle of Microwave Heating

2.08.3 Instrumental Aspects

2.08.4 Factors Affecting MAE

2.08.5 Typical Operating Conditions

2.08.6 Standard Methods

2.08.7 Novel Developments

2.08.8 Applications

2.08.9 Conclusion

2.08.10 Manufacturers

See also

REFERENCES

Relevant Websites

2.09. Solvent Microextraction

2.09.1 Introduction

2.09.2 The Development of SME

2.09.3 SME Theory

2.09.4 Major SME Modes

2.09.5 Practical Experimental Issues for SME

2.09.6 Current and Future Trends

2.09.7 Conclusions

See also

REFERENCES

2.10. Dispersive Liquid–Liquid Microextraction

2.10.1 Introduction

2.10.2 Principles of DLLME

2.10.3 Parameters Affecting DLLME Efficiency

2.10.4 Derivatization in DLLME

2.10.5 Combination of DLLME with Other Sample Preparation Methods

2.10.6 Automation of DLLME

2.10.7 New Configurations in DLLME

2.10.8 Applications of DLLME

2.10.9 Future Trends

2.10.10 Conclusions

See also

REFERENCES

2.11. Ionic Liquids

2.11.1 Introduction

2.11.2 LLE Using Ionic Liquids

2.11.3 Microextraction Approaches Using Ionic Liquids

2.11.4 Conclusion

See also

REFERENCES

Relevant Websites

2.12. Sorbent Chemistry, Evolution

2.12.1 Brief History of Solid-Phase Extraction

2.12.2 Theoretical Background of SPE

2.12.3 Evaluation of Formats, Sorbent Types, and Modes of Interaction in SPE

2.12.4 Physical and Chemical Characteristics of Adsorbents

2.12.5 Future Remarks

See also

REFERENCES

2.13. Sorbents for Gas Sampling

2.13.1 Introduction

2.13.2 Considerations for Choosing the Gas Sampling Device and Adsorbent

2.13.3 Physical Structure of Adsorbents

2.13.4 List of Adsorbents for Air Sampling

2.13.5 Conclusions

See also

REFERENCES

Relevant Websites

2.14. Principles and Practice of Solid-Phase Extraction

2.14.1 Introduction

2.14.2 Sampling Devices

2.14.3 Sorbent Types and Their Applications

2.14.4 Theory of SPE

2.14.5 Method Development

2.14.6 Automation

2.14.7 Conclusions

See also

REFERENCES

2.15. Matrix Solid-Phase Dispersion

2.15.1 Introduction: Development of the Matrix Solid-Phase Dispersion Technique

2.15.2 Principle of Matrix Solid-Phase Dispersion

2.15.3 Factors Affecting MSPD Performance

2.15.4 Recent Trends and Combined Use with Other Techniques

2.15.5 Conclusions

See also

REFERENCES

2.16. Sol–Gel Materials in Analytical Microextraction

2.16.1 Introduction

2.16.2 Historical Backdrop of the Sol–Gel Process

2.16.3 Historical Development of Microextraction

2.16.4 Solid-Phase Microextraction

2.16.5 Coating Basics

2.16.6 SPME Principle

2.16.7 The Sol–Gel Process

2.16.8 Sol Solution Components

2.16.9 Pretreatment of Microextraction Support Materials for Sol–Gel Process

2.16.10 Post-coating Treatment

2.16.11 Characterization of Sol–Gel Materials

2.16.12 Sol–Gel Coating Materials for Fiber SPME

2.16.13 Unique Materials used on Sol–Gel SPME Fibers

2.16.14 Capillary Microextraction Techniques and Sol–Gel Coatings

2.16.15 Stir-Bar Sorptive Extraction and Sol–Gel Coatings

2.16.16 Other Uses of Sol–Gel Materials in Analytical Microextraction

2.16.17 Conclusion

See also

REFERENCES

2.17. Molecularly Imprinted Polymers

2.17.1 Introduction

2.17.2 Synthetic Procedures to Produce MIPS

2.17.3 MIPs for Sample Preparation

2.17.4 Outlook and Expected Future Trends

See also

REFERENCES

Relevant Websites

2.18. Monoliths, Fundamentals for Sample Preparation

2.18.1 Introduction

2.18.2 Monoliths for Sample Preparation

2.18.3 Applications

2.18.4 Concluding Remarks

See also

REFERENCES

2.19. Bioaffinity Sorbents

2.19.1 Introduction

2.19.2 Immunosorbents

2.19.3 Oligosorbent: Immobilized Aptamers as an Alternative to Antibodies

2.19.4 Other Bioaffinity Sorbents Used for Solid-Phase Extraction

2.19.5 Conclusions

See also

REFERENCES

2.20. Nanomaterials for Sample Preparation

2.20.1 Introduction

2.20.2 Nanomaterials for Sample Preparation

2.20.3 Mechanism of Adsorption on Nanomaterials

2.20.4 Sorbents for Preconcentration

2.20.5 Other Sample Preparation Applications

2.20.6 Conclusions and Future Prospects

See also

REFERENCES

Relevant Websites

2.21. Solid-Phase Microextraction

2.21.1 Introduction

2.21.2 SPME Theory and Principles

2.21.3 Optimization of SPME Methods

2.21.4 Calibration in SPME

2.21.5 Automated and High-Throughput SPME Approaches

2.21.6 Microextraction Devices other than Fiber-SPME

2.21.7 SPME Applications and Future Directions

2.21.8 Conclusions

Acknowledgments

See also

REFERENCES

