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Pharmaceutical Analysis

Book Description

Pharmaceutical Analysis is a compulsory subject offered to all the under graduate students of Pharmacy. This book on Pharmaceutical Analysis has been designed considering the syllabi requirements laid down by AICTE and other premier institutes/universities. The book covers both the Titrimetric and Instrumental aspects of Pharmaceutical analysis which is helpful for use in multiple semesters.

Table of Contents

  1. Cover
  2. Title Page
  3. Brief Contents
  4. Contents
  5. Dedication
  6. Foreword
  7. Preface
  8. Unit I – Introduction to Analysis
    1. 1. Introduction to Pharmaceutical Analysis
      1. Introduction
      2. Introduction to Titrimetry
      3. Introduction to Electroanalytical Methods
      4. Introduction to Spectroscopy
      5. Introduction to Chromatography
      6. Statistical Analysis
      7. Review Questions
  9. Unit II – Physical Analytical Methods
    1. 1. Solubility Determinations
      1. Introduction
      2. Classification of Solutions
      3. Factors Affecting Solubility
      4. Theory
      5. Applications
      6. Review Questions
    2. 2. Molecular Weight Determinations
      1. Introduction
      2. Review Questions
    3. 3. Viscosity Determination
      1. Introduction
      2. Factors Affecting Viscosity
      3. Types of Viscometers
      4. Units for the Viscosity
      5. Applications
      6. Review Questions
    4. 4. Surface Tension Determination
      1. Introduction
      2. Factors Affecting Surface Tension
      3. Methods for Determining Surface Tension
      4. Applications
      5. Review Questions
    5. 5. Particle Size Analysis
      1. Introduction
      2. Methods for Particle Size Analysis
      3. Applications
      4. Review Questions
    6. 6. X-ray Diffractometry
      1. Introduction
      2. Principle
      3. Theory
      4. Instrumentation
      5. Types of X-ray Diffraction Methods
      6. Advantages
      7. Disadvantages
      8. Applications
      9. Review Questions
    7. 7. Polarimetry
      1. Introduction
      2. Theory
      3. Concept of the Circular Dichroism (CD) and Optical Rotatory Dispersion (ORD)
      4. Instrumentation
      5. Applications
      6. Advantages
      7. Disadvantages
      8. Review Questions
    8. 8. Refractometry
      1. Introduction
      2. Principle and Theory
      3. Instrumentation
      4. Factors Affecting the Refractive Index
      5. Applications
      6. Review Questions
  10. Unit III – Titrimetric Methods
    1. 1. Acid-base Titrations (Neutralization Titrations)
      1. Introduction
      2. Acid-base Concept
      3. Role of the Solvent
      4. Strengths of Acids and Bases
      5. Law of Mass Action
      6. Handerson-Hesselbach Equation
      7. Types of Acid-base Titrations and Titration Curves
      8. Indicators
      9. Applications
      10. Review Questions
    2. 2. Non-aqueous Titrations
      1. Introduction
      2. Principle
      3. Theory
      4. Types of Non-aqueous Solvents
      5. Preperation and Standardisation of Standard Solutions
      6. Factors Affecting the Non-aqueous Titrations
      7. Different Theories of Non-aqueous Titrations
      8. Interference of the Water in Non-aqueous Titrimetry
      9. Advantages
      10. Disadvantages
      11. Applications
      12. Review Questions
    3. 3. Redox Titration
      1. Introduction
      2. Principle
      3. Theory
      4. Oxidising and Reducing Agents
      5. Factors Affecting Redox Titrations
      6. Redox Indicators
      7. Types of Redox Titrations
      8. Titration Curve
      9. Procedure Followed for Redox Titration
      10. Applications
      11. Review Questions
    4. 4. Diazotization Titrations
      1. Introduction
      2. Principle
      3. Theory
      4. Procedure
      5. End Point Detection
      6. Factors Affecting the Diazotization
