Introduction to Pharmaceutical Chemical Analysis
, by Hansen, Steen; Pedersen-Bjergaard, Stig; Rasmussen, Knut
- ISBN: 9780470661222 | 0470661224
- Cover: Paperback
- Copyright: 12/12/2011
This textbook is the first to present a systematic introduction to chemical analysis of pharmaceutical raw materials, finished pharmaceutical products, and of drugs in biological fluids, which are carried out in pharmaceutical laboratories worldwide. In addition, this textbook teaches the fundamentals of all the major analytical techniques used in the pharmaceutical laboratory, and teaches the international pharmacopoeias and guidelines of importance for the field. It is primarily intended for the pharmacy student, to teach the requirements in "analytical chemistry" for the 5 years pharmacy curriculum, but the textbook is also intended for analytical chemists moving into the field of pharmaceutical analysis. Addresses the basic concepts, then establishes the foundations for the common analytical methods that are currently used in the quantitative and qualitative chemical analysis of pharmaceutical drugs Provides an understanding of common analytical techniques used in all areas of pharmaceutical development Suitable for a foundation course in chemical and pharmaceutical sciences Aimed at undergraduate students of degrees in Pharmaceutical Science/Chemistry Analytical Science/Chemistry, Forensic analysis Includes many illustrative examples
Steen Hansen is professor in analytical chemistry at the Faculty of Pharmaceutical Sciences at Copenhagen University (Denmark), and has extensive experience in the teaching of analytical chemistry for pharmacy students. His main research interests are in basic separation sciences (primarily HPLC and CE), in particular on separation mechanisms, but also extend into hyphenated techniques using NMR and ICP-MS besides conventional detection techniques. He has authored and/or coauthored more than 240 papers in international peer-review journals. For 20 years, he was the President of the Scandinavian Section of The Chromatographic Discussion Group until this was renamed the Separation Sciences Foundation of which he is President.
Knut Einar Rasmussen is professor in pharmacy at the School of Pharmacy at University of Oslo (Norway) and has similarly long experience in teaching of drug analysis for Pharmacy students. He has published extensively and his main research areas are focused on the development of innovative state-of-the-art miniaturized methods in separation science combined with detection and structure determination of drugs, naturally occurring biomolecules/biomarkers and environmental biomarkers.
Stig Pedersen-Bjergaard is professor at at the School of Pharmacy, University of Oslo (Oslo, Norway) as well as in 2008, being appointed as full Professor (part time) at Department of Pharmaceutics and Analytical Chemistry, Faculty of Pharmaceutical Sciences, University of Copenhagen (Copenhagen, Denmark). SPB has specialized in analytical micro extraction technologies, on development and applications of artificial liquid membranes, and on electrokinetic separation methods. SPB has published more than 90 papers in international journals, given more than 65 presentations at international symposia, authored 6 patent applications, and is a member of the Editorial board for Analytica Chimica Acta and International Journal of Analytical Chemistry.