Relevant Websites

2.22. Membrane Extraction: General Overview and Basic Techniques

2.22.1 Introduction

2.22.2 Different Formats for Membrane Extraction

2.22.3 Membrane Devices for Sample Preparation

2.22.4 Theory and Basic Principles of Membrane Extraction

2.22.5 Conclusion

Acknowledgements

See also

REFERENCES

2.23. Hollow Fiber Liquid-Phase Microextraction

2.23.1 Introduction

2.23.2 Historical Development

2.23.3 Theory and Fundamentals

2.23.4 Development of LPME Methods

2.23.5 Forefront Applications

2.23.6 Performance

2.23.7 EME

2.23.8 Future Perspectives

See also

REFERENCES

2.24. Membrane Inlets for Mass Spectrometry

2.24.1 Introduction

2.24.2 Fundamentals of Membrane Inlet Mass Spectrometry

2.24.3 Principles and Applications of Analysis

2.24.4 Conclusions and Future Perspectives

See also

REFERENCES

2.25. Microdialysis Sampling in the Brain: Analytical Approaches and Challenges

2.25.1 Introduction

2.25.2 Rationale for Use of Microdialysis

2.25.3 Probe Design and Function

2.25.4 Analytical Methods

2.25.5 On-line versus Off-line Analysis of Microdialysis Samples

2.25.6 On-line Coupling of Microdialysis to Analytical Systems

2.25.7 Summary

Acknowledgment

See also

REFERENCES

Extension of Extraction Technologies (Processes)

2.26. Analytical Derivatization Techniques

2.26.1 Introduction

2.26.2 Derivatization for Gas Chromatography (GC) and Hyphenated Techniques

2.26.3 Derivatization for Liquid Chromatography and Hyphenated Techniques

2.26.4 Sample Handling Methods for Derivatization

2.26.5 Methods and Conditions for Derivatization

2.26.6 Quantitation Aspects for Derivatization

2.26.7 Derivatization Reagents for Particular Applications/Specific Analytes

2.26.8 Conclusion

See also

REFERENCES

Abbreviations

2.27. Sample Preparation Automation for GC Injection

2.27.1 Introduction

2.27.2 Steps in the Analytical Process

2.27.3 Automation Equipment

2.27.4 Headspace Techniques

2.27.5 Solid-Phase Extraction (SPE)

2.27.6 Solid-Phase Microextraction

2.27.7 Thermal Methods

2.27.8 Automation for Solid Sample Analysis

2.27.9 Derivatization

2.27.10 Concluding Remarks

See also

REFERENCES

Relevant Websites

2.28. LC Automation

2.28.1 Introduction

2.28.2 Coupling of General Sample Preparation Processes with LC

2.28.3 High-Throughput On-Line Sample Preparation Using a Single Column

2.28.4 High-Throughput On-Line Sample Preparation Using Dual Columns

2.28.5 High-Throughput On-Line Sample Preparation Using Multiple Columns

2.28.6 On-Line Sample Preparation Using Disposable SPE Devices

2.28.7 Concluding Remarks

See also

REFERENCES

Relevant Websites

2.29. Column-Switching Sample Preparation

2.29.1 Introduction

2.29.2 Fundamentals of Column-Switching Techniques

2.29.3 Online Sample Preparation with Column Switching

2.29.4 Advantages and Disadvantages of Column-Switching Systems

2.29.5 Conclusions and Future Perspectives

See also

REFERENCES

2.30. Fundamentals and Applications of Needle Trap Devices

2.30.1 Introduction

2.30.2 Theory

2.30.3 Evolution of Needle Trap Technologies

2.30.4 Applications

2.30.5 Automation

2.30.6 Future Directions

Acknowledgment

See also

REFERENCES

Relevant Websites

2.31. Validation and Regulatory Issues for Sample Preparation

2.31.1 Introduction

2.31.2 Quality Assurance/Quality Control System

2.31.3 Method Validation

2.31.4 Validation Parameters

2.31.5 Summary

See also

REFERENCES

Relevant Websites

VOLUME 3. Extraction Techniques and Applications: Biological/Medical and Environmental/Forensics

Introduction to Extraction Techniques and Applications: Biological/Medical

3.01. General Considerations when Dealing with Biological Fluid Samples

3.01.1 Introduction

3.01.2 Characteristics of Biological Fluids

3.01.3 Biological Variations

3.01.4 Sample Collection, Handling, and Preservation

3.01.5 Conclusion

See also

REFERENCES

Relevant Websites

3.02. Considerations on Dealing with Tissues and Cell Samples (Include Tissue Banking)

3.02.1 General Introduction

3.02.2 Biospecimen Variables

3.02.3 Cellularity of Tumors and its Relevance to Research

3.02.4 RNA Integrity in Breast Cancer Tissues

3.02.5 Factors Affecting Quality of DNA

Acknowledgments

See also

REFERENCES

Relevant Websites

3.03. Cell Separation, Perfusion from Tissue, Organelle Fractionation: A Comparison of the Methods Used for Porcine Islet Isolation for Transplantation as a Treatment for Type 1 Diabetes Mellitus

