Bioanalysis of Pharmaceuticals
Sample Preparation, Separation Techniques and Mass Spectrometry
1st Edition
Published on 17. July 2015
Book
Paperback/Softback
336 pages
978-1-118-71682-3 (ISBN)
Description
Bioanalysis of Pharmaceuticals: Sample Preparation, Separation Techniques and Mass Spectrometry is the first student textbook on the separation science and mass spectrometry of pharmaceuticals present in biological fluids with an educational presentation of the principles, concepts and applications. It discusses the chemical structures and properties of low- and high-molecular drug substances; the different types of biological samples and fluids that are used; how to prepare the samples by extraction, and how to perform the appropriate analytical measurements by chromatographic and mass spectrometric methods.
Bioanalysis of Pharmaceuticals: Sample Preparation, Separation Techniques and Mass Spectrometry:
Is an introductory student textbook discussing the different principles and concepts clearly and comprehensively, with many relevant and educational examples
Focuses on substances that are administered as human drugs, including low-molecular drug substances, peptides, and proteins
Presents both the basic principles that are regularly taught in universities, along with the practical use of bioanalysis as carried out by researchers in the pharmaceutical industry and in hospital laboratories
Is aimed at undergraduate students, scientists, technicians and researchers in industry working in the areas of pharmaceutical analyses, biopharmaceutical analyses, biological and life sciences
The book includes multiple examples to illustrate the theory and application, with many practical aspects including calculations, thus helping the student to learn how to convert the data recorded by instruments into the real concentration of the drug substances within the biological sample.
Bioanalysis of Pharmaceuticals: Sample Preparation, Separation Techniques and Mass Spectrometry:
Is an introductory student textbook discussing the different principles and concepts clearly and comprehensively, with many relevant and educational examples
Focuses on substances that are administered as human drugs, including low-molecular drug substances, peptides, and proteins
Presents both the basic principles that are regularly taught in universities, along with the practical use of bioanalysis as carried out by researchers in the pharmaceutical industry and in hospital laboratories
Is aimed at undergraduate students, scientists, technicians and researchers in industry working in the areas of pharmaceutical analyses, biopharmaceutical analyses, biological and life sciences
The book includes multiple examples to illustrate the theory and application, with many practical aspects including calculations, thus helping the student to learn how to convert the data recorded by instruments into the real concentration of the drug substances within the biological sample.
More details
Language
English
Place of publication
New York
United States
Target group
Professional and scholarly
Dimensions
Height: 244 mm
Width: 244 mm
Thickness: 18 mm
Weight
522 gr
ISBN-13
978-1-118-71682-3 (9781118716823)
Copyright in bibliographic data and cover images is held by Nielsen Book Services Limited or by the publishers or by their respective licensors: all rights reserved.
Schweitzer Classification
Other editions
Additional editions
Steen Hansen | Stig Pedersen-Bjergaard
Bioanalysis of Pharmaceuticals
Sample Preparation, Separation Techniques and Mass Spectrometry
E-Book
10/2015
Wiley
€52.99
Available for download
Steen Honore Hansen | Stig Pedersen-Bjergaard
Bioanalysis of Pharmaceuticals
Sample Preparation, Separation Techniques and Mass Spectrometry
Book
