Comprehensive Sampling and Sample Preparation

Analytical Techniques for Scientists

1st Edition - June 1, 2012
Editors: Josep M. Bayona, Janusz Pawliszyn, Paola Dugo, X. Chris Le, Hian Kee Lee, Xing-Fang Li, Heather Lord
Language: English
eBook ISBN:
9 7 8 - 0 - 1 2 - 3 8 1 3 7 4 - 9

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 preparati… Read more

Purchase options

LIMITED OFFER

Save 50% on book bundles

Immediately download your ebook while waiting for your print delivery. No promo code is needed.

Institutional subscription on ScienceDirect

Request a sales quote

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.

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

Josep M. Bayona

Josep M. Bayona, BSc, PhD in Chemistry in 1985 at the Autonomous University of Barcelona, Research Professor at the Institute of Environmental Assessment and Water Research (IDAEA) from the Consejo Superior de Investigaciones Científicas (CSIC) in Barcelona (Spain). His main research interests are the Environmental Chemistry focusing on the transformation processes and the pathway of organic contaminants in the environment and engineered ecosystems. He has been appointed Member of the National Committee to cope with the ecological emergency in the Doñana, National Park 1997-1999, Steering Committee of the Catalan Society of Chemistry (2002-2004), GESAMP (Group of Experts on the Scientific Aspects of Marine Pollution) membership 2008. He was editor of the Analytical Chemistry A pages (2003-2005) and currently member of the editorial board of the International Journal of Environmental Chemistry. He is coauthor of 240 publications in peer-reviewed journals, 35 book chapters, H index 29 and 2900 citations.

Affiliations and expertise

International Journal of Environmental Chemistry

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

Paola Dugo

Paola Dugo is full professor of Food Chemistry at the University of Messina and at the "Campus Biomedico" in Rome. She received a degree in chemistry from the University of Messina and a Ph.D. in Pharmacognosy. Her research interests are vast, including the development of comprehensive chromatography and high throughput separation methods, applied to the study of the composition of citrus products (essential oils and juices); components with possible biological activity in natural matrices (carotenoids, anthocyanins, coumarins); essential oils from aromatic plants; the aromatic fraction of wine and other alcoholic beverages; triglycerides in food fats and oils.

Prof. Dugo is the author of approximately 130 scientific papers, and she has been speaker in national and international congresses and symposia. Moreover, her scientific activity includes invited article, book chapters and invited review articles for international journals, the collaboration for the preparation of the on-line encyclopedia Chromedia. She is member of the editorial board of international scientific journals, Journal of chromatography A and Flavour and Fragrance Journal.

Affiliations and expertise

Full professor of Food Chemistry at the University of Messina

X. Chris Le

Dr. X. Chris Le is an analytical and environmental chemist studying the effects of environmental contaminants on human health. His research team develops highly sensitive techniques and assays that enable studies of human exposure to environmental toxicants. His collaborative work on the determination of arsenic species, assays for trace levels of proteins and DNA damage, and new approaches to detection of these targets have enabled novel toxicological and biological studies. His research has resulted in better detection of environmental contaminants and greater understanding of their health effects.

Dr. Le is Distinguished University Professor, jointly appointed in the Departments of Laboratory Medicine and Pathology, Chemistry, and Public Health Sciences at the University of Alberta (Canada). He holds an inaugural Canada Research Chair in Bio-Analytical Technology and Environmental Health since 2001. He is an elected Fellow of the Royal Society of Canada, Academy of Science, and a Fellow of Chemical Institute of Canada. He has received the following awards that recognize his contributions to both teaching and research: Award for Excellence in Mentoring (2009) and Martha Cook Piper Research Prize (2000) from the University of Alberta; E.W.R. Steacie Fellowship from the Natural Sciences and Engineering Research Council of Canada (2000); W.A.E. McBryde Medal (2002), Maxxam Award (2011), and Environment Research and Development Award (2011) from the Canadian Society for Chemistry.

