Solid-State Properties of Pharmaceutical Materials

Name: Solid-State Properties of Pharmaceutical Materials
Brand: Wiley
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Stephen R. Byrn George Zografi Xiaoming (Sean) Chen(Autor*in)

Wiley (Verlag)

Erschienen am 12. Juli 2017

432 Seiten

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Inhalt

Intro
Solid-State Properties of Pharmaceutical Materials
Contents
Preface
Acknowledgments
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
2 Polymorphs
2.1 Introduction
2.2 How Are Polymorphs Formed?
2.3 Structural Aspect of Polymorphs
2.3.1 Configurational Polymorphs
2.3.2 Conformational Polymorphs
2.4 Physical, Chemical, and Mechanical Properties
2.4.1 Solubility
2.4.2 Chemical Stability
2.4.3 Mechanical Properties
2.5 Thermodynamic Stability of Polymorphs
2.5.1 Monotropy and Enantiotropy
2.5.2 Burger and Rambergers Rules
2.5.3 vant Hoff Plot
2.5.4 DG/Temperature Diagram
2.6 Polymorph Conversion
2.6.1 Solution-Mediated Transformation
2.6.2 Solid-State Conversion
2.7 Control of Polymorphs
2.8 Polymorph Screening
2.9 Polymorph Prediction
References
3 Solvates and Hydrates
3.1 Introduction
3.2 Pharmaceutical Importance of Hydrates
3.3 Classification of Pharmaceutical Hydrates
3.4 Water Activity
3.5 Stoichiometric Hydrates
3.6 Nonstoichiometric Hydrates
3.7 Hydration/Dehydration
3.8 Preparation and Characterization of Hydrates and Solvates
References
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 Salt Selection
References
5 Pharmaceutical Cocrystals
5.1 Introduction
5.2 Cocrystals and Crystal Engineering
5.3 Solubility Phase Diagrams For Cocrystals
5.4 Preparation of Cocrystals
5.5 Dissolution and Bioavailability of Cocrystals
5.6 Comparison of Pharmaceutical Salts and Cocrystals
References
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
6.6.1 Overview of Molecular Mobility
6.6.2 Viscosity and Molecular Mobility
6.6.3 Relaxation Time
6.6.4 Fragility in Supercooled Liquids
6.6.5 Diffusive Relaxation Time in the Glassy State
6.6.6 Secondary Relaxations in Amorphous Solids
6.7 Mixtures of Amorphous Solids
6.7.1 Overview
6.7.2 Thermodynamics of Molecular Mixing in Amorphous Solids
6.7.3 The Glass Transition Temperature and Molecular Mobility of Miscible Amorphous Mixtures
References
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
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
8.5.1 Diffraction of X-Rays
8.5.2 Experimental Measurements
8.5.3 Determination of Space Group Symmetry
8.5.4 Calculation of the Density of the Crystal
8.5.5 Structure Determination
8.5.6 Crystal Packing Drawings
8.5.7 Atomic Displacement Parameters and Molecular Mobility
8.5.8 Variable Temperature X-Ray Studies
References
9 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 Diffractometers
9.10 Variable Temperature XRPD
References
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
10.3.1 Melting
10.3.2 Glass Transition in Amorphous Solids
10.3.3 Enthalpy Relaxation for Amorphous Solids
10.3.4 Crystallization
10.3.5 Crystal Form Transitions
10.3.6 Desolvation/Dehydration
10.3.7 Chemical Degradation
10.4 DSC Instrumentation
10.4.1 Heat Flux DSC
10.4.2 Power-Compensated DSC
10.4.3 Modulated DSC
10.4.4 Fast Scan DSC
10.4.5 Operation of DSC Instrumentation
10.5 Thermogravimetric Analysis
10.6 Operating a TGA Instrument
10.7 Evolved Gas Analysis
10.8 Applications of DSC and TGA
10.8.1 The Study of Polymorphs, Solvates, and Hydrates
10.8.2 Polymer Characterization
10.8.3 Characterization of Amorphous Forms and Amorphous Solid Dispersions
10.8.4 Dehydration and Desolvation Kinetics
10.8.5 Optimization of the Freezing-Drying Cycle in Lyophilization
10.8.6 Determination of Chemical Purity of Organic Compounds
10.8.7 Study of Solid-State Reactions
10.8.8 Characterization of Macromolecules and Their Interactions
10.9 Summary of Using DSC and TGA
References
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
11.7.1 Amorphous and Crystalline Materials
11.7.2 Characterization of Polymorphs, Hydrates, and Solvates
