Description

The first edition of the translation of the book "Introduction to Pharmaceutical Analytical Chemistry" is a useful and modern concise manual for undergraduate/graduate students or scientists in pharmaceutical analysis and drug quality control.

The educational sections of this book primarily provide the fundamental knowledge of instrumental pharmaceutical analysis in real working conditions within a drug control laboratory. Additionally, it offers the opportunity to inform the reader about the requirements of Pharmacopeias [European (Eur.Ph), American (USP) and British (BP)] on quality control issues, presenting excerpts of analyses of pharmaceutical formulations and solving various problems.

Based on the provided theoretical and practical information at laboratory as well as industrial levels, it offers the necessary knowledge and skills to students, making them competitive scientists for their future employment in the Pharmaceutical Industry in the areas of Quality Control or Research and Development of Pharmaceutical Products.

As previously mentioned by the authors of the foreign language edition of the book, the aim of this work is to train and prepare scientists who are knowledgeable and specialized in the field of Pharmaceutical Analysis.

Contents

Foreword to the 2nd edition xv

Foreword to the Greek edition xvii

Abbreviations xix

Symbols and Units xxiv

1. Introduction to Pharmaceutical Analytical Chemistry 1

1.1 Introduction 1

1.2 Pharmaceutical Analytical Chemistry 5

1.3 This manuscript 8

2. Marketing Authorization, Production of Pharmaceutical Products, and International Pharmacopeias 11

2.1 Introduction 11

2.2 Marketing Authorization and Industrial Production 11

2.3 Pharmacopeias 16

2.4 Shelf Life of Pharmaceutical Products and their Components 17

3. Basic Principles of Acids, Bases, Solubility, Polarity, Distribution, and Stereochemistry 19

3.1 Acids, Bases, pH, and pKa 19

3.2 Buffer Solutions 21

3.3 Acidic and Basic Properties of Pharmaceutical Compounds 23

3.4 Phase Distribution 25

3.5 Stereoisomers 29

3.6 Pharmaceutical Active Ingredients – Examples 31

3.7 Stability of Pharmaceutical Active Ingredients 38

4. Principles of Pharmaceutical Analytical Chemistry 41

4.1 Pharmaceutical Analytical Chemistry 41

4.2 How to Determine Amounts, Concentrations, and the Composition of Mixtures 43

4.3 Laboratory Equipment 48

4.4 How to Prepare Solutions and Make Dilutions 59

4.5 Errors, Accuracy, and Precision 60

4.6 Statistical Tests 63

4.7 Linear Regression Analysis 73

4.8 How to Present an Analytical Result 75

4.9 Additional Vocabulary and Terminology 80

5. Titration 83

5.1 Introduction 83

5.2 Potentiometric Titrations and Electrodes 88

5.3 Aqueous Acid-Base Titrations 94

5.4 Titration in Non-Aqueous Solvents 99

5.5 Redox Titrations 104

5.6 Alternative Types of Titration 110

6. Introduction to Spectroscopic Techniques 113

6.1 Electromagnetic Radiation 113

6.2 Molecules and Absorption of Electromagnetic Radiation 116

6.3 Chemical Structures that Absorb – Chromophores 117

6.4 Fluorescence 118

6.5 Atoms and Electromagnetic Radiation 119

7. UV-Vis Spectrophotometry 121

7.1 Fields of Application 121

7.2 Quantitative Determination 122

7.3 Absorption Dependence on Measurement Conditions 123

7.4 Identification 127

7.5 Instrumentation 128

7.6 Practical Work and Method Development 133

7.7 Spectrophotometer Control 135

7.8 Fluorometry 139

8. IR Spectrophotometry 141

8.1 IR Spectrophotometry 141

8.2 Instrumentation 144

8.3 Recording of Spectra of Transmittance, Diffuse Reflection, and Attenuated Total Reflection 147

8.4 Instrument Calibration 149

8.5 NIR Spectrophotometry 149

9. Atomic Spectrometry 153

9.1 Applications of Atomic Spectrometry 153

9.2 Atomic Absorption Spectrometry (AAS) 154

9.3 AAS Instrumentation 154