Affiliations and expertise

Distinguished University Professor, Departments of Laboratory Medicine and Pathology, Chemistry, and Public Health Sciences, University of Alberta (Canada).

Hian Kee Lee

Hian Kee Lee is Professor in the Department of Chemistry, National University of Singapore (NUS). He obtained his B.Sc. (Honours) and Ph.D. degrees from the University of Canterbury, New Zealand. His research interests are focused on the development of microscale sample preparation techniques, and microscale separation science and environmental and bio-analytics. Specifically, his work is centred on developing and applying liquid-phase microextraction procedures. Professor Lee was an Editor of Analytica Chimica Acta from 2006-2011, and was a member of the editorial board of the Journal of Chromatography A from 2005-2010. He has also served as an editorial advisor for Analytica Chimica Acta (2003-2005), and as an international advisory board member of the Analyst (1997-2008). He is currently an Editor of the Journal of Chromatography A. He is a current scientific advisory board member of Analytical Sciences, an editorial advisory board member of LC•GC Europe and LC•GC Asia Pacific, and a member of the scientific advisory board of Separation Science, a web-based journal that runs the annual Separation Science Asia Symposium in Singapore. He is a co-contributor (on liquid-phase microextraction) to the web-based separation science resource, Chromedia. Professor Lee is the co-chairman of the engineering, physical and chemical sciences cluster of NUS' University Research Committee, a member of the university's Cross-Faculty Research Committee that fosters multidisciplinary research across different faculties, and was also a member of the University Promotion and Tenure Committee from 2007 to 2009. He has served as deputy head and head of his department. He is a member of the executive committee of the NUS Environmental Research Institute. He is a member of the international audit panel of Singapore's Water Reclamation and Desalination programme. He was a recipient of the NUS Outstanding Research Award (2006), the university's Faculty of Science Outstanding Scientist Award (2009), and the Federation of Asian Chemical Societies Foundation Lectureship Award (2009). He is a co-editor of the present Comprehensive Sampling and Sample Preparation monograph.

Affiliations and expertise

Professor in the Department of Chemistry, National University of Singapore (NUS).

Xing-Fang Li

Dr. Xing-Fang Li is a Professor at the University of Alberta (Canada) with cross appointment in the Faculty of Medicine and Dentistry and in the School of Public Health. She is the recipient of 2010 W.A.E. McBryde Medal from the Canadian Society for Chemistry, recognizing her significant achievement in pure or applied analytical chemistry. She currently serves as the Vice-Chair for Environmental Chemistry Division of the Canadian Society for Chemistry. Her diverse research deals with analytical technology development and detection of microbial pathogens, proteins, chemotherapeutics, and water contaminants. She leads two international collaborative projects on studies of microbial pathogens in water and on drinking water disinfection byproducts. Her research team develops new methods for selection of DNA aptamers binding to microbial cells, determines viable but non-culturable microbial organisms, studies molecular interactions using mass spectrometry, identifies new drinking water disinfection byproducts, and studies toxicity of contaminants significant to human health.

Dr. Li received B.Sc. (1983) in Chemistry from Hangzhou University, M.Sc. (1986) in Environmental Chemistry from the Research Centre for Eco-Environmental Sciences, Chinese Academy of Sciences, M.Sc. (1990) in Analytical Chemistry from Brock University, and Ph.D. (1995) in Environmental/Analytical Chemistry from the University of British Columbia, Canada. Dr. Li is a guest professor at the Research Center for Eco-Environmental Sciences (Chinese Academy of Sciences), Southwest University, and Zhejiang University.

Affiliations and expertise

Professor at the University of Alberta (Canada)

Heather Lord

Heather Lord is a Research Associate in the group of Professor Pawliszyn with experience in analytical device and method development, sorbent design, and solid phase sample preparation. She has authored over 40 scientific papers in biochemical toxicology and bioanalytical method development. Her primary research interests are in the areas of in vivo sample preparation and new bioanalytical methods development.