Pharmaceutical Analysis

A Textbook for Pharmacy Students and Pharmaceutical Chemists

5th Edition - June 10, 2020
Imprint: Elsevier
Author: David G. Watson
Language: English
Paperback ISBN:
9 7 8 - 0 - 7 0 2 0 - 7 8 0 8 - 8
Paperback ISBN:
9 7 8 - 0 - 7 0 2 0 - 7 8 0 7 - 1

Pharmaceutical analysis determines the purity, concentration, active compounds, shelf life, rate of absorption in the body, identity, stability, rate of release etc. of a drug. Te… Read more

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Pharmaceutical analysis determines the purity, concentration, active compounds, shelf life, rate of absorption in the body, identity, stability, rate of release etc. of a drug. Testing a pharmaceutical product involves a variety of analyses, and the analytical processes described in this book are used in industries as diverse as food, beverages, cosmetics, detergents, metals, paints, water, agrochemicals, biotechnological products and pharmaceuticals.
The mathematics involved is notoriously difficult, but this much-praised and well established textbook, now revised and updated for its fifth edition, guides a student through the complexities with clear writing and the author's expertise from many years' teaching pharmacy students.

Instructions for online access
Cover image
Title page
Table of Contents
Copyright
Learning resources
1. Control of the quality of analytical methods
Introduction
Control of errors in analysis
Accuracy and precision
Validation of analytical procedures
Standard operating procedure for the assay of paracetamol tablets
Compound random errors
Reporting of results
Other terms used in the control of analytical procedures
Basic calculations in pharmaceutical analysis
2. Physical and chemical properties of drug molecules
Introduction
Calculation of pH value of aqueous solutions of strong and weak acids and bases
Acidic and basic strength and pKa
Henderson–Hasselbalch equation
Ionization of drug molecules
Buffers
Salt hydrolysis
Activity, ionic strength and dielectric constant
Partition coefficient
Drug stability
Stereochemistry of drugs
Measurement of optical rotation (Animation 2.2)
Profiles of physico-chemical properties of some drug molecules
3. Titrimetric and chemical analysis methods
Introduction
Instrumentation and reagents
Direct acid/base titrations in the aqueous phase
Titrations of the salts of weak bases in mixed aqueous/non-aqueous media
Indirect titrations in the aqueous phase
Non-aqueous titrations
Argentometric titrations
Complexometric titrations
Redox titrations
Iodometric titrations
Ion pair titrations
Diazotization titrations
Potentiometric titrations
Karl Fischer titration (coulometric end-point detection)
Automation of wet chemical methods
Applications of FIA in pharmaceutical analysis
4. Ultraviolet and visible spectroscopy
Introduction
Factors governing absorption of radiation in the UV/visible region (Animations 4.1 and 4.2)
Beer–Lambert Law
Instrumentation
Diode array instruments
Instrument calibration
UV spectra of some representative drug molecules
Use of UV/visible spectrophotometry to determine pKa values
Applications of UV/visible spectroscopy to pharmaceutical quantitative analysis
Difference spectrophotometry
Derivative spectra
Applications of UV/visible spectroscopy in preformulation and formulation
5. Infrared spectrophotometry
Introduction
Factors determining intensity and energy level of absorption in IR spectra
Instrumentation
Sample preparation
Application of IR spectrophotometry in structure elucidation
Examples of IR spectra of drug molecules
IR spectrophotometry as a fingerprint technique
IR spectrophotometry as a method for identifying polymorphs
Near-infrared analysis (NIRA)
Introduction
Examples of NIRA applications
6. Atomic spectrophotometry
Atomic emission spectrophotometry
Introduction
Instrumentation
Examples of quantitation by AES
Interferences in AES analysis (see Animation 6.3)
Assays based on the method of standard additions
Atomic absorption spectrophotometry (AAS)
Introduction
Instrumentation
Examples of assays using AAS (Animation 6.4)
Some examples of limit tests employing AAS
Inductively coupled plasma emission spectroscopy
7. Molecular emission spectroscopy
Fluorescence spectrophotometry
Introduction
Instrumentation
Molecules that exhibit fluorescence
Factors interfering with fluorescence intensity
Applications of fluorescence spectrophotometry in pharmaceutical analysis
Raman spectroscopy
Introduction
8. Nuclear magnetic resonance spectroscopy
Introduction
Instrumentation
Proton (1H) NMR
Application of NMR to structure confirmation in some drug molecules
Carbon NMR
Two-dimensional NMR spectra
Application of NMR to quantitative analysis
Other specialized applications of NMR
9. Mass spectrometry
Introduction
Ion generation
Other ionization methods
Ion separation techniques
A more detailed consideration of mass spectra
Molecular fragmentation patterns
Gas chromatography–mass spectrometry
Applications of GC–MS with EI
Tandem MS (Animation 9.11)
High-resolution mass spectrometry
Mass spectrometry of proteins
Mass spectrometry in drug discovery
10. Chromatographic theory
Introduction
Void volume and capacity factor
Calculation of column efficiency
Origins of band broadening in HPLC
Parameters used in evaluating column performance
Data acquisition
Report generation
11. Gas chromatography
Introduction
Instrumentation
Selectivity of liquid stationary phases
Use of derivatization in GC
Summary of parameters governing capillary GC performance
GC detectors
Applications of GC in quantitative analysis
Determination of manufacturing and degradation residues by GC
Determination of residual solvents
Solid-phase microextraction (SPME) (Animation 11.3)
Applications of GC in bioanalysis
12. High-performance liquid chromatography
Introduction
Instrumentation (Animations 12.2 and 12.3)
Stationary and mobile phases
Structural factors which govern rate of elution of compounds from HPLC columns
More advanced consideration of solvent selectivity in reverse-phase chromatography
Effect of temperature on HPLC
Summary of stationary phases used in HPLC
A more advanced consideration of reverse-phase stationary phases
Summary of detectors used in HPLC
Performance of a diode array detector
Applications of HPLC to the quantitative analysis of drugs in formulations
Assays involving more specialized HPLC techniques
13. Thin-layer chromatography
Introduction
Instrumentation
TLC chromatogram
Stationary phases
Elutropic series and mobile phases
Modification of TLC adsorbant
Detection of compounds on TLC plates following development
Applications of TLC analysis
High-performance TLC (HPTLC)
14. High-performance capillary electrophoresis
Introduction
Instrumentation
Control of separation
Applications of CE in pharmaceutical analysis
Use of additives in the running buffer
15. Extraction methods in pharmaceutical analysis
Introduction
Commonly used excipients in formulations
Tablets and capsules
Solvent extraction methods
Microdialysis extraction
Solid-phase extraction (SPE)
Introduction
Methodology
Types of adsorbants used in SPE
Typical extraction methodologies using lipophilic silica gels
Adaptation of SPE for automated on-line extraction prior to HPLC analysis
Recent developments in solid-phase and on-line extraction
16. Methods used in the quality control of biotechnologically produced drugs
Protein drugs
Protein structure
Instrumental techniques used in the analysis of biotechnologically produced drugs
17. Electrochemical biosensors
Introduction
Basic principles of electrochemistry
Types of electrochemical biosensors
Instrumentation
Examples of biosensors utilized for pharmaceutical analysis
Limitations of biosensors in pharmaceutical analysis
Index

Life Sciences

Physical Sciences & Engineering

Social Sciences & Humanities

Health