Solid State Properties of Pharmaceutical Materials

Presents a detailed discussion of important solid–state properties, methods, and applications of solid–state analysis Illustrates the various phases or forms that solids can assume and discussesvarious issues related to the relative stability of solid forms and tendencies to undergo transformation Covers key methods of solid state analysis including X–ray powder diffraction, thermal analysis, microscopy, spectroscopy, and solid state NMR Reviews critical physical attributes of pharmaceutical materials, mainly related to drug substances, including particle size/surface area, hygroscopicity, mechanical properties, solubility, and physical and chemical stability Showcases the application of solid state material science in rational selection of drug solid forms, analysis of various solid forms within drug substance and the drug product, and pharmaceutical product development Introduces appropriate manufacturing and control procedures using Quality by Design, and other strategies that lead to safe and effective products with a minimum of resources and time INDICE: Preface .Acknowledgments .Chapter 1: Solid State Properties and Pharmaceutical Development .1.1 Introduction .1.2 Solid State Forms .1.3 ICH Q6A Decision Trees .1.4 Big Questions for Drug Development .1.5 Accelerating Drug Development .1.6 Solid State Chemistry in Preformulation and Formulation .1.7 Learning before Doing and Quality by Design .1.8 Performance and Stability in Pharmaceutical Development .1.9 Moisture Uptake .1.10 Solid State Reactions .1.11 Noninteracting Formulations Physical Characterizations .References .Chapter 2: Polymorphs .2.1 Introduction .2.2 How Are Polymorphs Formed? .2.3 Structural Aspect of Polymorphs .2.4 Physical, Chemical, and Mechanical Properties .2.5 Thermodynamic Stability of Polymorphs .2.6 Polymorph Cconversion .2.7 Control of Polymorphs .2.8 Polymorph Screening .2.9 Polymorph Prediction .References .Chapter 3: Solvates and Hhydrates .3.1 Introduction .3.2 Pharmaceutical Importance of Hydrates .3.3 Classification of Pharmaceutical Hydrates .3.4 Water Aactivity .3.5 Stoichiometric Hhydrates .3.6 Nonstoichiometric Hhydrates .3.7 Hydration/Dehydration .3.8 Preparation and Characterization of Hydrates and Solvates .References .Chapter 4: Pharmaceutical Salts .4.1 Introduction .4.2 Importance of Pharmaceutical Salts .4.3 Weak Acid, Weak Base, and Salt .4.4 pH–Solubility Profiles of Ionizable Compounds .4.5 Solubility, Dissolution and Bioavailability of Pharmaceutical Salts .4.6 Physical Stability of Pharmaceutical Salts .4.7 Strategies for S  salt Sselection .References .Chapter 5: Pharmaceutical Co–crystals .5.1 Introduction .5.2 Co–crystals and Crystal Engineering .5.3 Co–crystals and Crystal Engineering .5.4 Co–crystals and Crystal Engineering .5.5 Solubility Phase Diagrams for Co–crystals .5.6 Preparation of Co–crystals .5.7 Dissolution and Bioavailability of Co–crystals .5.8 Comparison of Ppharmaceutical Ssalts and Cco–crystals .References .Chapter 6: Amorphous Solids .6.1 Introduction .6.2 The Formation of Amorphous Solids .6.3 Methods of Preparing Amorphous Solids .6.4 The Glass Transition Temperature .6.5 Structural Features of Amorphous Solids .6.6 Molecular Mobility .6.7 Mixtures of Amorphous Solids .6.8 References .Chapter 7: Crystal Mesophases and Nanocrystals .7.1 Introduction .7.2 Overview of Crystal Mesophases .7.3 Liquid Crystals .7.4 Conformationally Disordered (Condis) Crystals .7.5 Plastic Crystals .7.6 Nanocrystals .References .Chapter 8: X–ray Crystallography and Crystal Packing Analysis .8.1 Introduction .8.2 Crystals .8.3 Miller Indices and Crystal Faces .8.4 Determination of the Miller