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Introduction to Pharmaceutical Chemical Analysis

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ISBN-13:
9781119953609
Einband:
E-Book
Seiten:
512
Autor:
Steen Hansen
eBook Typ:
PDF
eBook Format:
E-Book
Kopierschutz:
Adobe DRM [Hard-DRM]
Sprache:
Englisch
Beschreibung:

This textbook is the first to present a systematic introduction tochemical analysis of pharmaceutical raw materials, finishedpharmaceutical products, and of drugs in biological fluids, whichare carried out in pharmaceutical laboratories worldwide.
In addition, this textbook teaches the fundamentals of all themajor analytical techniques used in the pharmaceutical laboratory,and teaches the international pharmacopoeias and guidelines ofimportance for the field. It is primarily intended for the pharmacystudent, to teach the requirements in "analyticalchemistry" for the 5 years pharmacy curriculum, but thetextbook is also intended for analytical chemists moving into thefield of pharmaceutical analysis.
* Addresses the basic concepts, then establishes the foundationsfor the common analytical methods that are currently used in thequantitative and qualitative chemical analysis of pharmaceuticaldrugs
* Provides an understanding of common analytical techniques usedin all areas of pharmaceutical development
* Suitable for a foundation course in chemical andpharmaceutical sciences
* Aimed at undergraduate students of degrees in PharmaceuticalScience/Chemistry Analytical Science/Chemistry, Forensicanalysis
* Includes many illustrative examples
InhaltsangabePreface xv