      7. Conditions for the Diazotization Titration
      8. Advantages
      9. Disadvantages
      10. Applications
      11. Review Questions
    5. 5. Complexometry
      1. Introduction
      2. Principle
      3. Theory
      4. Ligands
      5. Chelating Agents
      6. Determination of the End Point
      7. End Point Detection Methods
      8. Types of Complexometric Titrations
      9. Concept of Werner Co-ordination Number
      10. Concept of Masking and Demasking Agents
      11. Factors Affecting the Titration Values
      12. Applications
      13. Review Questions
    6. 6. Gravimetry
      1. Introduction
      2. Principle
      3. Theory
      4. Mechanism of the Precipitation
      5. Types of Gravimetry
      6. Impurities Present in the Precipitates
      7. Advantages
      8. Disadvantages
      9. Applications
      10. Review Questions
    7. 7. Precipitation Titrations
      1. Introduction
      2. Theory
      3. Types of the Precipitation Titrations
      4. Factors Affecting the Precipitation Titrations
      5. Advantages
      6. Disadvantages
      7. Applications
      8. Review Questions
    8. 8. Miscellaneous Titrations
      1. Argentometry
      2. Advantages
      3. Disadvantages
      4. Applications
      5. Iodometry and Iodimetry
      6. Applications
      7. Review Questions
  11. Unit IV – Electroanalytical Methods
    1. 1. Electrogravimetry
      1. Introduction
      2. Principle
      3. Theory
      4. Applications
      5. Review Questions
    2. 2. Conductometry
      1. Introduction
      2. Principle
      3. Theory
      4. Apparatus
      5. Method
      6. Factors Affecting the Conductivity Measurements
      7. Advantages
      8. Disadvantages
      9. Applications
      10. Review Questions
    3. 3. Coulometry
      1. Introduction
      2. Principle
      3. Theory
      4. Instrumentation
      5. Applications
      6. Review Questions
    4. 4. Potentiometry
      1. Introduction
      2. Principle
      3. Theory
      4. Electrodes
      5. Potentiometric Titrations
      6. Instruments
      7. Advantages
      8. Disadvantages
      9. Applications
      10. Review Questions
    5. 5. Voltammetry
      1. Introduction
      2. Polarography
      3. Advantages
      4. Disadvantages
      5. Applications
      6. Amperometry
      7. Advantages
      8. Disadvantages
      9. Applications
      10. Review Questions
  12. Unit V – Spectroanalytical Methods
    1. 1. Spectrophotometry-UV/Visible Spectroscopy
      1. Introduction
      2. The Electromagnetic Spectrum
      3. Theory
      4. Beer–Lamber's Law
      5. Instrumentation
      6. Spectrophotometers
      7. The Origins of Absorption Spectra
      8. Solvent Effects
      9. Selection of Solvents
      10. Good Operating Practice
      11. Sources of Error
      12. Applications
      13. Experiments
      14. Review Questions
    2. 2. Infrared Spectrophotometry
      1. Introduction
      2. Theory
      3. Types of Vibrations
      4. Instrumentation
      5. Interpretation of the IR Spectra
      6. Limitations of IR Spectroscopy
      7. Advantages
      8. Disadvantages
      9. Applications of IR Spectroscopy
      10. Fourier Transform Infrared Spectroscopy (FTIR)
      11. Introduction
      12. Principle
      13. Instrumentation
      14. Advantages of FTIR
      15. Limitations of FTIR
      16. Applications
      17. Review Questions
    3. 3. Spectro Fluorimetry and X-ray Fluorescence Spectroscopy
      1. Introduction
      2. Principle
      3. Theory
      4. Types of Fluorescence
      5. Instrumentation
      6. Factors Affecting the Fluorescence Intensity
      7. Concept of Quenching
      8. Fluorescence Spectrum
      9. Advantages
      10. Limitations
      11. Applications
      12. Review Questions
      13. X-ray Fluorescence Spectroscopy
      14. Introduction
      15. Theory
