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<p>Preface to the Second Edition xv</p> <p>Abbreviations xvii</p> <p>Symbols and Units xxi</p> <p><b>1 Introduction to Pharmaceutical Analytical Chemistry 1</b></p> <p>1.1 Introduction 1</p> <p>1.2 Pharmaceutical Analytical Chemistry 4</p> <p>1.3 This Textbook 7</p> <p><b>2 Marketing Authorizations, Pharmaceutical Manufacturing, and International Pharmacopoeias 9</b></p> <p>2.1 Introduction 9</p> <p>2.2 Marketing Authorization and Industrial Production 10</p> <p>2.3 Pharmacopoeias 13</p> <p>2.4 Life Time of Pharmaceutical Preparations and Ingredients 14</p> <p><b>3 Fundamentals of Bases, Acids, Solubility, Polarity, Partition, and Stereochemistry 17</b></p> <p>3.1 Acids, Bases, pH, and pKa 17</p> <p>3.2 Buffers 19</p> <p>3.3 Acid and Base Properties of Drug Substances 20</p> <p>3.4 Distribution Between Phases 21</p> <p>3.5 Stereoisomers 26</p> <p>3.6 Active Pharmaceutical Ingredients – A Few Examples 28</p> <p>3.7 Stability of Drug Substances 34</p> <p><b>4 Fundamentals of Pharmaceutical Analytical Chemistry 37</b></p> <p>4.1 Pharmaceutical Analytical Chemistry 37</p> <p>4.2 How to Specify Quantities, Concentrations, and Compositions of Mixtures 39</p> <p>4.3 Laboratory Equipment 43</p> <p>4.4 How to Make Solutions and Dilutions 52</p> <p>4.5 Errors, Accuracy, and Precision 54</p> <p>4.6 Statistical Tests 56</p> <p>4.7 Linear Regression Analysis 65</p> <p>4.8 How to Present an Analytical Result 68</p> <p>4.9 Additional Words and Terms 70</p> <p><b>5 Titration 73</b></p> <p>5.1 Introduction 73</p> <p>5.2 Potentiometric Titration and Electrodes 79</p> <p>5.3 Aqueous Acid–Base Titrations 82</p> <p>5.4 Titration in Non-aqueous Solvents 88</p> <p>5.5 Redox Titrations 91</p> <p>5.6 Alternative Principles of Titration 95</p> <p><b>6 Introduction to Spectroscopic Methods 97</b></p> <p>6.1 Electromagnetic Radiation 97</p> <p>6.2 Molecules and Absorption of Electromagnetic Radiation 99</p> <p>6.3 Absorbing Structures – Chromophores 101</p> <p>6.4 Fluorescence 101</p> <p>6.5 Atoms and Electromagnetic Radiation 102</p> <p><b>7 UV-Vis Spectrophotometry 105</b></p> <p>7.1 Areas of Use 105</p> <p>7.2 Quantitation 106</p> <p>7.3 Absorbance Dependence on Measurement Conditions 108</p> <p>7.4 Identification 110</p> <p>7.5 Instrumentation 111</p> <p>7.6 Practical Work and Method Development 115</p> <p>7.7 Test of Spectrophotometers 116</p> <p>7.8 Fluorimetry 119</p> <p><b>8 IR Spectrophotometry 121</b></p> <p>8.1 IR Spectrophotometry 121</p> <p>8.2 Instrumentation 125</p> <p>8.3 Recording by Transmission, Diffuse Reflectance, and Attenuated Total Reflection 125</p> <p>8.4 Instrument Calibration 128</p> <p>8.5 NIR Spectrophotometry 129</p> <p><b>9 Atomic Spectrometry 131</b></p> <p>9.1 Applications of Atomic Spectrometry 131</p> <p>9.2 Atomic Absorption Spectrometry (AAS) 132</p> <p>9.3 AAS Instrumentation 132</p> <p>9.4 AAS Practical Work and Method Development 137</p> <p>9.5 Atomic Emission Spectrometry (AES) 138</p> <p>9.6 Flame Photometry 139</p> <p>9.7 Inductively Coupled Plasma Emission Spectrometry 140</p> <p>9.8 Inductively Coupled Plasma Mass Spectrometry 141</p> <p><b>10 Introduction to Chromatography 143</b></p> <p>10.1 Introduction 143</p> <p>10.2 General Principles 144</p> <p>10.3 Retention 146</p> <p>10.4 Efficiency 149</p> <p>10.5 Selectivity 151</p> <p>10.6 Resolution 152</p> <p>10.7 Peak Symmetry 154</p> <p>10.8 The