3.03.1 Introduction

3.03.2 Fundamentals of Pancreatic Islet Isolation

3.03.3 Quantitative and Qualitative Assessment of Islets

3.03.4 Recent Improvements and Optimization of Method Parameters

Acknowledgements

See also

REFERENCES

Relevant Websites

3.04. Tissue Preparation for Microscopy and Histology

3.04.1 Tissue Fixation

3.04.2 Tissue Processing

3.04.3 Tissue Embedding and Sectioning

3.04.4 General Aspects of Staining

3.04.5 H&E Staining

3.04.6 Special Stains

3.04.7 Frozen Section Technique

3.04.8 Immunohistochemical Stains

3.04.9 Nucleic Acid In Situ Hybridization

3.04.10 Tissue Microarray

3.04.11 Electron Microscopy

See also

REFERENCES

Relevant Websites

Clinical Analysis

3.05. Blood Sample Collection and Handling

3.05.1 Introduction

3.05.2 Infection Control and Safety

3.05.3 Communication with the Patient

3.05.4 Anatomy and Sites for Blood Collection

3.05.5 Venipuncture Equipment

3.05.6 Details for Performing Blood Collection by Venipuncture

3.05.7 Labeling and Documentation

3.05.8 Issues to Avoid

3.05.9 Complications of Phlebotomy

3.05.10 Post-Venipuncture Care

3.05.11 Blood Specimen Handling and Storage

3.05.12 Components of Blood

3.05.13 Preparation of Blood Smears

3.05.14 Summary

See also

REFERENCES

Relevant Websites

3.06. Urine Sample Collection and Handling

3.06.1 Introduction

3.06.2 Types of Urine Samples

3.06.3 Safety and Infection Control

3.06.4 Communication and Ethical Considerations in Urine Collection

3.06.5 Collection of Urine

3.06.6 Urine Specimen Labeling

3.06.7 Collection of Animal Urine

3.06.8 Storage and Preservation of Urine

3.06.9 Pretreatment of Urine

3.06.10 Conclusion

Acknowledgment

REFERENCES

3.07. Clinical Immunoassays and Immunosensing

3.07.1 Introduction

3.07.2 Antigen, Antibody and Immunoreaction

3.07.3 Immunoassay Technologies

3.07.4 Immunosensors

3.07.5 Immunosensor Development for Clinical Applications

3.07.6 Conclusion

See also

REFERENCES

Relevant Websites

3.08. Preparation and Analytical Applications of Quantum Dots

3.08.1 Introduction

3.08.2 Preparation of QDs

3.08.3 Fluorescent Applications of QDs

3.08.4 ECL Applications of QDs

3.08.5 Electrochemical Applications of QDs

3.08.6 Conclusion

See also

REFERENCES

3.09. Newborn Screening of Genetic Diseases

3.09.1 Background to Newborn Screening

3.09.2 The Newborn Screen Sample

3.09.3 The Influence of External Factors on Newborn Screen Sample Integrity

3.09.4 Properties of the Filter Paper Matrix and its Quality Assurance for Newborn Screening

3.09.5 Preparation of Whole Blood Calibrators, Quality Control, and Proficiency Testing Materials for Newborn Screening

3.09.6 Stability of Analytes in DBS Samples

3.09.7 Newborn Screening Assays

3.09.8 Amino Acid and Acylcarnitine Analysis by MS/MS

3.09.9 Enzyme Analysis in DBS Samples

3.09.10 Analysis of Hormones in DBS Samples

3.09.11 Newborn Screening for Cystic Fibrosis

3.09.12 DNA Extraction and Analysis on DBS Samples

3.09.13 Newborn Screening for Hemoglobinopaties

3.09.14 New Developments in Newborn Screening

3.09.15 Conclusion

See also

REFERENCES

Relevant Websites

3.10. Issues and Pitfalls in Biomarker Development and Clinical Relevance

3.10.1 Biological Markers: Perspective and Current Translational Challenges

3.10.2 Biomarker Discovery and Development: Difficulties and Discontent

3.10.3 Preanlaytical Influences on Biomarker Development

3.10.4 Biomarker Validation

3.10.5 Conclusion and Future Outlooks: Improved Biomarker Research

See also

REFERENCES

Genomic, Proteomic and Metabolomics Analysis

3.11. DNA Damage, Repair, and Genome Instability (Including Affinity Techniques)