07/2015
Wiley-Blackwell
€154.50
Article exhausted; check different version
Steen Hansen | Stig Pedersen-Bjergaard
Bioanalysis of Pharmaceuticals
Sample Preparation, Separation Techniques and Mass Spectrometry
E-Book
05/2015
Wiley
€52.99
Available for download
Persons
Steen Honore Hansen
Department of Pharmacy, Faculty of Health and Medical Sciences, Copenhagen University, Denmark
Stig Pedersen-Bjergaard
School of Pharmacy, University of Oslo, Norway, and Department of Pharmacy, Faculty of Health and Medical Sciences, Copenhagen University, Denmark
Department of Pharmacy, Faculty of Health and Medical Sciences, Copenhagen University, Denmark
Stig Pedersen-Bjergaard
School of Pharmacy, University of Oslo, Norway, and Department of Pharmacy, Faculty of Health and Medical Sciences, Copenhagen University, Denmark
Content
Contributing Authors ix Preface xi
1. Introduction 1
Stig Pedersen-Bjergaard
1.1 What Is Bioanalysis? 1
1.2 What Is the Purpose of Bioanalysis, and Where Is It Conducted? 2
1.3 Bioanalysis Is Challenging 6
1.4 The Different Sections of This Textbook 7
2. Physicochemical Properties of Drug Substances 9
Steen Honore Hansen and Leon Reubsaet
2.1 Bioanalysis in General 9
2.2 Protolytic Properties of Analytes 10
2.3 Partitioning of Substances 12
2.4 Stereochemistry 15
2.5 Peptides and Proteins 18
3. Biological Samples: Their Composition and Properties, and Their Collection and Storage 23
Steen Honore Hansen
3.1 Introduction 23
3.2 Blood, or Whole Blood 24
3.3 Plasma and Serum 26
3.4 Urine 26
3.5 Feces 27
3.6 Saliva 28
3.7 Cerebrospinal Fluid 28
3.8 Synovial Fluid 28
3.9 Hair and Nails 29
3.10 Tissue (Biopsies) 29
4. General Chromatographic Theory and Principles 31
Steen Honore Hansen
4.1 General Introduction 31
4.2 General Chromatographic Theory 32
4.3 Theory of Partition 33
4.4 Retention 34
4.5 Separation Efficiency 35
4.6 Resolution 36
4.7 Selectivity 37
4.8 The Separation Process 38
4.9 Chromatographic Principles 41
4.10 Reversed Phase Chromatography 45
4.11 Size Exclusion Chromatography (SEC) 54
4.12 Ion Exchange Chromatography 56
4.13 Chiral Separations 57
5. Quantitative and Qualitative Chromatographic Analysis 61
Steen Honore Hansen
5.1 Collection of Chromatographic Data 61
5.2 Quantitative Measurements 62
5.3 Calibration Methods 63
5.4 Validation 67
5.5 Qualitative Analysis 69
6. Sample Preparation 73
Stig Pedersen-Bjergaard, Astrid Gjelstad, and Trine Gronhaug Halvorsen
6.1 Why Is Sample Preparation Required? 73
6.2 What Are the Main Strategies? 75
6.3 Protein Precipitation 75
6.4 Liquid-Liquid Extraction 80
6.5 Solid-Phase Extraction 94
6.6 Dilute and Shoot 110
6.7 What Are the Alternative Strategies? 113
7. High-Performance Liquid Chromatography (HPLC) and High-Performance Liquid Chromatography-Mass Spectrometry (LC-MS) 123
Steen Honore Hansen and Leon Reubsaet
7.1 Introduction 123
7.2 The Solvent Delivery System 125
7.3 Degassing and Filtering of Mobile Phases 127
7.4 Injection of Samples 128
7.5 Temperature Control 128
7.6 Mobile Phases 129
7.7 Stationary Phases and Columns 130
7.8 Detectors 135
7.9 Mass Spectrometric Detection 143
8. Gas Chromatography (GC) 173
Stig Pedersen-Bjergaard
8.1 Basic Principles of GC 173
8.2 GC Instrumentation 174
8.3 Carrier Gas 177
8.4 Stationary Phases 178
8.5 Separation Selectivity in GC 180
8.6 Columns 182
8.7 Injection Systems 183
8.8 Detectors 185
8.9 Derivatization 187
8.10 Gas Chromatography-Mass Spectrometry (GC-MS) 188
9. Analysis of Small-Molecule Drugs in Biological Fluids 207
Steen Honore Hansen and Stig Pedersen-Bjergaard
9.1 Plasma and Serum Samples 207
9.2 Whole Blood Samples 234
9.3 Dried Blood Spots 241
9.4 Urine Samples 245
9.5 Saliva 253
References 259
10. Analysis of Peptide and Protein Drugs in Biological Fluids 261