      16. Instrumentation
      17. Advantages
      18. Disadvantages
      19. Applications
      20. Review Questions
    4. 4. Atomic Absorption Spectroscopy
      1. Introduction
      2. Principle
      3. Theory
      4. Instrumentation
      5. Interferences in AAS
      6. Advantages
      7. Disadvantages
      8. Applications
      9. Review Questions
    5. 5. Flame Photometry
      1. Introduction
      2. Principle and Theory
      3. Principle
      4. Instrumentation for Flame Photometry
      5. Applications of Flame Photometry
      6. Interferences in Quantitative Determinations
      7. Merits and Limitations of Flame Photometry
      8. Limitations
      9. Advantages
      10. Review Questions
    6. 6. Mass Spectrometry
      1. Introduction
      2. Principle
      3. Theory
      4. Instrumentation
      5. Advantages
      6. Disadvantages
      7. Advantages
      8. Disadvantages
      9. Advantages
      10. Disadvantages
      11. Types of Mass Spectrometry
      12. Advantages
      13. Disadvantages
      14. Applications
      15. Review Questions
    7. 7. Nuclear Magnetic Resonance Spectroscopy
      1. Introduction
      2. Principle and Theory
      3. Chemical Shift
      4. Instrumentation
      5. Solvents Requirements
      6. Advantages
      7. Disadvantages
      8. Applications
      9. Review Questions
    8. 8. Electron Spin Resonance Spectroscopy
      1. Introduction
      2. Theory
      3. Relaxation and Saturation
      4. Instrumentation
      5. Double Resonance Spectrometers
      6. Interpretation of Derivative Curves in ESR
      7. Applications
      8. Advantages
      9. Disadvantages
      10. Review Questions
    9. 9. Plasma Emission Spectroscopy
      1. Introduction
      2. Principle
      3. Theory
      4. Instrumentation
      5. Advantages
      6. Limitations
      7. Applications
      8. Review Questions
    10. 10. Nephelometry and Turbidimetry
      1. Introduction
      2. Principle
      3. Theory
      4. Factors Affecting Measurement
      5. Instrumentation
      6. Applications of Nephlometry and Turbidimetry
      7. Review Questions
  13. Unit VI – Chromatographic Techniques
    1. 1. Paper Chromatography
      1. Introduction
      2. Principle
      3. Theory
      4. Types of Paper Chromatography
      5. Detection of the Spots in Paper Chromatography
      6. Advantages
      7. Disadvantages
      8. Applications
      9. Review Questions
    2. 2. Column Chromatography
      1. Introduction
      2. Principle
      3. Theory
      4. Factors Affecting the Column Efficiency
      5. Advantages
      6. Disadvantages
      7. Applications
      8. Review Questions
    3. 3. Thin Layer Chromatography
      1. Introduction
      2. Principle
      3. Theory
      4. The Process of TLC
      5. Advantages of TLC Over Other Techniques
      6. Disadvantages of TLC
      7. Trouble Shooting in TLC
      8. Applications
      9. Review Questions
    4. 4. High-Performance Liquid Chromatography
      1. Introduction
      2. Types of HPLC Techniques
      3. Instrumentation for HPLC
      4. The Rate Theory of Chromatography
      5. Advantages of HPLC
      6. Disadvantages of HPLC
      7. HPLC Trouble Shooting
      8. Applications of HPLC
      9. Review Questions
    5. 5. Ion Exchange Chromatography
      1. Introduction
      2. Principle
      3. Theory
      4. Instrumental Components (or) Instrumentation
      5. Ion Exchange Resins Efficiency Parameters
      6. Advantages of IEC
      7. Applications
      8. Review Questions
    6. 6. Gas Chromatography
      1. Introduction
      2. Principle and Theory
      3. Types of GC
      4. Instrumentation
      5. Factors that Affect GC Separations
      6. Parameters
      7. Advantages
      8. Disadvantages
      9. Applications
      10. Review Questions
    7. 7. Vapour Phase Chromatography
      1. Introduction
      2. Theory