3.11.1 Introduction

3.11.2 Method Development of CE–LIF Immunoassays

3.11.3 CE Immunoassays for Detection of BPDE-DNA Adducts

3.11.4 DNA Adduct as Biomarker for DNA Repair Study

3.11.5 DNA Methylation Analysis and Application in Evaluation of Epigenetic Toxicity

See also

REFERENCES

3.12. Proteolytic Digestion Methods for Shotgun Proteomics

3.12.1 Introduction

3.12.2 Proteomic Analysis Challenges

3.12.3 Sample Cleanup Prior to Digestion

3.12.4 Protein Solubility and Resolubilization

3.12.5 Proteolytic Enzymes

3.12.6 Peptide Heterogeneity from Proteolytic Digestions

3.12.7 Protein Complex Digestions

3.12.8 Digestion Strategies for Analysis of Posttranslational Modifications

3.12.9 Strategies for Multiple Protease Digestions

3.12.10 Digestions for Analysis of Integral Membrane Proteins

3.12.11 Protocols

See also

REFERENCES

Relevant Websites

3.13. Microwave Digestion of Protein Samples for Proteomics Applications

3.13.1 Introduction

3.13.2 Microwave-Assisted Enzyme Reactions

3.13.3 Microwave-Assisted Chemical Reactions

3.13.4 Conclusions

See also

REFERENCES

3.14. Selective Enrichment of Phosphopeptides Using Nanomaterials and Monolithic Materials for the Analysis of Protein Phosphorylation

3.14.1 Introduction

3.14.2 Phosphopeptide Enrichment by Nanomaterials and Nanostructured Materials

3.14.3 Phosphopeptide Enrichment by Magnetic Materials

3.14.4 Phosphopeptide Enrichment by Monolithic Capillary Column

3.14.5 Phosphopeptide Enrichment by Other New Adsorbents

3.14.6 Conclusions and Perspectives

Acknowledgments

See also

REFERENCES

3.15. Sample Preparation for Glycoproteins

3.15.1 Introduction

3.15.2 Preparation of Total Proteins

3.15.3 Extraction and Enrichment of Glycoproteins

3.15.4 Digestion of Glycoproteins

3.15.5 Separation of Glycopeptides and Glycans

3.15.6 Cleavage and Derivatization of Glycans

3.15.7 Perspectives

See also

REFERENCES

3.16. Sample Preparation for Single-Molecule Enzyme Assays

3.16.1 Introduction

3.16.2 Use of CE for Single-Molecule Enzymology

3.16.3 Other Methodologies Used in Single-Molecule Enzymology

3.16.4 Enzyme Heterogeneity

3.16.5 Choice of Enzyme

3.16.6 Enzyme Source

3.16.7 Purification and Handling of the Enzyme

3.16.8 Modification of the Enzyme

3.16.9 Enzyme Concentration

3.16.10 Choice of Substrate

3.16.11 Purification of Substrate Prior to Assay

3.16.12 Optimum Buffer pH and Substrate Concentration

3.16.13 Choice of Capillary

3.16.14 Molecular Biology

See also

REFERENCES

Relevant Websites

3.17. Sampling and Sample Preparation for LC-MS-Based Metabonomics/Metabolomics of Samples of Mammalian Origin

3.17.1 Overview

3.17.2 Sampling Issues

3.17.3 The Preparation of Quality-Control samples

3.17.4 Sample Preparation for Different Types of Sample

3.17.5 Conclusions

See also

REFERENCES

Relevant Websites

3.18. Tissue, Serum and Saliva Sampling for Proteomic Analysis

3.18.1 Introduction

3.18.2 Tissue Samples

3.18.3 Serum and Plasma

3.18.4 Saliva Sampling for Proteomic Analysis

See also

REFERENCES

Chemical Speciation, Bioavailability, Toxicology

3.19. Pre-concentration and Sample Treatment Techniques for Trace Element Analysis

3.19.1 The Significance of Trace Element Analysis in Biological and Medical Samples

3.19.2 Analytical Techniques for Trace Element Analysis in Biological and Medical Samples

3.19.3 Sample Preparation Techniques for Biological and Medical Applications

3.19.4 Conclusion

See also

REFERENCES

3.20. Enzyme Treatment of Biological Samples for Speciation

3.20.1 Introduction

3.20.2 Sample Preparation Requirements in Species-Selective Determinations: The Need for the Preservation of the Analytes