11.7.3 Polymorph Conversion
11.7.4 Control of Crystallization
11.7.5 Screening for Cocrystals
11.7.6 Analysis of Particle Size
11.7.7 Contaminant Analysis
11.8 Scanning Electron Microscope
11.9 Environmental Scanning Electron Microscopy
11.10 Atomic Force Microscopy
References
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
12.14.1 Spectral Information
12.14.2 Spectral Resolution
12.14.3 Sampling
12.14.4 Environmental Control
12.14.5 Microscopy
12.14.6 Florescence and Photodamage
References
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 Pharmaceutical Analysis
13.5.1 Interrupted Decoupling for Protonated CarbonAtoms
13.5.2 Bloch-Decay Experiments for Screening Submolecular Mobility
13.6 Determination of the Domain Structure of Amorphous Dispersions Using Solid-State NMR
References
14 Particle and Powder Analysis
14.1 Introduction
14.2 Particles in Pharmaceutical Systems
14.2.1 Micelles
14.2.2 Protein Aggregates
14.2.3 Liposomes
14.2.4 Microemulsions
14.2.5 Nanoemulsions
14.2.6 Nanosuspensions
14.2.7 Nanoparticles
14.2.8 Aerosols
14.2.9 Emulsions
14.2.10 Suspensions
14.2.11 Powders
14.2.12 Granules
14.2.13 Pellets
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 Powders
14.11 Surface Area Measurement
References
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
15.4.1 Measurement of Water Content
15.4.2 Measurement of Water Vapor SorptionDesorption Isotherms
15.5 Modes of Water Vapor Sorption
15.5.1 Introduction
15.5.2 Adsorption
15.5.3 Deliquescence
15.5.4 Capillary Condensation
15.5.5 Absorption by Amorphous Solids
References
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: Beam Bending
16.13.1 Thermomechanical Analyzer
16.13.2 Dynamic Mechanical Analyzer
16.14 Nanoindentation
References
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 Nonsink Dissolution Test
17.12 Intrinsic Dissolution Studies
References
18 Physical Stability of Solids
18.1 Introduction
18.2 Underlying Basis for Physical Instability in Pharmaceutical Systems
18.3 Disorder in Crystals
18.3.1 Quantitative Determination of Partially Amorphous Material in Crystals
18.3.2 Solvent-Mediated Phase Transformations
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
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
19.3.1 Some General Principles Governing the Rates of Solid-State Reactions
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
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
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 Cocrystal Screening
21.6 Polymorph Screening
21.7 Slurrying
21.8 High Throughput Screening
21.9 Crystallization in Confined Space
21.10 Nonsolvent-Based Polymorph Screening
21.11 Polymer-Induced Heteronucleation
21.12 Physical Characterization
21.13 Thermodynamic Stability and form Selection
References
22 Mixture Analysis
22.1 Introduction
22.2 Limitations of Wet Chemistry
22.3 Pharmaceutical Analysis in the Solid State
22.3.1 Sample Preparation
22.3.2 Data Collection
22.3.3 Data Transformation
22.3.4 Development and Validation of a Calibration Model
22.4 Measurement of Amorphous Content
22.5 Detection of the Degree of Crystallinity
22.6 Quantification of Mixtures of Polymorphs
22.7 Salt and Free Form Composition
22.8 Process Analytical Technology
22.8.1 Physical and Chemical Attributes of a Process
22.8.2 Selection of Process Analyzers
22.8.3 Location of the Process Analyzer
22.8.4 Development of Analytical Models for Process Monitoring
22.8.5 Validation
References
23 Product Development
23.1 Chemistry, Manufacture, and Control
23.2 Preformulation
23.3 Drug Excipient Compatibility
23.4 Solid Dispersions
23.5 Abuse-Deterrent Dosage Forms
23.6 Drug-Eluting Stents
23.7 Dry Powder Inhalers (DPI)
23.8 Lyophilization and Biopharmaceutical Products
References
24 Quality by Design
24.1 Introduction
24.2 Quality by Design Wheel
24.3 Learning Before Doing
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 IVIVC for Quality by Design
24.10 Conclusion
References
Index
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