      3. Instrumentation
      4. Parameters Checked for the VPC
      5. Procedure
      6. Factors Effecting Elution Time and Resolution Power
      7. Applications
      8. Review Questions
    8. 8. Supercritical Fluid Chromatography
      1. Introduction
      2. Theory
      3. Important Properties of SCFs
      4. Advantages
      5. Disadvantages
      6. Instrumentation
      7. Categorisation of SFC
      8. Advantages of SCF Over HPLC and GC
      9. Limitations
      10. Precautions
      11. Comparison of SFC with HPLC and GC
      12. Applications of SFC
      13. Review Questions
    9. 9. Affinity Chromatography
      1. Introduction
      2. Classification of Affinity Chromatography
      3. General Procedure for the Development of Affinity Chromatography
      4. Advantages of Affinity Chromatography
      5. Factors Affecting Affinity Chromatographic Separation
      6. Type of Matrices
      7. Applications
      8. Review Questions
    10. 10. Nano Flow Liquid Chromatography
      1. Introduction
      2. Principle
      3. Instrumentation
      4. Sample Injection
      5. Detectors
      6. Comparison Between Well Established On-line Two-dimensional Nano LC-MS and Off-line Two-dimensional NANO LC-MS
      7. Advantages
      8. Applications
      9. Review Questions
    11. 11. Electrophoresis
      1. Introduction
      2. Principle
      3. Theory
      4. Types of Electrophoresis
      5. Instrumentation
      6. Elution Method
      7. Factors Affecting the Electrophoresis
      8. Advantages
      9. Disadvantages
      10. Applications
      11. Review Questions
    12. 12. Size Exclusion Chromatography
      1. Introduction
      2. Principle
      3. Theory
      4. Instrumentation
      5. Elution Procedure
      6. Column Parameters
      7. Factors Affecting SEC Separations
      8. Advantages of SEC
      9. Disadvantages of SEC
      10. Applications
      11. Gel Permeation Chromatography
      12. Factors Affecting GPC Separation
      13. Advantages of GPC
      14. Disadvantages
      15. Applications
      16. Review Questions
  14. Unit VII – Reagents
    1. Introduction
    2. 1. 3-Methyl-2-Benzothiazolinone Hydrazone (MBTH)
      1. Introduction
      2. Structure
      3. Mechanism of Action
      4. Oxidising Agent Used for Colour Production with MBTH
      5. Factors Affecting Nature and Intensity of Colour
      6. Advantages of MBTH
      7. Review Questions
    3. 2. Tri Keto Hydrindine Hydrate (Ninhydrin Reagent)
      1. Introduction
      2. Structure
      3. Mechanism of Action
      4. Preparation
      5. Applications
      6. Review Questions
    4. 3. Para Dimethyl Amino Benzaldehyde (PDAB) and Para Dimethyl Amino Cinnamaldehyde (PDAC)
      1. Introduction
      2. Structures
      3. Mechanism of Action
      4. Applications
      5. Review Questions
    5. 4. 2,4,6-Tripyridyl-S-Triazine (TPTZ)
      1. Introduction
      2. Structure
      3. Procedure for Determinations
      4. Mechanism of Action
      5. Review Questions
    6. 5. 1,2-Naphtha Quinone-4-Sulphonate Sodium (NQS)
      1. Introduction
      2. Structure
      3. Mechanism of Action
      4. Procedure
      5. Preparation of NQS
      6. Applications
      7. Mechanism of Action
      8. Procedure
      9. Review Questions
    7. 6. Bratton-Marshall Reagent (BM Reagent)
      1. Introduction
      2. Structure
      3. Mechanism of Action
      4. Preparation of BM Reagent
      5. Review Questions
    8. 7. Folin–Ciocalteu Reagent (FC Reagent)
      1. Introduction
      2. Structure
      3. Mechanism of Action
      4. Preparation
      5. Storage
      6. Applications
      7. Review Questions
    9. 8. 2,6-Dichloro Quinone Chloroimide (Gibb's Reagent)
      1. Introduction
      2. Structure
      3. Mechanism of Action
      4. Applications
      5. Review Questions
  15. Unit VIII – Analysis of Functional Groups