Dynamics of Chromatography 155</p> <p><b>11 Separation Principles in Liquid Chromatography 159</b></p> <p>11.1 Introduction 159</p> <p>11.2 Reversed-Phase Chromatography 160</p> <p>11.3 Ion-Pair Chromatography 168</p> <p>11.4 Normal-Phase Chromatography 170</p> <p>11.5 Thin-Layer Chromatography 173</p> <p>11.6 Hydrophilic Interaction Chromatography 175</p> <p>11.7 Ion Exchange Chromatography 177</p> <p>11.8 Size Exclusion Chromatography 178</p> <p>11.9 Chiral Separations 180</p> <p>11.10 Supercritical Fluid Chromatography 182</p> <p><b>12 High Performance Liquid Chromatography 185</b></p> <p>12.1 Introduction 185</p> <p>12.2 The Column 186</p> <p>12.3 Scaling Between Columns 188</p> <p>12.4 Pumps 189</p> <p>12.5 Injectors 191</p> <p>12.6 Detectors 192</p> <p>12.7 Mobile Phases 197</p> <p>12.8 Solvents for Sample Preparation 198</p> <p><b>13 Gas Chromatography 199</b></p> <p>13.1 Introduction 199</p> <p>13.2 Basic Principle 200</p> <p>13.3 Instrumentation 201</p> <p>13.4 Carrier Gas 203</p> <p>13.5 Stationary Phases 205</p> <p>13.6 Retention 207</p> <p>13.7 Columns 208</p> <p>13.8 Injection 209</p> <p>13.9 Detectors 211</p> <p>13.10 Derivatization 213</p> <p><b>14 Electrophoretic Methods 215</b></p> <p>14.1 Introduction 215</p> <p>14.2 Principle and Theory 216</p> <p>14.3 Gel Electrophoresis 218</p> <p>14.4 SDS-PAGE 220</p> <p>14.5 Western Blotting 221</p> <p>14.6 Isoelectric Focusing 223</p> <p>14.7 Capillary Electrophoresis 223</p> <p><b>15 Mass Spectrometry 231</b></p> <p>15.1 Introduction 231</p> <p>15.2 Basic Theory of Mass Spectrometry 233</p> <p>15.3 Ionization 235</p> <p>15.4 The Mass Spectrometer as a Chromatographic Detector – Data Acquisition 236</p> <p>15.5 Quantitation by MS 238</p> <p>15.6 Identification by MS 238</p> <p>15.7 Instrumentation 251</p> <p><b>16 Sample Preparation 259</b></p> <p>16.1 When is Sample Preparation Required? 259</p> <p>16.2 Main Strategies 260</p> <p>16.3 Recovery and Enrichment 261</p> <p>16.4 Liquid–Liquid Extraction 263</p> <p>16.5 Solid–Liquid Extraction 269</p> <p>16.6 Solid Phase Extraction 270</p> <p><b>17 Quality of Analytical Data and Validation 281</b></p> <p>17.1 Instrumental Signals 281</p> <p>17.2 Calibration Methods 282</p> <p>17.3 Analytical Procedures 290</p> <p>17.4 Validation 291</p> <p>17.5 System Suitability 301</p> <p><b>18 Chemical Analysis of Pharmaceutical Ingredients 305</b></p> <p>18.1 Pharmaceutical Ingredients, Production, and Control 306</p> <p>18.2 Pharmacopoeia Monographs 308</p> <p>18.3 Impurities in Pharmaceutical Ingredients 321</p> <p>18.4 Identification of Pharmaceutical Ingredients 324</p> <p>18.5 Impurity Testing of Pharmaceutical Ingredients (Pure Chemical Ingredients) 344</p> <p>18.6 Identification and Impurity Testing of Organic Multi-Chemical Ingredients 368</p> <p>18.7 Assay of Pharmaceutical Ingredients 375</p> <p>18.8 Chemical Analysis of Pharmaceutical Ingredients Not Included in Pharmacopoeias 388</p> <p><b>19 Chemical Analysis of Pharmaceutical Preparations 389</b></p> <p>19.1 Chemical Analysis of Pharmaceutical Preparations 389</p> <p>19.2 Monographs and Chemical Analysis 390</p> <p>19.3 Identification of the API 395</p> <p>19.4 Assay of the Active Pharmaceutical Ingredient 410</p> <p>19.5 Chemical Tests for Pharmaceutical Preparations 427</p> <p><b>20 Bioanalysis Chemical Analysis of Pharmaceuticals in Biological Fluids 433</b></p> <p>20.1 Bioanalysis 433</p> <p>20.2 Biological Fluids 