Contents. Contributors. 1 Quality control and regulation 1 C.J. MOORES

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1 Contents Contributors Preface xiii xiv 1 Quality control and regulation 1 C.J. MOORES 1.1 Introduction The quality of medicines The meaning of quality Medicines are special End-product testing General quality system requirements ISO UKAS NAMAS Good laboratory practice (GLP) Organisation for economic co-operation and development (OECD) GLP guide Principles of GLP Good manufacturing practice (GMP) USA GMP regulations EU/UK GMP requirements USA/EU GMP differences International GMPs International harmonisation of quality standards Quality control, quality assurance and regulatory filings Pre-clinical development Early phase development (Phases I/II) Late phase development (Phase III) Commercial manufacture Regulatory inspection key areas Inspection of analytical test facilities Computerised systems (21 CFR part 11) Out-of-specification (OOS) test results System audits Conclusions and the future of regulatory scrutiny 29 References 30

2 vi CONTENTS 2 Development of achiral separation methods in pharmaceutical analysis 31 GEORGE N. OKAFO and JOHN K. ROBERTS 2.1 Introduction Historical perspective of separation methods and their uses in pharmaceutical analysis Regulatory considerations for separation methods in pharmaceutical analysis General guidance for method development in separation sciences Separation goals/objectives Nature of the sample Choosing the separation technique Sample pre-treatment and detection Developing the separation High performance liquid chromatography (HPLC) Brief historical perspective of HPLC Different modes of HPLC Key developments in HPLC Stationary phase and column technology Instrumentation Microcolumn liquid chromatography Combined HPLC methods Gas chromatography (GC) Brief historical perspective GC in pharmaceutical analysis Key developments in GC Sensitivity enhancement with large volume injection Thermally labile samples Analytes in complex matrices Detection systems Efficiency increases in GC Automation Capillary electrophoretic techniques Brief historical perspective Developments in detection modes in CE Different modes and method development options in CE Capillary zone electrophoresis Micellar electrokinetic chromatography Microemulsion electrokinetic chromatography Capillary electrochromatography 57

3 CONTENTS vii 2.6 Other separation techniques Thin layer chromatography Supercritical fluid chromatography Hyphenated separation techniques Use of automated approaches to method development in chromatography Separation optimisation programmes Column switching devices Use of chemometric approaches to method development 66 Abbreviations 67 References 68 3 Chiral analysis of pharmaceuticals 74 W. JOHN LOUGH 3.1 Significance of chirality in pharmaceutical R&D Evolution of methodologies for chiral resolution Recent developments in commercial CSP for LC Polysaccharide-based CSP Macrocyclic antibiotic CSP Synthetic multiple-interaction CSP Role of historical CSP Chiral drug bioanalysis Preparative chiral separations Present and future perspectives Alternatives to chiral LC Fit for intended purpose? The future 102 Ancillary reading 103 References 103 Commercial literature Nuclear magnetic resonance spectroscopy in pharmaceutical analysis 105 RICHARD J. SMITH and ANDREW J. EDWARDS 4.1 Introduction Structure elucidation Background and historical perspective The move to higher fields Modern 1 H NMR experiments Nuclei other than the proton C F 119

4 viii CONTENTS P O N Computer-assisted structure determination Computer-assisted interpretation Computer-assisted structure elucidation On-line separations LC/NMR Chromatographic considerations NMR mode Solvent suppression in LC/NMR Applications of LC/NMR LC/NMR/MS Capillary LC/NMR Hyphenation to other separation techniques Quantitation The basics of quantitation Optimising the experimental parameters Quantitative impurity determinations Summary of experimental considerations Method validation Solid state NMR Introduction Basic theory of solid state NMR Methods of assignment of solid state NMR spectra One-dimensional editing methods Two-dimensional solid state methods Distance measurements in the solid state recoupling Heteronuclear recoupling Homonuclear recoupling Application of solid state NMR to pharmaceuticals 153 Acknowledgements 157 References Mass spectrometry in pharmaceutical analysis 165 NEVILLE HASKINS 5.1 Introduction Mass spectrometry Sample introduction systems Ionisation techniques Electron ionisation Chemical ionisation 169

