Detection of drugs at low concentration is required in a variety of biological and medical situations, in order to avoid harmful side effects posed by some drug residues. The book details the instrumentation, detection, and application of nano chromatography (that is, any chromatographic and capillary electrophoretic method dealing with the detection of a sample at nano gram per liter or lower) and capillary electrophoresis in the analyses of biological and environmental samples. Methods discussed include: Nano Gas Chromatography, Nano Capillary Electrophoresis, Nano Chiral Chromatography, Micellar Electrokinetic Chromatography, Supercritical Fluid Chromatography, and Nano High Performance Liquid Chromatography.

Imran Ali, PhD, is Associate Professor at the Department of Chemistry, Jamia Millia Islamia (Central University), New Delhi, India. Dr. Ali has published more than 150 scholarly works, including complete books, book and encyclopedia chapters, review articles, research papers, technical reports, and conference presentations.

Hassan Y. Aboul-Enein, PhD, is a Professor at Pharmaceutical and Medicinal Chemistry Department, Pharmaceutical and Drug Industries Research Division, National Research Centre, Dokki, Cairo, Egypt. He has published more than 600 articles, including several books and encyclopedia chapters.

Vinod K. Gupta is a Professor in the Department of Chemistry, Indian Institute of Technology, Roorkee, India. He has published more than 200 articles including book and encyclopedia chapters, review articles, research papers, technical reports, and conference presentations.

The latest tested and proven methods for detecting nanolevels of drugs and xenobiotics

Filling an important gap in the literature, this book enables you to successfully perform nanoanalyses using chip-based nanoliquid chromatography (NLC) and nanocapillary electrophoresis (NCE). The authors carefully guide readers through each stage of the instrumentation, detection, and applications of NLC and NCE in order to accurately identify compounds at a nanogram per liter or lower. This is the first book in the world describing NLC and NCE techniques in separation science.

Nanochromatography and Nanocapillary Electrophoresis begins with an introductory chapter that defines and sets forth a protocol for nanoanalyses. The chapters that follow guide you step by step through such important topics as:

• Fabrication of microchips

• Instrumentation, detection, and sample preparation in NLC and NCE

• Nano high-performance liquid chromatography

• Nanocapillary electrochromatography and nanomicellar electrokinetic chromatography

• Chiral separations by nanoliquid chromatography and nanocapillary electrophoresis

Throughout the book, the authors translate theory into practice, with examples of applications in materials science, nutrition, agriculture, chemistry, biology, and environmental science. Each chapter ends with a set of conclusions highlighting the most salient points as well as references to guide readers to the primary literature for further research.

This book equips readers with new, sophisticated tools to detect and analyze drugs and xenobiotics at nano levels. It is therefore highly recommended for scientists, researchers, academicians, and students in analytical chemistry, environmental monitoring, drugs analyses, and chromatography.

PREFACE xiii

ACKNOWLEDGMENTS xv

1 Introduction 1

1.1. Nanoanalyses 1

1.2. Definition of Nanochromatography and Nanocapillary Electrophoresis 2

1.3. Nanochromatography and Nanocapillary Electrophoresis 3

1.4. Fabrication of Microdevices 4

1.5. Developments in Nanoanalyses 6

1.6. Data Integration 7

1.7. Protocol of Nanoanalyses 10

1.8. Scope of the Book 12

1.9. Conclusion 12

2 Fabrication of Microchips 17

2.1. Introduction 17

2.2. Substrates 18

2.3. Techniques of Fabrication 20

2.4. Surface Modification 39

2.5. Designs of Chips 45

2.6. Bindings in Chips 49

2.7. Conclusion 50

3 Instrumentation of Nanochromatography and Nanocapillary Electrophoresis 59

3.1. Introduction 59

3.2. Nanoliquid Chromatography (NLC) 60

3.3. Nanocapillary Electrophoresis 74

3.4. Conclusion 85

4 Detection in Nanochromatography and Nanocapillary Electrophoresis 91

4.1. Introduction 91

4.2. Mass Spectrometer Detectors 92

4.3. Fluorescence Detectors 97

4.4. Electrochemical Detectors 99

4.5. Element Specific Detectors 101

4.6. Miscellaneous Detectors 103

4.7. Conclusion 105

5 Sample Preparation in Nanochromatography and Nanocapillary Electrophoresis 109

5.1. Introduction 109

5.2. Sample Preparation 111

5.3. Sampling 111

5.4. Preservation 115

5.5. Filtration 116

5.6. Digestion/Homogenization 118

5.7. Extractions 119

5.8. Clean Up 119

5.9. Preconcentration 121

5.10. Off-Line Nanosample Preparation Methods 121

5.11. Online Nanosample Preparation Methods 125

5.12. Conclusion 138

6 Nano-High Performance Liquid Chromatography 145

6.1. Introduction 145

6.2. Nano-HPLC 146

6.3. Applications 146

6.4. Optimization of Separations in Nano-HPLC 161

6.5. Troubleshooting in Nano-HPLC 161

6.6. Conclusion 161

7 Nanocapillary Electrochromatography and Nanomicellar Electrokinetic Chromatography 167

7.1. Introduction 167

7.2. Nanocapillary Electrochromatography 167

7.3. Nanomicellar Electrokinetic Chromatography 181

7.4. Conclusion 188

8 Nanocapillary Electrophoresis 191

8.1. Introduction 191

8.2. Optimization 192

8.3. Applications 200

8.4. Mechanism of Separation 234

8.5. Conclusion 234

9 Chiral Separations by Nanoliquid Chromatography and Nanocapillary Electrophoresis 245

9.1. Introduction 245

9.2. Nanoliquid Chromatography 246

9.3. Nanocapillary Electrophoresis 249

9.4. Mechanisms of Chiral Separation 260

9.5. Conclusion 261

10 Perspectives on Nanoanalyses 263

10.1. Introduction 263

10.2. Future of Microfluidic Devices 264

10.3. Future Challenges 265

10.4. Conclusion 266

References 267

Subject Index 269