| Preface | p. xv |
| Introduction to Pharmaceutical Analysis | p. 1 |
| Applications and Definitions | p. 1 |
| The Life of Medicines | p. 4 |
| The Quality of Medical Products | p. 8 |
| Summary | p. 11 |
| International Pharmacopoeias, Regulations and Guidelines | p. 13 |
| Overview of Legislation | p. 13 |
| Legislation and Regulations for Industrial Production | p. 14 |
| Life Time of Drugs and Drug Substances | p. 17 |
| Pharmacopoeias | p. 18 |
| International Harmonization | p. 19 |
| International Conference on Harmonization | p. 20 |
| Pharmacopoeial Discussion Group | p. 20 |
| Legislation and Regulations for Pharmacy Production | p. 20 |
| Summary | p. 21 |
| Fundamental Chemical Properties, Buffers and pH | p. 23 |
| pH and pKa | p. 23 |
| Partition | p. 25 |
| Stereochemistry | p. 28 |
| Stability Testing | p. 29 |
| Summary | p. 30 |
| Fundamentals of Pharmaceutical Analysis | p. 33 |
| What is a Pharmaceutical (Chemical) Analysis? | p. 33 |
| How to Specify Quantities and Concentrations? | p. 35 |
| Basic Laboratory Equipment | p. 37 |
| The Analytical Balance | p. 37 |
| Pipettes | p. 41 |
| Volumetric Flasks | p. 44 |
| Burettes | p. 47 |
| How to Make Solutions and Dilutions | p. 47 |
| Calibration of Analytical Methods | p. 49 |
| Errors, Accuracy, and Precision | p. 50 |
| Systematic and Random Errors | p. 50 |
| Accuracy and Precision | p. 51 |
| Statistics | p. 52 |
| Mean Value and Standard Deviation | p. 52 |
| Confidence Intervals | p. 54 |
| Comparison of Means with a t-Test | p. 55 |
| Q-Test to Reject Outliers | p. 56 |
| Linear Regression with the Method of Least Squares | p. 57 |
| How to Present an Analytical Result | p. 58 |
| Some Words and Concepts | p. 62 |
| Analysis and Determination | p. 62 |
| Sample Replicates and Measuring Replicates | p. 62 |
| Interference | p. 62 |
| Blind Samples | p. 62 |
| Titrimetric Methods | p. 65 |
| Introduction | p. 65 |
| Acid-Base Titrations | p. 72 |
| Acid-Base Titrations in Non-Aqueous Media | p. 75 |
| Redox Titrations | p. 78 |
| Other Principles of Titration | p. 81 |
| Summary | p. 82 |
| Introduction to Spectroscopic Methods | p. 83 |
| Electromagnetic Radiation | p. 83 |
| Molecules and Electromagnetic Radiation | p. 85 |
| Atoms and Electromagnetic Radiation | p. 86 |
| Summary | p. 88 |
| UV Spectrophotometry | p. 89 |
| Principle of Quantitative Determination | p. 89 |
| Principle of Identification | p. 94 |
| Which Substances Have Strong UV Absorbance? | p. 95 |
| Instrumentation | p. 95 |
| Practical Work and Method Development | p. 99 |
| Areas of Usage and Performance | p. 101 |
| System Testing | p. 101 |
| Summary | p. 102 |
| IR Spectrophotometry | p. 103 |
| IR Spectrophotometry | p. 103 |
| Instrumentation | p. 106 |
| Scope | p. 109 |
| Instrument Calibration | p. 109 |
| NIR Spectrophotometry | p. 110 |
| Applications | p. 112 |
| Summary | p. 114 |
| Atomic Spectrometry | p. 115 |
| Atomic Absorption Spectrometry | p. 115 |
| Instrumentation | p. 118 |
| Applications and Performance | p. 121 |
| Practical Work and Method Development | p. 122 |
| Atomic Emission Spectrometry | p. 123 |
| Instrumentation | p. 124 |
| Summary | p. 124 |
| Chromatography | p. 127 |
| General Principles | p. 127 |
| Retention | p. 131 |
| Column Efficiency | p. 133 |
| Selectivity | p. 135 |
| Peak Symmetry | p. 136 |
| Resolution | p. 138 |
| Chromatographic Techniques | p. 140 |