    1. 1. Analysis of Hydroxyl Groups
      1. Review Questions
    2. 2. Analysis of Carbonyl Groups
      1. Introduction
      2. Review Questions
    3. 3. Analysis of Carboxylic Acids
      1. Introduction
      2. Review Questions
    4. 4. Analysis of Esters
      1. Introduction
      2. Review Questions
    5. 5. Analysis of Amides
      1. Introduction
      2. Review Questions
    6. 6. Analysis of Amino, Imino and Quaternary Ammonium Compounds
      1. Introduction
      2. Review Questions
    7. 7. Analysis of Nitriles
      1. Introduction
      2. Review Questions
  16. Unit IX – Analysis of Pharmaceutical Agents
    1. 1. Analysis of Anti-Tubercular Drugs
      1. Introduction
      2. Classification
      3. Review Questions
    2. 2. Analysis of Antimalarials
      1. Definition
      2. Review Questions
    3. 3. Analysis of Anti-Pyretics and Analgesics
      1. Introduction
      2. Analysis Methods
      3. Review Questions
    4. 4. Analysis of Barbiturates
      1. Introduction
      2. Review Questions
    5. 5. Analysis of Local Anaesthetic Drugs
      1. Review Questions
    6. 6. Analysis of Diuretics
      1. Introduction
      2. Analytical Methods for Diuretics
      3. Review Questions
    7. 7. Analysis of Adrenergic Drugs
      1. Introduction
      2. Review Questions
    8. 8. Analysis of Sulphonamides
      1. Review Questions
    9. 9. Analysis of Vitamins
      1. Introduction
      2. Classification
      3. Analysis of Vitamin
      4. Analysis Vitamin B1 (Thiamine)
      5. Analysis of Vitamin B2 (Riboflavin)
      6. Analysis of Vitamin B6 (Pyridoxine Hydrochloride)
      7. Analysis of Vitamin B12 (Cyanocobalamin)
      8. Analysis of Pantothenic Acid
      9. Analysis of Nicotinic Acid and Nicotinamide
      10. Analysis of Vitamin C (Ascorbic Acid)
      11. Analysis of Vitamin D (Calciferol)
      12. Analysis of Vitamin K
      13. Analysis of p-Amino Benzoic Acid (Vitamin B4)
      14. Analysis of Folic Acid
      15. Analysis of Vitamin E
      16. Review Questions
    10. 10. Analysis of Antibiotics
      1. Introduction
      2. Review Questions
    11. 11. Analysis of Alkaloidal Drugs
      1. Chemical Tests
      2. Review Questions
    12. 12. Analysis of Steroids
      1. Introduction
      2. Review Questions
  17. Unit X – Specific Methods
    1. 1. Radiometric Analysis
      1. Introduction
      2. Advantages
      3. Limitations
      4. Applications
      5. Advantage
      6. Limitation
      7. Advantages
      8. Disadvantages
      9. Applications
      10. Review Questions
    2. 2. Analysis of Biological Compounds
      1. Introduction
      2. General Procedure for the Elisa
      3. Advantages
      4. Applications
      5. Bioassays
      6. Review Questions
    3. 3. Thermal Analysis
      1. Introduction
      2. Thermogravimetry
      3. Differential Thermal Analysis
      4. Differential Scanning Calorimetry
      5. Review Questions
    4. 4. Analysis of Water
      1. Introduction
      2. Moisture Content Determination
      3. Procedure
      4. Review Questions
  18. Unit XI – Miscellaneous Methods
    1. 1. Analysis of Food Components
      1. Crude Protein Analysis (Nitrogen Determination)
      2. Carbohydrates
      3. Analysis of Lipids (Oils and Fats)
      4. Review Questions
    2. 2. Analysis of Packing Materials
      1. Introduction
      2. Review Questions
  19. Unit XII – Quality Assurance and Quality Control
    1. 1. Quality Assurance and Regulatory Affairs
      1. Quality Assurance (QA)
      2. New Drug Application
      3. Abbreviated New Drug Application
      4. Definition of IND
      5. Documentation
    2. 2. Concept of Validation
      1. Introduction
      2. Types of Validation
      3. Validation of Air Handling Systems
      4. Validation of Water Handling System
  20. Appendix
  21. Multiple-choice Questions
  22. Acknowledgements
  23. Copyright