Leon Reubsaet and Trine Gronhaug Halvorsen
References 282
11. Regulated Bioanalysis and Guidelines 283
Martin Jorgensen and Morten A. Kall
11.1 Introduction 283
11.2 The Evolution of Regulated Bioanalysis 284
11.3 Bioanalytical Method Validation 286
11.4 Pre-study Validation 287
11.5 In-Study Validation 299
11.6 Documentation 300
11.7 Regulatory Requirements to Bioanalysis 300
11.8 Quality Systems in Regulated Bioanalysis 301
Index 305
1. Introduction 1
Stig Pedersen-Bjergaard
1.1 What Is Bioanalysis? 1
1.2 What Is the Purpose of Bioanalysis, and Where Is It Conducted? 2
1.3 Bioanalysis Is Challenging 6
1.4 The Different Sections of This Textbook 7
2. Physicochemical Properties of Drug Substances 9
Steen Honore Hansen and Leon Reubsaet
2.1 Bioanalysis in General 9
2.2 Protolytic Properties of Analytes 10
2.3 Partitioning of Substances 12
2.4 Stereochemistry 15
2.5 Peptides and Proteins 18
3. Biological Samples: Their Composition and Properties, and Their Collection and Storage 23
Steen Honore Hansen
3.1 Introduction 23
3.2 Blood, or Whole Blood 24
3.3 Plasma and Serum 26
3.4 Urine 26
3.5 Feces 27
3.6 Saliva 28
3.7 Cerebrospinal Fluid 28
3.8 Synovial Fluid 28
3.9 Hair and Nails 29
3.10 Tissue (Biopsies) 29
4. General Chromatographic Theory and Principles 31
Steen Honore Hansen
4.1 General Introduction 31
4.2 General Chromatographic Theory 32
4.3 Theory of Partition 33
4.4 Retention 34
4.5 Separation Efficiency 35
4.6 Resolution 36
4.7 Selectivity 37
4.8 The Separation Process 38
4.9 Chromatographic Principles 41
4.10 Reversed Phase Chromatography 45
4.11 Size Exclusion Chromatography (SEC) 54
4.12 Ion Exchange Chromatography 56
4.13 Chiral Separations 57
5. Quantitative and Qualitative Chromatographic Analysis 61
Steen Honore Hansen
5.1 Collection of Chromatographic Data 61
5.2 Quantitative Measurements 62
5.3 Calibration Methods 63
5.4 Validation 67
5.5 Qualitative Analysis 69
6. Sample Preparation 73
Stig Pedersen-Bjergaard, Astrid Gjelstad, and Trine Gronhaug Halvorsen
6.1 Why Is Sample Preparation Required? 73
6.2 What Are the Main Strategies? 75
6.3 Protein Precipitation 75
6.4 Liquid-Liquid Extraction 80
6.5 Solid-Phase Extraction 94
6.6 Dilute and Shoot 110
6.7 What Are the Alternative Strategies? 113
7. High-Performance Liquid Chromatography (HPLC) and High-Performance Liquid Chromatography-Mass Spectrometry (LC-MS) 123
Steen Honore Hansen and Leon Reubsaet
7.1 Introduction 123
7.2 The Solvent Delivery System 125
7.3 Degassing and Filtering of Mobile Phases 127
7.4 Injection of Samples 128
7.5 Temperature Control 128
7.6 Mobile Phases 129
7.7 Stationary Phases and Columns 130
7.8 Detectors 135
7.9 Mass Spectrometric Detection 143
8. Gas Chromatography (GC) 173
Stig Pedersen-Bjergaard
8.1 Basic Principles of GC 173
8.2 GC Instrumentation 174
8.3 Carrier Gas 177
8.4 Stationary Phases 178
8.5 Separation Selectivity in GC 180
8.6 Columns 182
8.7 Injection Systems 183
8.8 Detectors 185
8.9 Derivatization 187
8.10 Gas Chromatography-Mass Spectrometry (GC-MS) 188
9. Analysis of Small-Molecule Drugs in Biological Fluids 207
Steen Honore Hansen and Stig Pedersen-Bjergaard
9.1 Plasma and Serum Samples 207
9.2 Whole Blood Samples 234
9.3 Dried Blood Spots 241
9.4 Urine Samples 245
9.5 Saliva 253
References 259
10. Analysis of Peptide and Protein Drugs in Biological Fluids 261
Leon Reubsaet and Trine Gronhaug Halvorsen
References 282
11. Regulated Bioanalysis and Guidelines 283
Martin Jorgensen and Morten A. Kall
11.1 Introduction 283
11.2 The Evolution of Regulated Bioanalysis 284
11.3 Bioanalytical Method Validation 286
11.4 Pre-study Validation 287
11.5 In-Study Validation 299
11.6 Documentation 300
11.7 Regulatory Requirements to Bioanalysis 300
11.8 Quality Systems in Regulated Bioanalysis 301
Index 305