| Summary | p. 140 |
| Chromatographic Separation Principles | p. 141 |
| General Introduction | p. 141 |
| Normal Phase Chromatography | p. 142 |
| Silica | p. 142 |
| Interactions | p. 143 |
| Order of Elution | p. 144 |
| Other Stationary Phases | p. 145 |
| Mobile Phases | p. 146 |
| Summary of Normal Phase Chromatography | p. 147 |
| Reversed Phase Chromatography | p. 148 |
| Stationary Phases | p. 148 |
| Retention Mechanisms | p. 150 |
| Mobile Phases | p. 152 |
| Ion-Pair Chromatography | p. 155 |
| Summary of Reversed Phase Chromatography | p. 155 |
| Hydrophilic Interaction Chromatography | p. 156 |
| Chiral Separations | p. 156 |
| Size Exclusion Chromatography | p. 158 |
| Principle | p. 158 |
| Summary of SEC | p. 160 |
| Ion Exchange Chromatography | p. 160 |
| Thin-Layer Chromatography | p. 163 |
| Introduction | p. 163 |
| Apparatus | p. 164 |
| TLC Plates | p. 166 |
| Stationary Phases | p. 166 |
| Mobile Phases | p. 167 |
| Chromatographic Development | p. 168 |
| Detection | p. 169 |
| Applications of TLC | p. 169 |
| Quantitative Analysis and Instrumentation | p. 170 |
| Summary | p. 171 |
| High Performance Liquid Chromatography | p. 173 |
| Introduction | p. 173 |
| The Chromatographic Separation Process | p. 175 |
| The Column | p. 177 |
| Pumps | p. 180 |
| Detectors | p. 182 |
| UV detector | p. 182 |
| Fluorescence Detector | p. 184 |
| Electrochemical Detector | p. 186 |
| Refractive Index, Evaporative Light Scattering and Corona Discharge Detectors | p. 186 |
| Combination of Detectors | p. 187 |
| Injectors | p. 187 |
| Mobile Phases | p. 188 |
| Solvents for Sample Preparation | p. 189 |
| Reporting the Results | p. 189 |
| Summary | p. 190 |
| Gas Chromatography | p. 191 |
| Introduction | p. 191 |
| Apparatus | p. 192 |
| Temperature | p. 193 |
| Carrier Gas | p. 195 |
| Stationary Phases | p. 196 |
| Selectivity in GC | p. 197 |
| Columns | p. 198 |
| Capillary Columns | p. 198 |
| Packed Columns | p. 199 |
| Injection Systems | p. 200 |
| Injection Systems for Capillary Columns | p. 200 |
| Injection Systems for Packed Columns | p. 202 |
| Detectors | p. 203 |
| Flame Ionization Detector | p. 203 |
| Nitrogen-Phosphorus Detector | p. 203 |
| Thermal Conductivity Detector | p. 204 |
| Electron Capture Detector | p. 204 |
| Mass Spectrometry Detector | p. 206 |
| Derivatization | p. 206 |
| Silylation | p. 206 |
| Alkylation | p. 207 |
| Acylation | p. 207 |
| The Uses of GC | p. 208 |
| More Advanced GC techniques | p. 209 |
| Summary | p. 209 |
| Capillary Electrophoresis | p. 211 |
| Principle and Theory | p. 211 |
| Electroosmotic Flow | p. 213 |
| Instrumentation | p. 214 |
| The Capillary | p. 217 |
| Sample Introduction | p. 218 |
| Capillary Zone Electrophoresis; an Example | p. 221 |
| Micellar Electrokinetic Chromatography | p. 222 |
| Chiral Separations | p. 224 |
| Coated Capillaries | p. 225 |
| Non-Aqueous CE | p. 229 |
| Summary | p. 229 |
| Mass Spectrometry | p. 231 |
| Introduction | p. 231 |
| Basic Theory | p. 233 |
| Electron Ionization | p. 236 |
| Identification using Electron Ionization Spectra | p. 237 |
| Characterization of Totally Unknowns using Electron Ionization Spectra | p. 239 |
| Chemical Ionization | p. 244 |
| Electrospray Ionization | p. 246 |
| Atmospheric Pressure Chemical Ionization | p. 247 |
| High-Resolution Mass Spectrometry | p. 248 |
| Instrumentation | p. 250 |
