Solid-State Properties of Pharmaceutical Materials

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

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• Engenharia química