9.4 Practical Work and AAS Method Development 160

9.5 Atomic Emission Spectrometry (AES) 162

9.6 Flame Photometry 163

9.7 Inductively Coupled Plasma Emission Spectrometry 164

9.8 Inductively Coupled Plasma Mass Spectrometry 165

10. Introduction to Chromatography 169

10.1 Introduction 169

10.2 General Principles 170

10.3 Retention 173

10.4 Efficiency 176

10.5 Selectivity 178

10.6 Resolving Power 179

10.7 Peak Symmetry 180

10.8 Flow Dynamics in Chromatography 182

11. Principles of Separation in Liquid Chromatography 187

11.1 Introduction 187

11.2 Reversed-Phase Chromatography 188

11.3 Ion-Pair Chromatography 197

11.4 Normal-Phase Chromatography 200

11.5 Thin-Layer Chromatography 204

11.6 Hydrophilic Interaction Chromatography 207

11.7 Ion-Exchange Chromatography 208

11.8 Size-Exclusion Chromatography 211

11.9 Handwritten Separations 213

11.10 Supercritical Fluid Chromatography 213

12. High-Performance Liquid Chromatography 217

12.1 Introduction 217

12.2 The Column 219

12.3 Geometric Characteristics of Columns 221

12.4 Pumps 221

12.5 Sample Introducers 225

12.6 Detectors 226

12.7 Mobile Phases 232

12.8 Solvents for Sample Pre-treatment 233

13. Gas Chromatography 235

13.1 Introduction 235

13.2 Basic Principles 236

13.3 Instrumentation 238

13.4 Carrier Gas 241

13.5 Stationary Phases 242

13.6 Retention 244

13.7 Columns 245

13.8 Sample Injection 248

13.9 Detectors 250

13.10 Derivatization 253

14. Electrophoretic Techniques 255

14.1 Introduction 255

14.2 Basic Principles and Theory 256

14.3 Gel Electrophoresis 258

14.4 SDS-PAGE 261

14.5 Western Blotting 262

14.6 Isoelectric Focusing Electrophoresis 263

14.7 Capillary Electrophoresis 265

15. Mass Spectrometry 275

15.1 Introduction 275

15.2 Basic Theory of Mass Spectrometry 276

15.3 Ionization 279

15.4 The Mass Spectrometer as a Chromatography Detector – Data Acquisition 281

15.5 Quantitative Determination by MS 283

15.6 Identification by MS 284

15.7 Instrumentation 298

16. Sample Pre-treatment 309

16.1 When is Sample Pre-treatment Required? 309

16.2 Main Strategies 310

16.3 Recovery and Preconcentration 311

16.4 Liquid-Liquid Extraction 314

16.5 Solid-Liquid Extraction 322

16.6 Solid-Phase Extraction 323

17. Quality of Analytical Data and Validation 335

17.1 Instrument Signals 335

17.2 Calibration Methods 337

17.3 Analytical Procedures 342

17.4 Validation 347

17.5 System Suitability 358

18. Chemical Analysis of Pharmaceutical Ingredients 363

18.1 Pharmaceutical Ingredients, Production, and Control 364

18.2 Pharmacopeial Monographs 367

18.3 Impurities in Pharmaceutical Ingredients 382

18.4 Identification of Pharmaceutical Ingredients 387

18.5 Control of Impurities in Pharmaceutical Ingredients (Pure Chemical Ingredients) 408

18.6 Identification and Control of Impurities in Organic Polymer Ingredients 437

18.7 Quantitative Determination of Pharmaceutical Ingredients 445

18.8 Chemical Analysis of Pharmaceutical Ingredients Not Included in Pharmacopeias 459

19. Chemical Analysis of Pharmaceutical Formulations 463

19.1 Chemical Analysis of Pharmaceutical Formulations 463

19.2 Monographs and Chemical Analysis 464

19.3 Identification of APIs 470

19.4 Quantitative Determination of Active Pharmaceutical Ingredient 485

19.5 Chemical Controls for Pharmaceutical Formulations 497

20. Bioanalysis - Chemical Analysis of Pharmaceutical Compounds in Biological Fluids 513

20.1 Bioanalysis 513

20.2 Biological Fluids 519

20.3 Bioanalytical Methods – Overview 522

20.4 Sampling 522

20.5 Sample Pre-treatment 523

20.6 Separation and Detection 529

20.7 Quantitation 531

20.8 Control 534

21. Chemical Analysis of Biopharmaceuticals 545

21.1 Biopharmaceuticals 545

21.2 Biopharmaceuticals vs. Small Molecule APIs 550

21.3 Biopharmaceuticals and Pharmaceutics 551

21.