3.20.3 Enzymatic Sample Preparation in Arsenic Speciation

3.20.4 Enzymatic Sample Preparation in Tin, Lead and Mercury Speciation

3.20.5 Analytical Approaches Targeting Specific Groups of Species

3.20.6 Bioavailability/Bioaccessibility Studies: The Use of Simulated Gastric and Gastrointestinal Digestion

See also

REFERENCES

3.21. Enzyme Digestion for Speciation of Arsenic

3.21.1 Introduction

3.21.2 Arsenic Species in Biological Systems

3.21.3 Challenges of Arsenic Speciation in Biological Samples

3.21.4 Current Methods for Extraction of Arsenic from Biological Samples

3.21.5 Enzyme Digestion for Extraction of Arsenic from Biological Samples

3.21.6 Conclusions

See also

REFERENCES

3.22. Mercury Speciation and Binding to Biomacromolecules

3.22.1 Introduction

3.22.2 Sample Preparation for Mercury Speciation

3.22.3 Speciation Analysis of Mercury

3.22.4 Binding of Mercury Species with Biomacromolecules

3.22.5 Conclusions

See also

REFERENCES

3.23. Determination of Cadmium Species Including Complexes with Metallothionein and Phytochelatin

3.23.1 Significance of Cd Speciation

3.23.2 The State-of-the-Art of Cd Speciation

3.23.3 Cd Binding to MTs

3.23.4 Cd Binding to PCs

3.23.5 Outlook on Speciation of Cd

See also

REFERENCES

Relevant Website

3.24. Bioaccessibility Extractions for Contaminant Risk Assessment

3.24.1 Introduction

3.24.2 Development of Bioaccessibility Methods

3.24.3 Bioaccessibility Models

3.24.4 Method Variables Influencing Bioaccessibility

3.24.5 Validation of Bioaccessibility Extractions

3.24.6 Summary and Recommendations

See also

REFERENCES

Relevant Websites

Recent Development in Sample Preparation Techniques for Biomedical/Biological Applications