438</p> <p>20.3 Bioanalytical Methods – An Overview 440</p> <p>20.4 Sampling 440</p> <p>20.5 Sample Preparation 441</p> <p>20.6 Separation and Detection 446</p> <p>20.7 Quantitation 447</p> <p>20.8 Screening 453</p> <p><b>21 Chemical Analysis of Biopharmaceuticals 459</b></p> <p>21.1 Biopharmaceuticals 459</p> <p>21.2 Biopharmaceuticals versus Small Molecule APIs 463</p> <p>21.3 Biopharmaceuticals and Pharmacopoeias 464</p> <p>21.4 Production of Biopharmaceuticals 465</p> <p>21.5 Identification Procedures for Biopharmaceuticals (Active Substance) 467</p> <p>21.6 Impurity Tests for Biopharmaceuticals (Active Substances) 488</p> <p>21.7 Assay of Biopharmaceuticals (Active Substance) 498</p> <p>21.8 Monoclonal Antibodies 500</p> <p>21.9 Analysis of Biopharmaceutical Products 502</p> <p>21.10 Bioanalysis of Biopharmaceuticals Using LC-MS/MS 503</p> <p>Index 505</p>

<p><b>STIG PEDERSEN-BJERGAARD</b> is Professor at the Department of Pharmacy, University of Oslo and Professor at the Department of Pharmacy, University of Copenhagen. <p><b>BENTE GAMMELGAARD</b> is Professor at the Department of Pharmacy, University of Copenhagen. <p><b>TRINE GRØNHAUG HALVORSEN</b> is Associate Professor at the Department of Pharmacy, University of Oslo.

<p><b>The definitive textbook on the chemical analysis of pharmaceutical drugs – fully revised and updated</b> <p><i>Introduction to Pharmaceutical Analytical Chemistry</i> enables students to gain fundamental knowledge of the vital concepts, techniques and applications of the chemical analysis of pharmaceutical ingredients, final pharmaceutical products and drug substances in biological fluids. A unique emphasis on pharmaceutical laboratory practices, such as sample preparation and separation techniques, provides an efficient and practical educational framework for undergraduate studies in areas such as pharmaceutical sciences, analytical chemistry and forensic analysis. Suitable for foundational courses, this essential undergraduate text introduces the common analytical methods used in quantitative and qualitative chemical analysis of pharmaceuticals. <p>This extensively revised second edition includes a new chapter on chemical analysis of biopharmaceuticals, which includes discussions on identification, purity testing and assay of peptide and protein-based formulations. Also new to this edition are improved full-colour illustrations and tables, a streamlined chapter structure and text revised for increased clarity and comprehension. <ul> <li>Introduces the fundamental concepts of pharmaceutical analytical chemistry and statistics</li> <li>Presents a systematic investigation of pharmaceutical applications absent from other textbooks on the subject</li> <li>Examines various analytical techniques commonly used in pharmaceutical laboratories</li> <li>Provides practice problems, up-to-date practical examples and detailed illustrations</li> <li>Includes updated content aligned with the current European and United States Pharmacopeia regulations and guidelines</li> </ul> <p>Covering the analytical techniques and concepts necessary for pharmaceutical analytical chemistry, <i>Introduction to Pharmaceutical Analytical Chemistry</i> is ideally suited for students of chemical and pharmaceutical sciences as well as analytical chemists transitioning into the field of pharmaceutical analytical chemistry.

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