Indices of the Faces of a Crystal .8.5 Determination of Crystal Structure .References .Chapter 9: X–ray Crystallography and Crystal Packing Analysis X–ray Powder Diffraction .9.1 Introduction .9.2 X–ray Powder Diffraction of Crystalline Materials .9.3 Qualitative Analysis of Crystalline Materials .9.4 Phase Transformations .9.5 Quantitative Phase Analysis Using XRPD .9.6 Solving Crystal Structures Using Powder X–ray Diffraction .9.7 X–ray Diffraction of Amorphous and Crystal Mesophase Forms .9.8 Pair Distribution Function .9.9 X–ray Ddiffractometers .9.10 Variable Ttemperature XRPD .9.11 References .Chapter 10: Differential Scanning Calorimetry and Thermogravimetric Analysis .10.1 Introduction .10.2 The Basics of Differential Scanning Calorimetry .10.3 Thermal Transitions of Pharmaceutical Materials .10.4 DSC Instrumentation .10.54 Thermogravimetric Analysis .10.65 Operating a TGA Instrument .10.76 Evolved Gas Analysis .10.87 Applications of DSC and TGA .10.8 Optimization of the Freezing–Drying Cycle in Lyophilization .10.9 Determination of Chemical Purity of Organic Compounds .References .Chapter 11: Microscopy .11.1 Introduction .11.2 Light Microscopy .11.3 Polarized Light Microscopy .11.4 Thermal Microscopy .11.5 Functionality of the Light Microscope .11.6 Digital Microscope .11.7 Application of Light Microscopy to Pharmaceutical Materials .11.8 Scanning Electron Microscope .11.9 Environmental Scanning Electron Microscopy (ESEM) .11.10 Atomic Force Microscopy .References .Chapter 12: Vibrational Spectroscopy .12.1 Introduction .12.2 The Nature of Molecular Vibrations .12.3 Fourier Transformed Infrared Spectroscopy .12.4 Material Characterization by FT–IR Spectroscopy .12.5 FT–IR Instrumentation .12.6 Diffuse Reflectance FT–IR .12.7 Attenuated Total Reflectance FT–IR .12.8 FT–IR Microscopy .12.9 Near Infrared Spectroscopy .12.10 Raman Spectroscopy .12.11 Raman Instrumentation and Sampling .12.12 Raman Microscope .12.13 Terahertz Spectroscopy .12.14 Comparison of FT–IR, NIR, Raman, and Terahertz Spectroscopy .References .Chapter 13: Solid–State NMR Spectroscopy .13.1 Introduction .13.2 An Overview of Solid–State 13C CP/MAS NMR Spectroscopy .13.3 Solid State NMR Studies of Pharmaceuticals .13.4 Phase Identification in Dosage Forms .13.5 Other Basic Solid–State NMR Experiments Useful for Pharmaceu–tical Analysis .13.6 Determination of the Domain Structure of Amorphous Dispersions Using SSNMR .References .Chapter 14: Particle and Powder Analysis .14.1 Introduction .14.2 Particles in Pharmaceutical Systems .14.3 Particle Size and Shape .14.4 Particle Size Distribution .14.5 Dynamic Light Scattering .14.6 Zeta Potential .14.7 Laser Diffraction .14.8 Dynamic Image Analysis .14.9 Sieve Analysis .14.10 Bulk Properties of Pharmaceutical Particulates and Powder .14.11 Surface Area Measurement .References .Chapter 15: Hygroscopic Properties of Solids .15.1 Introduction .15.2 Water Vapor Sorption–Desorption .15.3 Water Vapor Sorption Isotherms, Relative Humidity and Water Activity .15.4 Measurement of Water Content and Water Vapor Sorption/Desorption Isotherms .15.5 Measurement of Water Vapor Sorption/Desorption Isotherms .15.56 Modes of Water Vapor Sorption .References .Chapter 16: Mechanical Properties of Pharmaceutical Materials .16.1 Introduction .16.2 Stress and Strain .16.3 Elasticity .16.4 Plasticity .16.5 Viscoelasticity .16.6 Brittleness .16.7 Hardness .16.8 Powder Compression .16.9 Powder Compression Models and Compressibility .16.10 Compactibility and Tensile Strength .16.11 Effect of Solid Form on Mechanical Properties .16.12 Effect of Moisture on Mechanical Properties .16.13 Methods  for Testing Mechanical Properties .16.14 Nanoindention .References .Chapter 17: Solubility and Dissolution .17.1 Introduction .17.2 Principle Concepts Associated with Solubility .17.3 Prediction of Aqueous Drug Solubility .17.4 Solubility of Pharmaceutical Solid Forms .17.5 Solubility Determination Using the Shake Flask Method .17.6 High Throughput Screening of Solubility .17.7 Solubility Measurement of Metastable Forms .17.8 Kinetic Solubility Measurement .17.9 Solubility Determination of Drugs in Polymer Matrices .17.10 Dissolution Testing .17.11 Non–sink Dissolution  Test .17.12 Intrinsic Dissolution Studies .References .Chapter 18: Physical Stability of Solids .18.1 Introduction .18.2 Underlying Basis for Physical Instability in Pharmaceutical Systems .18.3 Disorder in Crystals .18.4 Examples of the Role of Process–Induced Disorder in Solid–State Physical Instability in Pharmaceutical Systems .18.5 Considerations in Evaluating Solid–State Physical Stability .References .Chapter 19: Chemical Stability of Solids .19.1 Introduction .19.2 Examples of Chemical Reactivity in the Solid State .19.3 Some General Principles That Establish the Rate of Chemical Reactions in Solution .19.4 The Role of Crystal Defects in Solid–State Reactions .19.5 Chemical Reactivity in the Amorphous Solid State .19.6 Chemical Reactivity and Processed–Induced– Disorder .19.7 The Effects of Residual Water on Solid–State Chemical Reactivity .19.8 Drug– Excipient Interactions .19.9 Summary .References .Chapter 20: Solid–State Properties of Proteins .20.1 Introduction .20.2 Solution Properties of Proteins .20.3 Amorphous Properties of Proteins .20.4 Crystalline Properties of Proteins .20.5 Local Molecular Motions and the Dynamical Transitional Temperature, Td .20.6 Solid–State Physical and Chemical Stability of Proteins .20.7 Cryoprotection and Lyoprotection .References .Chapter 21: Form Selection of Active Pharmaceutical Ingredients .21.1 Introduction .21.2 Form Selection .21.3 Amorphous Form Screening .21.4 Salt Selection .21.5 Co–crystal Screening .21.6 Polymorph Screening .21.7 Slurrying .21.8 High–throughput Screening .21.9 Crystallization in Cconfined Sspace .21.10 Non–solvent Based Polymorph Screening .21.11 Polymer Induced Heteronucleation .21.12 Physical Characterization .21.13 Thermodynamic Stability and Form Selection .References .Chapter 22: Mixture Analysis .22.1 Introduction .22.2 Limitations of Wet Chemistry .22.3 Pharmaceutical Analysis in the Solid State .22.4 Development and Validation of a Calibration Model .22.5 Measurement of Amorphous Content .22.6 Detection of the Degree of Crystallinity .22.7 Quantification of Mixtures of Polymorphs .22.8 Salt and Free Form Composition .22.9 Process Analytical Technology (PAT) .22.10 Physical and Chemical Attributes of a Process .22.11 Selection of Process Analyzers .References .Chapter 23: Product Development .23.1 Chemistry, Manufacture, and Control (CMC) .23.2 Preformulation .23.3 Drug Excipient Compatibility .23.4 Solid Dispersions .23.5 Abuse–Deterrent Dosage Forms .23.6 Drug Eluting Stents (DES) .23.7 Dry Powder Inhalers (DPI) .23.8 Lyophilization and Biopharmaceutical Products .References .Chapter 24: Quality by Design .24.1 Introduction .24.2 Quality by Design Wheel .24.3 Learning before Doing (LbD) .24.4 Risk Based Orientation .24.5 API Attributes and Process Design .24.6 Development and Design Space .24.7 Process Design Crystallization .24.8 Phase Transformations during Wet Granulation .24.9 Dissolution Tests with an In–Vitro in–Vivo Correlation (IVIVC) for Quality by Design .24.10 Conclusion .References

• ISBN: 978-1-118-14530-2
• Editorial: Wiley–Blackwell
• Encuadernacion: Cartoné
• Páginas: 496
• Fecha Publicación: 09/06/2017
• Nº Volúmenes: 1
• Idioma: Inglés