Introduction to Pharmaceutical Chemical Analysis

, by Hansen, Steen; Pedersen-Bjergaard, Stig; Rasmussen, Knut

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ISBN: 9780470661222 | 0470661224
Cover: Paperback
Copyright: 12/12/2011

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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

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
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Introduction to Pharmaceutical Chemical Analysis

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