3.2 Pharmaceutical Analysis

1. Quality Assurance

a. Introduction, Sources of Quality Variation, Control of Quality Variation

b. Concept of Statistical Quality Control

c. Validation Methods-Quality of Equipment, Validation of Equipment and Validation of Analytical Instruments and Calibration

d. GLP, ISO 9000.

e. Total Quality Management

f. Quality Review and Documentation

g. International Conference for Harmonization (ICH) Guidelines

h. Regulatory control

2. Chromatography

a. Column Chromatography:

i. Adsorption Column Chromatography

ii. Operational Technique

iii. Frontal Analysis

iv. Elution analysis

v. Factors Affecting Column Efficiency

vi. Applications

vii. Partition Chromatography

b. TLC:

i. Introduction

ii. Principle

iii. Techniques

iv. Rf Value and Applications

c. PC:

i. Introduction

ii. Principle

iii. Types of Paper Chromatography

iv. Preparation Techniques

v. Development Techniques

vi. Applications

d. Ion-Exchange Chromatography:

i. Introduction

ii. Principles

iii. Types of Ion Exchange Synthetic Resins

iv. Physical Properties

v. Factors Affecting Ion Exchange

vi. Methodology

vii. Applications

e. HPLC:

i. Introduction

ii. Theory

iii. Instrumentation

iv. Applications

f. HPTLC:

i. Introduction

ii. Theory

iii. Instrumentation

iv. Applications

g. Gas Chromatography:

i. Introduction

ii. Theory

ii. Instrumentation

  • Carrier Gases
  • Types of Columns
  • Stationary Phases in GLC & GSC

iv. Detectors

  • Flame Ionization Detectors
  • Electron Capture Detector
  • Thermal Conductivity Detector

v. Typical Gas Chromatogram

vi. Derivatisation Techniques

vii. Programmed Temperature Gas Chromatography

viii. Applications

h. Electrophoresis:

i. Principles of Separation

ii. Equipment for Paper and Gel Electrophoresis

iii. Application

i. Gel Filtration and Affinity Chromatography:

i. Introduction

ii. Technique

iii. Applications

3. Electrometric Methods:

a. Potentiometry:

i. Electrical Potential

ii. Electrochemical Cell

iii. Reference Electrodes

iv. Indicator Electrodes

v. Measurement of Potential and pH

vi. Construction and Working of Electrodes

vii. Potentiometric Titrations

viii. Methods of Detecting End Point

ix. Karl Fischer Titration

b. Conductometry:

i. Introduction

ii. Conductivity Cell

iii. Conductometric Titration

iv. Applications

c. Polarography:

i. Instrumentation

ii. DME

iii. Residual Current

iv. Diffusion Current and Limiting Current

v. Polarographic Wave

vi. Ilkovic’s equation

vii. Effect of Oxygen on Polarographic Wave

viii. Polarographic Maxima and Suppressors

ix. Applications

d. Amperometric Titrations:

i. Introduction

ii. Types of Electrodes used

iii. Reference and Indicator Electrode

iv. Instrumentation

v. Titration Procedure

vi. Advantages and Disadvantages of Amperometry over Potentiometry

vii. Pharma applications

4. Spectroscopy:

a. Absorption Spectroscopy:

i. Theory:

  • Theory of Electronic, Atomic and Molecular Spectra
  • Fundamental Laws of Photometry
  • Beer-Lambert’s Law
  • Application and its Deviation
  • Limitation of Beer Law
  • Application of the Law to Single and Multiple Component Analysis
  • Measurement of Equilibrium Constant and Rate Constant by Spectroscopy
  • Spectra of:
    • Isolated Chromophores
    • Auxochromes
    • Batho-Chromic Shift
    • Hypsochromic Shift
    • Hyperchromic and Hypochromic Effect
    • Effect of Solvent on Absorption Spectra
    • Molecular Structure
    • Infrared Spectra

ii. Instrumentation

  • Photometer
  • U.V Visible Spectrophotometer
  • Sources of U.V Visible Radiations
  • Collimating Systems
  • Monochromators
  • Samples Cells
  • Detectors:
    • Photocell
    • Barrier Layer Cell
    • Phototube
    • Diode Array
  • Applications of U.V Visible Spectroscopy in Pharmacy
  • Spectrophotometric Titrations

b. Infrared Spectroscopy:

i. Theory

  • Vibrational Transitions
  • Frequency – Structure Correlations
  • Infrared Absorption Bands

ii. Instrumentation

  • IR Spectrometer
    • Sources of IR
    • Collimating Systems
    • Monochromators
    • Sample Cells
    • Sample Handling in IR Spectroscopy
  • Detectors
    • Thermocouple
    • Golay Cells
    • Thermistor
    • Bolometer
    • Pyroelectric Detector
    • Applications of IR in Pharmacy

c. Fluorimetric Analysis:

i. Theory

  • Luminescence
  • Factors Affecting Fluorescence
  • Quenching

ii. Instrumentation

  • Applications
  • Fluorescent Indicators
  • Study of Pharmaceutically important compounds estimated by Fluorimetry

d. Flame Photometry:

i. Theory

ii. Nebulisation

iii. Flame and Flame Temperature

iv. Interferences

v. Flame Spectrometric Techniques

vi. Instrumentation

vii. Pharmaceutical Applications

e. Atomic Absorption Spectrometry:

i. Introduction

ii. Theory

iii. Types of Electrodes

iv. Instrumentation

v. Applications

f. Atomic Emission Spectroscopy:

i. Spectroscopic Sources

ii. Atomic Emission Spectrometers

iii. Photographic and Photoelectric Detection

g. NMR & ESR:

i. Introduction

ii. Theoretical Aspects

iii. Applications

h. Mass Spectroscopy:

i. Fragmentation

ii. Types of Ions Produced

iii. Mass Spectrum

iv. Applications

i. Polarimetry:

i. Introduction to Optical Rotatory Dispersion

ii. Circular Dichroism

iii. Polarimeter

j. X-RAY Diffraction:

i. Theory

ii. Reciprocal Lattice Concept

iii. Diffraction Patterns

iv. Applications

k. Thermal Analysis:

i. Introduction

ii. Instrumentation

iii. Applications

iv. DSC

v. DTA