3.25. Application of SPME to Pharmacodynamics, Pharmacokinetics, and Toxicology

3.25.1 Introduction: Challenges in Sample Preparation for Pharmacodynamics, Pharmacokinetics, and Toxicology

3.25.2 Analytical Methods Used with SPME for Bioanalytical Applications

3.25.3 Applications

3.25.4 Conclusions

See also

REFERENCES

3.26. Electrospun Nanofiber-Based Solid-Phase Microextraction Media

3.26.1 Introduction

3.26.2 Analysis of BTEX Compounds by Electrospun SPME

3.26.3 Analysis of Pharmaceutical Pollutants

3.26.4 Conclusions

Acknowledgment

See also

REFERENCES

Relevant Website

Environmental Applications

3.27. Sorbent-Phase Sample Preparation in Environmental Analysis

3.27.1 Introduction

3.27.2 SPE

3.27.3 SPME

3.27.4 In-Tube SPME

3.27.5 SBSE

3.27.6 MSPD

3.27.7 Miscellaneous

3.27.8 Conclusion and Outlook

REFERENCES

Relevant Websites

3.28. Recent Advances in Sample Preparation for Pesticide Analysis

3.28.1 Introduction

3.28.2 General Considerations

3.28.3 Extraction Approaches

3.28.4 Conclusions and Future Perspectives

Acknowledgments

See also

REFERENCES

Relevant Websites

3.29. Membrane-Based Extraction for Environmental Analysis

3.29.1 Introduction

3.29.2 Membrane Extraction for Organic Trace Analysis in Environmental Water Samples

3.29.3 Membrane Extraction for Solid Samples

3.29.4 Membrane Extraction for Air and Aerosol Samples

3.29.5 Conclusions

See also

REFERENCES

3.30. Chemical Warfare Agents: Development and Applications of Sample Preparation Approaches

3.30.1 Introduction

3.30.2 General Considerations on Sample Preparation of CWAs and Related Substances from Different Sample Matrices

3.30.3 Sample Preparation Methodologies for CWAs

3.30.4 Conclusion and Outlook

See also

REFERENCES

Relevant Websites

3.31. Sample Pretreatment Techniques for Perfluorinated Compounds

3.31.1 Overview of Perfluorinated Compounds

3.31.2 Analysis Techniques for PFCs

3.31.3 Sample Pretreatment Techniques for PFCs

3.31.4 Current Challenges

3.31.5 Future Trends

Acknowledgments

See also

REFERENCES

Relevant Websites

3.32. Recent Advances in Solid-Phase Microextraction for Environmental Applications

3.32.1 Introduction

3.32.2 SPME Fiber Coatings

3.32.3 New SPME Devices

3.32.4 SPME Derivatization

3.32.5 Applications

3.32.6 Conclusion

See also

REFERENCES

Relevant Websites

3.33. Environmental Applications of Cloud-Point Extraction

3.33.1 Introduction

3.33.2 Concept and Theory of CPE

3.33.3 Applications of CPE

3.33.4 Conclusions

See also

REFERENCES

Relevant Websites

3.34. Sample Preparation of Complex Biological Samples in the Analysis of Trace-Level Contaminants

3.34.1 Introduction

3.34.2 Applications of Solid-Phase Microextraction

3.34.3 Applications of Stir Bar Sorptive Extraction

3.34.4 Applications of Liquid-Phase Microextraction

3.34.5 Applications of Electromembrane Extraction

3.34.6 Applications of Solid-Phase Extraction

3.34.7 Applications of Molecularly Imprinted Polymers

3.34.8 Analytical Methods for Complex Biological Solid Samples

3.34.9 Conclusions

Acknowledgments

See also

REFERENCES

3.35. Sample Preparation for Capillary Electrophoretic Applications

3.35.1 Capillary Electrophoresis

3.35.2 Extraction Techniques for CE

3.35.3 Applications in Environmental Analysis

3.35.4 Conclusions and Future Prospects

See also

REFERENCES

Relevant Websites

3.36. Sample Preparation of Microbial Contaminants in Water

3.36.1 Introduction

3.36.2 Preconcentration Techniques for Microbial Analysis

3.36.3 Pretreatment for Detecting Viable Microorganisms in Water by Molecular Techniques

3.36.4 Conclusions

REFERENCES

3.37. Inorganic Contaminants: Sample Preparation Approaches

3.37.1 Introduction

3.37.2 Sample Preparation and Pretreatment Procedures

3.37.3 Extraction of Inorganic Contaminants

3.37.4 Determination of Heavy Metals in Environmental Samples

3.37.5 Determination of Heavy Metals in Forensic Samples

3.37.6 Conclusions

Acknowledgments

See also

REFERENCES

Relevant Websites

3.38. Advances in Sample Preparation of Environmental Solid Matrices

3.38.1 Introduction

3.38.2 Most Popular Techniques and Recent Developments

3.38.3 Matrices and Common Analytes in Environmental Analysis

3.38.4 Most Common Analytes

See also

REFERENCES

Relevant Websites

3.39. Environmental and Biological Applications of Stir Bar Sorptive Extraction

3.39.1 Introduction

3.39.2 Theory

3.39.3 SBSE Tools

3.39.4 Instrumentation

3.39.5 Technical Aspects

3.39.6 Applications

3.39.7 Conclusions

See also

REFERENCES

Relevant Website

3.40. Sample Preparation for Food Contaminant Analysis

3.40.1 Introduction

3.40.2 Food as a Matrix

3.40.3 Extraction of Solid Samples

3.40.4 Extraction of Liquid Samples

3.40.5 Microextraction Methods

3.40.6 Headspace Analysis

3.40.7 Conclusions and Future Trends

See also

REFERENCES

Relevant Websites

3.41. Liquid-Based Microextraction Techniques for Environmental Analysis

3.41.1 Introduction

3.41.2 Liquid-Based Microextraction Techniques

3.41.3 Solvents Used in Liquid-Based Microextraction Techniques

3.41.4 Instruments Combined with Liquid-Based Microextraction Techniques for Environmental Analysis

3.41.5 Chemical Reactions in Liquid-Based Microextraction

3.41.6 Experimental Parameters Affecting Extraction Efficiency

3.41.7 Environmental Applications of Liquid-Based Microextraction Techniques

3.41.8 Developmental Trend

Acknowledgments

See also

REFERENCES

Forensic Applications

3.42. Sample Preparation for Chromatographic Applications in Forensic Science

3.42.1 Introduction

3.42.2 Examples of Forensic Samples Requiring Chromatography

3.42.3 Processes for Sample Preparation

3.42.4 Addition of Internal Standards during Sample Preparation

3.42.5 Factors that Govern the Extent of Sample Preparation Required

3.42.6 Sample Preparation for Metals by Ion Chromatography or GC/LC Coupled to Inductively Coupled Plasma Mass Spectrometry