5 CONTENTS ix Electrospray Nanospray Atmospheric pressure chemical ionisation (APCI) Analysers Sectors Quadrupole analysers Quadrupole ion traps Time of flight analysers Ion cyclotron resonance mass spectrometers Hybrid instruments Ion detection systems Conversion dynode and electron multiplier Conversion dynode and photon multipliers Data acquisition and processing Strategies for structural elucidation Determination of molecular weight Collisionally induced decomposition and MS n Accurate mass measurement Structural confirmation Library searches Using MS n techniques Process monitoring Quantitation Development of an assay The calibration process Use of stable isotopically labelled substance Use of double labelling Using the data system Automation Data processing Data mining 201 References Vibrational spectroscopy in pharmaceutical analysis 203 CLARE L. ANDERTON 6.1 Introduction Molecular motion Infrared spectroscopy Instrumentation for infrared spectroscopy Sample preparation for infrared spectroscopy 204

6 x CONTENTS Raman spectroscopy Instrumentation for Raman spectroscopy Sample preparation for Raman spectroscopy Applications Vibrational spectroscopy to investigate molecular structure Introduction Techniques in structural elucidation and specialist applications Tautomerism Hydrogen bonding Chirality Contaminant analysis Products from combinatorial chemistry Theoretical calculations Routine chemical identification Vibrational spectroscopy of polymorphs, hydrates and solvates Introduction Identifying structural differences between solid-state forms Polymorphs Hydrates and solvates Amorphous material Quantifying solid-state forms in drug substance Identifying the solid-state form in formulated product Vibrational spectroscopy for in situ characterisation Investigating solid phase transformations Variable temperature spectroscopy Combining spectroscopy with other solid-state techniques Monitoring chemical reactions and processes Chromatography detection Summary 236 Acknowledgements 236 References Solid-state analysis and polymorphism 240 ULRICH J. GRIESSER and JOSEPH G. STOWELL 7.1 Introduction Solid-state properties of drug compounds Determinant levels of solid-state properties 242

7 CONTENTS xi Types and properties of pharmaceutical solids Crystalline solids Amorphous solids Regulatory aspects and quality control Methods of solid-state analysis X-ray diffraction and crystallography Spectroscopy Ultraviolet-visible diffuse reflectance spectroscopy Infrared spectroscopy Raman spectroscopy Solid-state NMR Thermal analysis and calorimetry Thermomicroscopy (hot-stage microscopy) Differential thermal analysis and differential scanning calorimetry Thermogravimetry Thermomechanical analysis Dielectric analysis Microcalorimetry Vapour pressure determination of solids Micromeritic measurements Particle-size analysis Particle shape Specific surface area Porosity Density Other technologies Atomic force microscopy Summary 289 References Microscopy and imaging in pharmaceutical analysis 295 ROBERT A. CARLTON 8.1 Introduction Solid-state analysis Early stage solid-state analysis (polymorph discovery) Optical crystallography Solvent recrystallization experiments Thermal microscopy Late stage solid-state analysis (polymorph relationships) Summary 307

8 xii CONTENTS 8.3 Particle size and morphology Particle morphology Particle size analysis/image analysis Summary Contaminant identification Conclusion 321 References Process analysis in the pharmaceutical industry 324 MARTIN WARMAN and STEVE HAMMOND 9.1 Introduction Pharmaceutical manufacturing Drug substance manufacture Raw material testing Reaction mixture Reaction monitoring Crystallisation monitoring Dryer monitoring Monitoring the milling process Cleaning monitoring Drug product manufacturing Raw material monitoring Formulation monitoring Tablet cores Tablet coating Packaging Conclusions 355 References 356 Index 357

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