| Chromatography Coupled with Mass Spectrometry | p. 253 |
| Quantitative GC-MS and LC-MS | p. 256 |
| Areas of Usage and Performance | p. 257 |
| Matrix-Assisted Laser Desorption/Ionization Mass Spectrometry | p. 257 |
| Inductively Coupled Plasma Mass Spectrometry | p. 258 |
| Summary | p. 259 |
| Miscellaneous Chemical Techniques | p. 261 |
| Potentiometric Determination of Ions using Ion-Selective Electrodes | p. 261 |
| Paper Chromatography | p. 263 |
| Supercritical Fluid Chromatography | p. 264 |
| Gel Electrophoresis | p. 265 |
| Iso-Electric Focusing | p. 267 |
| Nuclear Magnetic Resonance Spectrometry | p. 268 |
| Raman Spectrometry | p. 270 |
| Sample Preparation | p. 273 |
| Why is Sample Preparation Required? | p. 273 |
| Main Strategies | p. 274 |
| Recovery and Enrichment | p. 276 |
| Protein Precipitation | p. 278 |
| Liquid-Liquid Extraction | p. 279 |
| Fundamentals | p. 279 |
| A Closer Look at the Theory | p. 279 |
| Extraction Solvents | p. 282 |
| Calculation of Recovery | p. 283 |
| Multiple Extractions | p. 285 |
| LLE with Back-Extraction | p. 286 |
| Solid-Liquid Extraction | p. 287 |
| Solid Phase Extraction | p. 287 |
| Fundamentals | p. 287 |
| The SPE Column | p. 288 |
| Conditioning | p. 289 |
| Equipment | p. 290 |
| Reversed-Phase SPE | p. 290 |
| Secondary Interactions | p. 292 |
| Ion Exchange SPE | p. 293 |
| Mixed-Mode SPE | p. 295 |
| Normal-Phase SPE | p. 297 |
| Summary | p. 298 |
| Analytical Chemical Characteristics of Selected Drug Substances | p. 299 |
| Amitriptyline and Mianserin | p. 299 |
| Morphine and Codeine | p. 301 |
| Ibuprofen and Naproxen | p. 302 |
| Furosemide | p. 304 |
| Paracetamol (Acetaminophen) | p. 306 |
| Neutral Drugs | p. 307 |
| Quantification and Quality of Analytical Data | p. 309 |
| Peak Height and Peak Area | p. 309 |
| Calibration Methods | p. 310 |
| External Standard Method | p. 310 |
| Internal Standard Method | p. 313 |
| Standard Addition | p. 314 |
| Normalization | p. 314 |
| Validation | p. 314 |
| Analytical Procedure | p. 317 |
| Accuracy | p. 317 |
| Precision | p. 318 |
| Specificity | p. 320 |
| Detection Limit | p. 320 |
| Quantification Limit | p. 321 |
| Linearity and Range | p. 321 |
| Robustness | p. 323 |
| Test Methods in the European Pharmacopeia | p. 325 |
| System Suitability | p. 325 |
| Adjustment of Chromatographic Conditions | p. 326 |
| Chemical Analysis of Drug Substances | p. 327 |
| What is a Pharmaceutical Raw Material, how is it Produced and why must it be Controlled? | p. 327 |
| The Pharmacopoeias - the Basis for Control of Pharmaceutical Raw Materials | p. 330 |
| Which Contaminants are Found in Raw Materials, What are the Requirements in a Maximum Content and Why? | p. 337 |
| Well Defined Chemical Compounds | p. 339 |
| Mixtures of Organic Compounds | p. 343 |
| How to Check the Identity of Pharmaceutical Raw Materials | p. 344 |
| Overview of the Identification Procedures | p. 344 |
| Techniques used for the Identification of Well Defined Chemical Compounds | p. 344 |
| Infrared Absorption Spectrophotometry | p. 344 |
| Ultraviolet and Visible Absorption Spectrophotometry | p. 347 |
| Thin-Layer Chromatography | p. 351 |
| Melting Point | p. 352 |
| Polarimetry | p. 353 |
| High Performance Liquid Chromatography | p. 356 |
| Chloride and Sulfate Identification | p. 359 |
| How to Test for Impurities in Pharmaceutical Raw Materials | p. 359 |