3.42.7 Sample Preparation for Stable Isotope Ratio

3.42.8 Sample Volume

3.42.9 Automated Sample Preparation

3.42.10 Examples of Future Challenges in Sample Preparation

3.42.11 Conclusion – Don’t Reinvent the Wheel

See also

REFERENCES

Relevant Websites

3.43. Recent Advances in Solid-Phase Microextraction for Forensic Applications

3.43.1 Recent Advances in Solid-Phase Microextraction

3.43.2 Applications of SPME in Forensic Toxicology

3.43.3 Vitreous Humor and Related Postmortem Specimens

3.43.4 Applications of SPME for Drug Profiling

3.43.5 Applications of SPME for Chemical Warfare Agents

3.43.6 Applications of SPME for the Recovery of Explosives and Ignitable Liquid Residues

3.43.7 Applications of SPME for Determining Time Since Discharge of Spent Cartridges

3.43.8 Applications of SPME for the Identification of Human Scent Volatile Chemical Signatures

Conclusions

REFERENCES

Relevant Websites

3.44. Recent Advances in Sample Preparation for Explosives

3.44.1 Overview and Introduction

3.44.2 Chemistry of Explosives

3.44.3 Sample Types

3.44.4 Extraction Techniques for Explosives and Related Compounds

3.44.5 Conclusions

Acknowledgments

REFERENCES

New Directions in Sample Preparation for Environmental Analysis

3.45. Needle-Trap Devices for Environmental Sample Preparation

3.45.1 Introduction

3.45.3 Simultaneous Derivatization/Extraction of Air Samples with Fiber-Packed Sample Preparation Devices

3.45.4 Sample Preparation of Water Samples with a Fiber-Packed Needle Device

3.45.5 Future Prospects and Potential Applications of Needle Extraction Techniques

See also

REFERENCES

3.46. Use of Unconventional Solvents for Sample Preparation in Environmental Analysis

3.46.1 Introduction

3.46.2 Liquid-Liquid Extraction (LLE)

3.46.3 Dispersive Liquid-Liquid Microextraction (DLLME)

3.46.4 Liquid-Phase Microextraction (LPME)/Single Drop Microextraction (SDME)

3.46.5 Hollow-Fiber Protected Liquid-Phase Microextraction (HF-LPME)

3.46.6 Supercritical Fluid Extraction (SFE)

3.46.7 Subcritical Water Extraction (SWE)

3.46.8 Summary

See also

REFERENCES

Relevant Websites

3.47. Preparative Gas Chromatography as a Sample Preparation Approach

3.47.1 Introduction

3.47.2 Conventional Preparative GC

3.47.3 General Description of Multidimensional GC/Multidimensional Chromatography

3.47.4 Comprehensive Two-Dimensional Chromatography

3.47.5 Selected Applications

3.47.6 Conclusions

See also

REFERENCES

Relevant Websites

VOLUME 4. Extraction Technqiues and Applications: Food and Beverage

Food Constituents: Volatiles

4.01. Headspace Sampling in Flavor and Fragrance Field

4.01.1 Introduction

4.01.2 Flavor, Fragrances, and Plant Volatile Fraction: Some Definitions

4.01.3 Analysis of Flavor and Fragrance Composition

4.01.4 Headspace Sampling: Definitions

4.01.5 Headspace Sampling: History and Present Evolution

4.01.6 Static Headspace

4.01.7 Dynamic Headspace

4.01.8 Static and Trapped Headspace

4.01.9 High Concentration Capacity Headspace Techniques (HCC-HS)

4.01.10 Headspace and Volatile Quantitation

4.01.11 Concluding Remarks

See also

REFERENCES

4.02. Sampling Techniques for the Determination of Volatile Components in Grape Juice, Wine and Alcoholic Beverages

4.02.1 Chemistry of Volatile Components of Grape Juice, Wine, and Alcoholic Beverages

4.02.2 Extraction Techniques

Acknowledgments

REFERENCES

Relevant Websites

4.03. Sampling and Sample Preparation Techniques for the Determination of the Volatile Components of Milk and Dairy Products

