Pharmaceutical Analysis


1. Quality Assurance:
a. Introduction, Sources of quality variation, contorl of quality variation.
Concept of statistical quality control
c. Validation methods- quality of equipment, validation of equipment and vadilation of analytical instruments and calibration.
d. GLP, ISO 9000.
e. Total quality management, quality review and documentation
f. ICH-international conference for harmonization- guidelines.
g. Regulatory control

2. Chromatography:
Introduction, history, classification, separation techniques, choice of methods.
The following techniques be discussed with relevant examples of pharmaceutical products involving principles and techniques of separation of drugs from excipients.
a. Column Chromatography: Absorption column chromatorgraphy, Operational technique, frontal analysis and elution analysis. Factors affecting column efficiency, applications and partition chromatography.

b. TLC: Introduction, principle, techniques, Rfvalue and applicaitons.

c. PC: Introduction, principle, types of paper chromatography, preparation techniques, development techniques, applications.

d. Ion-exchange chromatography: Introduction, principles, types of ion exchange synthetic resins, physical properties, factors affecting ion exchange, methodology and applicaitons.

e. HPLC: Introduction, theory, instrumentation and applications.

f. HPTLC: Introduction, theory, instrumentation and applications.

g. Gas chromatography: Introduction, theory, instrumentation-carriergases, types of columns, stationary phases in GLC and GSC. Detectors-Flame ionization detectors, electron capture detector, thermal conductivity detector. Typical gas chromatogram, derivatisation techniques, programmed temperature gas chromatography, applications.

h. Electrophoresis: Principles of separation, equipment for paper and gel electrophoresis, and application

i. Gel filtration and affinity chromatography: Intruduction, technique, applications.

3. Electrometric Methods:
Theoretical aspects, instrumentation, interpretation of data/ spectra and analytical applicaitons be discussed on the following topics.
a. Potentiometry: Electrical potential, electrochemical cell, reference electrodes, indicator electrodes, measurement of potential and pH, construction and working of electrodes, Potentiometric tirations, methods of detecting end point, Karl Fischer titration.

b. Conductometry: Introduction, conductivity cell, conductometric titrations and applications.

c. Polarography: Instrumentation, DME, residual current, diffusion current and limiting current, polarographic wave, Illkovic's equation, Effect of oxygen on polarographic wave, Polarographic maxima and suppressors and applications.

d. Amperometric Titraitons: Introduction, types of electrodes used, reference and indicator electrode, instumentaiton, titration procedure, advantages and disadvantages of Amperometry over potentiometry. Pharma applicaitons.

4. Spectroscopy:
Theoretical aspects, instumentaiton, elements of interpretation of data/spectra and application of analytical techniques be discussed on:
a. Absorption Spectroscopy:
-Theory of electronic, atomic and molecular spectra. Fundamental laws of photometry, Beer-Lambert's law, applicaiton 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 and infrared spectra.

-Instrumentation- Photometer, U.V.Visible spectrophotometer- sources of U.V.-Visible radiations, collimating systems, monochromators, samples cels and following detectors- Photocell, Barrier layer cell, Phototube, Diode array, applications of U.V.-Visible spectroscopy in pharmacy and spectrophotometric titrations.

-Infrared Spectroscopy: Vibrational transitions, frequency-structure correlaitons, Infrared absorption bands, Instrumentation-IR spectro-meter- sources of IR, Collimating systems, monochromators, sample cells, sample handling in IR spectroscopy and detectors- Thermocouple, Golay Cells, Thermistor, Bolometer, Pyroelectric detector, Applications of IR in pharmacy.

-Fluorimetric Analysis: Theory, luminescence, factors affecting fluorescence, quenching. Instrumentaiton, Applications, fluorescentindicators, study of pharmaceutically important compounds estimated by fluorimetry.

b.Flame Photometry: Theory, nebulisation, flame and flame temperature, interferences, flame spectrometric techniques and instrumentaiton and pharmaceutical applicaitons.

c. Atomic Absorption Spectrometry: Introduction, Theory, types of electrodes, instrumentation and applications.

d. Atomic Emission Spectroscopy: Spectroscopic sources, atomic emission spectrometers, photographic and photoelectric detection.

5. a. NMR and ESR (introduction only): Introduction, theroretical aspects and applicaitons.

b. Mass Spectroscopy: (Introduction only)- Fragmentation, types of ions produced mass spectrum and applicaitons.

c. Polarimetry: (Introduction only)- Introduction to optical rotatory dispersion, circular dichronism, polarimeter.

d. X-RAY Diffusion: (Introduciton only)- Theory, reciprocal lattice concept, diffration patterns and applicaitons.

e. Thermal Analysis: Introduciton, instrumentation, applications, and DSC and DTA.