| Main Purity Tests for Well Defined Chemical Compounds | p. 359 |
| Appearance of Solution | p. 361 |
| Absorbance | p. 364 |
| Acidity/Alkalinity | p. 365 |
| Optical Rotation | p. 365 |
| Related Substances | p. 366 |
| Solvent Residues | p. 372 |
| Foreign Anions | p. 372 |
| Cationic Impurities | p. 376 |
| Loss on Drying | p. 378 |
| Determination of Water | p. 379 |
| Purity Tests for Raw Materials of the Type of Mixtures of Organic Compounds | p. 382 |
| Oxidizing Substances | p. 383 |
| Acid Value | p. 383 |
| Hydroxyl Value | p. 384 |
| Iodine Value | p. 384 |
| Peroxide Value | p. 385 |
| Saponification Value | p. 385 |
| Unsaponifiable Matter | p. 386 |
| Other Tests | p. 386 |
| Identification of the Raw Materials of the Type of Mixtures of Organic Compounds | p. 388 |
| How to Determine the Purity of Pharmaceutical Raw Materials | p. 389 |
| Acid-Base Titration in Aqueous Environment | p. 389 |
| Acid-Base Titration in a Non-Aqueous Environment | p. 393 |
| Redox Titrations | p. 396 |
| High Performance Liquid Chromatography | p. 396 |
| UV spectrophotometry | p. 401 |
| How to Control Compounds for Which no Pharmacopoeia Monograph Exists | p. 402 |
| How are Ph.Eur. and USP Updated? | p. 402 |
| Chemical Analysis of Final Pharmaceutical Products | p. 405 |
| Quality Control of Final Pharmaceutical Products | p. 405 |
| Monographs and Chemical Testing | p. 406 |
| Identification of the Active Pharmaceutical Ingredient | p. 412 |
| Assay of the Active Pharmaceutical Ingredient | p. 427 |
| Chemical Tests for Final Pharmaceutical Products | p. 446 |
| Test for Related Substances | p. 446 |
| Uniformity of Content | p. 449 |
| Dissolution | p. 451 |
| Analysis of Drugs in Biological Fluids | p. 453 |
| Introduction | p. 453 |
| Drug Development | p. 453 |
| Therapeutic Drug Monitoring | p. 455 |
| Forensic and Toxicological Analysis | p. 456 |
| Doping Control Analysis | p. 457 |
| The Biological Matrix | p. 458 |
| Bioanalytical Methods | p. 460 |
| Sampling | p. 460 |
| Sample Preparation | p. 461 |
| Protein Precipitation | p. 462 |
| Liquid-Liquid Extraction | p. 463 |
| Solid-Phase Extraction | p. 463 |
| Separation | p. 464 |
| Detection | p. 464 |
| Calibration and Quantification | p. 465 |
| Examples | p. 466 |
| Sample Preparation | p. 466 |
| Sample Preparation Procedure by LLE | p. 466 |
| Comments to the Procedure | p. 466 |
| Sample Preparation Procedure by LLE and Back Extraction | p. 467 |
| Comments to the Procedure | p. 467 |
| Sample Preparation Procedure by SPE | p. 467 |
| Comments to the Procedure | p. 468 |
| Sample Preparation Procedure by Protein Precipitation | p. 468 |
| Comments to the Procedure | p. 468 |
| Quantitative Determination | p. 468 |
| Quantitative Determination of Amitriptyline in Serum by LC-MS | p. 468 |
| Comments to the Procedure | p. 469 |
| Determination of Valproic Acid in Serum by GC-MS | p. 471 |
| Comments to the Procedure | p. 471 |
| Identification | p. 472 |
| Sample Preparation Procedure for Unknown Screening by Mixed Mode Cation Exchange | p. 472 |
| Comments to the Procedure | p. 472 |
| GC-MS Procedure for Unknown Screening | p. 473 |
| Comments to the Procedure | p. 473 |
| LC-MS-MS Procedure for Unknown Screening | p. 475 |
| Comments to the Procedure | p. 475 |
| Index | p. 477 |
| Table of Contents provided by Publisher. All Rights Reserved. |
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