1 Introduction to Pharmaceutical Analysis 1

1.1 Applications and Definitions 1

1.2 The Life of Medicines 4

1.3 The Quality of Medical Products 8

1.4 Summary 11

2 International Pharmacopoeias, Regulations and Guidelines 13

2.1 Overview of Legislation 13

2.2 Legislation and Regulations for Industrial Production 14

2.3 Life Time of Drugs and Drug Substances 17

2.4 Pharmacopoeias 18

2.5 International Harmonization 19

2.5.1 International Conference on Harmonization 20

2.5.2 Pharmacopoeial Discussion Group 20

2.6 Legislation and Regulations for Pharmacy Production 20

2.7 Summary 21

3 Fundamental Chemical Properties, Buffers and pH 23

3.1 pH and pKa 23

3.2 Partition 25

3.3 Stereochemistry 28

3.4 Stability Testing 29

3.5 Summary 30

4 Fundamentals of Pharmaceutical Analysis 33

4.1 What is a Pharmaceutical (Chemical) Analysis? 33

4.2 How to Specify Quantities and Concentrations? 35

4.3 Basic Laboratory Equipment 37

4.3.1 The Analytical Balance 37

4.3.2 Pipettes 41

4.3.3 Volumetric Flasks 44

4.3.4 Burettes 47

4.4 How to Make Solutions and Dilutions 47

4.5 Calibration of Analytical Methods 49

4.6 Errors, Accuracy, and Precision 50

4.6.1 Systematic and Random Errors 50

4.6.2 Accuracy and Precision 51

4.7 Statistics 52

4.7.1 Mean Value and Standard Deviation 52

4.7.2 Confidence Intervals 54

4.7.3 Comparison of Means with a t-Test 55

4.7.4 Q-Test to Reject Outliers 56

4.7.5 Linear Regression with the Method of Least Squares 57

4.7.6 How to Present an Analytical Result 58

4.8 Some Words and Concepts 62

4.8.1 Analysis and Determination 62

4.8.2 Sample Replicates and Measuring Replicates 62

4.8.3 Interference 62

4.8.4 Blind Samples 62

5 Titrimetric Methods 65

5.1 Introduction 65

5.2 Acid–Base Titrations 72

5.3 Acid–Base Titrations in Non-Aqueous Media 75

5.4 Redox Titrations 78

5.5 Other Principles of Titration 81

5.6 Summary 82

6 Introduction to Spectroscopic Methods 83

6.1 Electromagnetic Radiation 83

6.2 Molecules and Electromagnetic Radiation 85

6.3 Atoms and Electromagnetic Radiation 86

6.4 Summary 88

7 UV Spectrophotometry 89

7.1 Principle of Quantitative Determination 89

7.2 Principle of Identification 94

7.3 Which Substances Have Strong UV Absorbance? 95

7.4 Instrumentation 95

7.5 Practical Work and Method Development 99

7.6 Areas of Usage and Performance 101

7.7 System Testing 101

7.8 Summary 102

8 IR Spectrophotometry 103

8.1 IR Spectrophotometry 103

8.2 Instrumentation 106

8.3 Scope 109

8.4 Instrument Calibration 109

8.5 NIR Spectrophotometry 110

8.6 Applications 112

8.7 Summary 114

9 Atomic Spectrometry 115

9.1 Atomic Absorption Spectrometry 115

9.2 Instrumentation 118

9.3 Applications and Performance 121

9.4 Practical Work and Method Development 122

9.5 Atomic Emission Spectrometry 123

9.6 Instrumentation 124

9.7 Summary 124

10 Chromatography 127

10.1 General Principles 127

10.2 Retention 131

10.3 Column Efficiency 133

10.4 Selectivity 135

10.5 Peak Symmetry 136

10.6 Resolution 138

10.7 Chromatographic Techniques 140

10.8 Summary 140

11 Chromatographic Separation Principles 141

11.1 General Introduction 141

11.2 Normal 169

12.8 Applications of TLC 169

12.9 Quantitative Analysis and Instrumentation 170

12.10 Summary 171

13 High Performance Liquid Chromatography 173

13.1 Introduction 173

13.2 The Chromatographic Separation Process 175

13.3 The Column 177

13.4 Pumps 180

13.5 Detectors 182

13.5.1 UV detector 182

13.5.2 Fluorescence Detector 184

13.5.3 Electrochemical Detector 186

13.5.4 Refractive Index, Evaporative Light Scattering and Corona Discharge Detectors 186

13.5.5 Combination of Detectors 187

13.6 Injectors 187

13.7 Mobile Phases 188

13.8 Solvents for Sample Preparation 189

13.9 Reporting the Results 189

13.10 Summary 190

14 Gas Chromatography 191

14.1 Introduction 191

14.2 Apparatus 192

14.3 Temperature 193

14.4 Carrier Gas 195

14.5 Stationary Phases 196

14.6 Selectivity in GC 197

14.7 Columns 198

14.7.1 Capillary Columns 198

14.7.2 Packed Columns 199

14.8 Injection Systems 200

14.8.1 Injection Systems for Capillary Columns 200

14.8.2 Injection Systems for Packed Columns 202

14.9 Detectors 203

14.9.1 Flame Ionization Detector 203

14.9.2 Nitrogen–Phosphorus Detector 203

14.9.3 Thermal Conductivity Detector 204

14.9.4 Electron Capture Detector 204

14.9.5 Mass Spectrometry Detector 206

14.10 Derivatization 206

14.10.1 Silylation 206

14.10.2 Alkylation 207

14.10.3 Acylation 207

14.11 The Uses of GC 208

14.12 More Advanced GC techniques 209

14.13 Summary 209

15 Capillary Electrophoresis 211

15.1 Principle and Theory 211

15.2 Electroosmotic Flow 213

15.3 Instrumentation 214

15.4 The Capillary 217

15.5 Sample Introduction 218

15.6 Capillary Zone Electrophoresis; an Example 221

15.7 Micellar Electrokinetic Chromatography 222

15.8 Chiral Separations 224

15.9 Coated Capillaries 225

15.10 Non-Aqueous CE 229

15.11 Summary 229

16 Mass Spectrometry 231

16.1 Introduction 231

16.2 Basic Theory 233

16.3 Electron Ionization 236

16.4 Identification using Electron Ionization Spectra 237

16.5 Characterization of Totally Unknowns using Electron Ionization Spectra 239

16.6 Chemical Ionization 244

16.7 Electrospray Ionization 246

16.8 Atmospheric Pressure Chemical Ionization 247

16.9 High-Resolution Mass Spectrometry 248

16.10 Instrumentation 250

16.11 Chromatography Coupled with Mass Spectrometry 253

16.12 Quantitative GC-MS and LC-MS 256

16.13 Areas of Usage and Performance 257

16.14 Matrix-Assisted Laser Desorption/Ionization Mass Spectrometry 257

16.15 Inductively Coupled Plasma Mass Spectrometry 258

16.16 Summary 259

17 Miscellaneous Chemical Techniques 261

17.1 Potentiometric Determination of Ions using Ion-Selective Electrodes 261

17.2 Paper Chromatography 263

17.3 Supercritical Fluid Chromatography 264

17.4 Gel Electrophoresis 265

17.5 Iso-Electric Focusing 267

17.6 Nuclear Magnetic Resonance Spectrometry 268

17.7 Raman Spectrometry 270

18 Sample Preparation 273

18.1 Why is Sample Preparation Required? 273

18.2 Main Strategies 274

18.3 Recovery and Enrichment 276

18.4 Protein Precipitation 278

18.5 Liquid–Liquid Extraction 279

18.5.1 Fundamentals 279

18.5.2 A Closer Look at the Theory 279

18.5.3 Extraction Solvents 282

18.5.4 Calculation of Recovery 283

18.5.5 Multiple Extractions 285

18.5.6 LLE with Back-Extraction 286

18.6 Solid–Liquid Extraction 28720.3 Validation 314

20.3.1 Analytical Procedure 317

20.3.2 Accuracy 317

20.3.3 Precision 318

20.3.4 Specificity 320

20.3.5 Detection Limit 320

20.3.6 Quantification Limit 321

20.3.7 Linearity and Range 321

20.3.8 Robustness 323

20.3.9 Test Methods in the European Pharmacopeia 325

20.4 System Suitability 325

20.4.1 Adjustment of Chromatographic Conditions 326

21 Chemical Analysis of Drug Substances 327

21.1 What is a Pharmaceutical Raw Material, how is it Produced and why must it be Controlled? 327

21.2 The Pharmacopoeias – the Basis for Control of Pharmaceutical Raw Materials 330

21.3 Which Contaminants are Found in Raw Materials, What are the Requirements in a Maximum Content   and Why? 337

21.3.1 Well Defined Chemical Compounds 339

21.3.2 Mixtures of Organic Compounds 343

21.4 How to Check the Identity of Pharmaceutical Raw Materials 344

21.4.1 Overview of the Identification Procedures 344

21.4.2 Techniques used for the Identification of Well Defined Chemical Compounds 344

21.4.2.1 Infrared Absorption Spectrophotometry 344

21.4.2.2 Ultraviolet and Visible Absorption Spectrophotometry 347

21.4.2.3 Thin-Layer Chromatography 351

21.4.2.4 Melting Point 352

21.4.2.5 Polarimetry 353

21.4.2.6 High Performance Liquid Chromatography 356

21.4.2.7 Chloride and Sulfate Identification 359

21.5 How to Test for Impurities in Pharmaceutical Raw Materials 359

21.5.1 Main Purity Tests for Well Define

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