4.03.1 Flavor Constituents of Milk and Dairy Products

4.03.2 Applications

See also

REFERENCES

Relevant Website

4.04. Sampling Techniques for the Determination of Volatile Components in Food of Animal Origin

4.04.1 Flavor in Food of Animal Origins

4.04.2 Off-Flavor in Food of Animal Origins

4.04.3 Sample-Preparation Techniques for the Determination of Volatile Components in Meat and Meat Products

4.04.4 Sample-Preparation Techniques for the Determination of Volatile Components in Fish and Fish Products

4.04.5 Conclusions and Future Trends

See also

REFERENCES

4.05. Sampling Techniques for the Determination of the Volatile Fraction of Honey

4.05.1 Honey Volatiles

4.05.2 Extraction Techniques

4.05.3 E-nose

4.05.4 Conclusion

See also

REFERENCES

4.06. Sample Preparation for Food Flavor Analysis (Flavors/Off-Flavors)

4.06.1 Specificity of Food Flavor/Off-Flavor Analysis

4.06.2 Strategies for Flavor Compound Analysis

4.06.3 Methods for Isolation and Analysis of Free Flavor Compounds

4.06.4 Methods for Isolation of Volatile Compounds for Gas Chromatography–Olfactometry

4.06.5 Methods for Isolation of Volatile Compounds for Electronic Noses

4.06.6 Methods for Isolation and Analysis of Bound Flavor Compounds

4.06.7 Conclusions

See also

REFERENCES

Relevant Websites

4.07. In Vivo Sampling of Flavor Components

4.07.1 Introduction

4.07.2 The Nature of Flavor and the Sampled Subject

4.07.3 Techniques and Devices to Sample the Headspace

4.07.4 Applications

4.07.5 Conclusions

See also

REFERENCES

Relevant Websites

Food Constituents: Non-Volatiles or Semivolatiles

4.08. Extraction Techniques for the Determination of Phenolic Compounds in Food

4.08.1 Introduction

4.08.2 Types and Distribution of Phenolic Compounds in Foods

4.08.3 Factors Affecting the Phenolics Content in Foods

4.08.4 Extraction of Phenolic Compounds from Food

4.08.5 Conclusions

Acknowledgments

See also

REFERENCES

Relevant Websites

4.09. Extraction Techniques for the Determination of Carotenoids and Vitamins in Food

4.09.1 Introduction

4.09.2 Extraction of Carotenoids from Food

4.09.3 Extraction of Vitamins from Food

4.09.4 Conclusions and Future Outlook

Acknowledgments

See also

REFERENCES

Relevant Websites

4.10. Sample Preparation Techniques for the Determination of Fats in Food

4.10.1 Introduction

4.10.2 Soxhlet and Improved Soxhlet Devices

4.10.3 Classical Solvent Extraction: Folch Method, and Bligh and Dyer Method

4.10.4 Microwave-Assisted Extraction

4.10.5 Supercritical Fluid Extraction

4.10.6 Accelerated Solvent Extraction (ASE) or Pressurized Liquid Extraction (PLE) of Fats

4.10.7 Concluding Remarks

Acknowledgments

See also

REFERENCES

Relevant Websites

4.11. Sample Preparation for the Determination of Carbohydrates in Food and Beverages

4.11.1 Introduction

4.11.2 Sampling

4.11.3 Sample Treatments

4.11.4 Basic Sample Types

See also

REFERENCES

Relevant Websites

Food Additives and Contaminants

4.12. Solvent-Based Extraction Techniques for the Determination of Pesticides in Food

4.12.1 Introduction

4.12.2 Liquid Extraction Techniques

4.12.3 Energy-Assisted Liquid Extraction Techniques

4.12.4 Conclusions

See also

REFERENCES

4.13. Sorbent-Based Techniques for the Determination of Pesticides in Food

4.13.1 Introduction

4.13.2 Solid-Phase Extraction

4.13.3 Solid-Phase Microextraction

4.13.4 Stir-Bar Sorptive Extraction

4.13.5 Matrix Solid-Phase Dispersion

4.13.6 Conclusions and Future Trends

Acknowledgment

See also

REFERENCES

Relevant Websites

4.14. Sample Preparation Techniques for the Determination of Some Food Contaminants (Polycyclic Aromatic Hydrocarbons, Mineral Oils and Phthalates)

4.14.1 Introduction

4.14.2 Polycyclic Aromatic Hydrocarbons

4.14.3 Mineral Oil

4.14.4 Phthalates

See also

REFERENCES

Relevant Websites

4.15. Sampling Techniques for the Determination of Migrants from Packaging Materials in Food

4.15.1 Introduction

4.15.2 Migration into Food Simulants

4.15.3 Migration into Foods

4.15.4 Overall Conclusions

See also

REFERENCES

4.16. Sampling Techniques for the Determination of Mycotoxins in Food Matrices

4.16.1 Introduction

4.16.2 Sampling Strategies for Mycotoxin Analysis

4.16.3 Sample Extraction and Cleanup

4.16.4 Milk and Dairy Products

4.16.5 Botanicals, Spices and Herbs

4.16.6 Fruit, Juices and Puree

4.16.7 Meat Products

4.16.8 Coffee and Cocoa

4.16.9 Wine

4.16.10 Cereals

4.16.11 Dried Fruits and Nuts

4.16.12 Conclusions

See also

REFERENCES

Relevant Websites

4.17. Sample Preparation Techniques for the Determination of Veterinary Drugs in Food Matrices

4.17.1 Veterinary Drugs and Food Matrices

4.17.2 Analysis Routines

4.17.3 Screening Methods

4.17.4 Single Analyte Methods

4.17.5 Multi-Class/Multi-Residue Sampling and Analysis

See also

REFERENCES

New Technologies in Food Applications

4.18. Application of Supercritical Fluid Extraction in Food Processing

4.18.1 Introduction

4.18.2 Extraction of Lipids and Lipid-Soluble Components

4.18.3 Extraction of Polar Nutraceuticals

4.18.4 Inactivation of Microorganisms in Foods and Beverages

4.18.5 Scale-Up and Industrial Applications

4.18.6 Future Considerations of Supercritical CO2 Food and Beverage Processing

See also

REFERENCES

Relevant Websites

4.19. Accelerated Methods for Sample Preparation in Food

4.19.1 Introduction

4.19.2 Microwave-Assisted Extraction

4.19.3 Ultrasound-Assisted Extraction

4.19.4 The Instant Controlled Pressure Drop (DIC) Technology

4.19.5 Pressurized Fluid Extraction

4.19.6 Comparison of Sample Preparation Techniques

4.19.7 Future Trends

See also

REFERENCES

Relevant Websites

4.20. Applications of SPE-MIP in the Field of Food Analysis

4.20.1 Introduction

4.20.2 Molecularly Imprinted Polymers

4.20.3 MI-SPE in Food Analysis

4.20.4 Conclusions

REFERENCES

Relevant Websites

4.21. Application of Stir-Bar Sorptive Extraction in Food Analysis

4.21.1 Introduction

4.21.2 Fundamentals

4.21.3 Practical Considerations When Using SBSE for Food Applications

4.21.4 Applications

4.21.5 Conclusion

See also

REFERENCES

Relevant Websites

4.22. Sample Preparation for the Determination of Metals in Food Samples

4.22.1 Introduction

4.22.2 Sampling

4.22.3 Drying of Samples

4.22.4 Homogenization

4.22.5 Causes of Contamination

4.22.6 Purity of the Reagents

4.22.7 Digestion Methods

4.22.8 Ultrasonic Extraction

4.22.9 Direct Analysis of Solid Samples

4.22.10 Conclusion

See also

REFERENCES

Relevant Websites

4.23. Membrane-Based Extraction Techniques in Food Analysis

4.23.1 Introduction

4.23.2 Membrane Separation for Direct Analysis of Complex Mixtures

4.23.3 Conclusions

See also

REFERENCES

4.24. Sample Preparation for Direct MS Analysis of Food

4.24.1 General Considerations

4.24.2 Sample Preparation for GC-MS Analysis of Selected Food Matrices

4.24.3 Direct MS Analysis of Volatile Compounds

4.24.4 Sample Preparation for Direct MS Analysis of Selected Food Matrices

4.24.5 SPME GC-MS Method Performance Evaluation in Food Analysis

See also

REFERENCES

Index

 
 
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