Course

‘Pharmaceutical Analysis – Theory’ is a course offered in the third year of Pharm. D. program at School of Pharmacy, Health Sciences campus, Amrita Vishwa Vidyapeetham.

Course Duration: 3 Hrs./Week

1. Quality Assurance:
   1. Introduction, sources of quality variation, control of quality variation.
   2. Concept of statistical quality control.
   3. Validation methods- quality of equipment, validation of equipment and validation of analytical instruments and calibration.
   4. GLP, ISO 9000.
   5. Total quality management, quality review and documentation.
   6. ICH- international conference for harmonization-guidelines.
   7. Regulatory control.
2. Chromatography:Introduction, history, classification, separation techniques, choice of methods. The following tech- niques be discussed with relevant examples of pharmaceutical products involving principles and tech- niques of separation of drugs from excipients.
   1. Column Chromatography: Adsorption column chromatography, Operational technique, frontal analysis and elution analysis. Factors affecting column efficiency, applications and partition chro- matography.
   2. TLC: Introduction, principle, techniques, Rf value and applications.
   3. PC: Introduction, principle, types of paper chromatography, preparation techniques, development techniques, applications.
   4. Ion-exchange chromatography: Introduction, principles, types of ion exchange synthetic resins, physical properties, factors affecting ion exchange, methodology and applications.
   5. HPLC: Introduction, theory, instrumentation, and applications.
   6. HPTLC: Introduction, theory, instrumentation, and applications.
   7. Gas Chromatography: Introduction, theory, instrumentation-carrier gases, types of columns, stationary phases in GLC & GSC. Detectors-Flame ionization detectors, electron capture detec- tor, thermal conductivity detector. Typical gas chromatogram, derivatisation techniques, pro- grammed temperature gas chromatography, applications.
   8. Electrophoresis: Principles of separation, equipment for paper and gel electrophoresis, and application.
   9. Gel filtration and affinity chromatography: Introduction, technique, applications.
3. Electrometric Methods:Theoretical aspects, instrumentation, interpretation of data/spectra and analytical applications be dis- cussed on the following topics.
   1. Potentiometry: Electrical potential, electrochemical cell, reference electrodes, indicator elec- trodes, measurement of potential and pH, construction and working of electrodes, Potentiomet- ric titrations, methods of detecting end point, Karl Fischer titration.
   2. Conductometry: Introduction, conductivity cell, conductometric titrations and applications.
   3. Polarography: Instrumentation, DME, residual current, diffusion current and limiting current, polarographic wave, Ilkovic’s equation, Effect of oxygen on polarographic wave, Polarographic maxima and suppressors and applications.
   4. Amperometric Titrations: Introduction, types of electrodes used, reference and indicator elec- trode, instrumentation, titration procedure, advantages and disadvantages of Amperometry over potentiometry. Pharma applications.
4. Spectroscopy:Theoretical aspects, instrumentation, elements of interpretation of data/spectra and application of analytical techniques be discussed on:
   1. Absorption Spectroscopy:
      1. Theory of electronic, atomic and molecular spectra. Fundamental laws of photometry, Beer-Lam- bert’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 spec- troscopy. 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 radia- tions, collimating systems, monochromators, samples cells and following detectors-Photocell, Barrier layer cell, Phototube, Diode array, applications of U.V.-Visible spectroscopy in pharmacy and spectrophotometric titrations.
      2. Infrared Spectroscopy: Vibrational transitions, frequency – structure correlations, Infrared ab- sorption bands, Instrumentation–IR spectro-meter – sources of IR, Collimating systems, mono- chromators, sample cells, sample handling in IR spectroscopy and detectors–Thermocouple, Go- lay Cells, Thermistor, Bolometer, Pyroelectric detector, Applications of IR in pharmacy.
      3. Fluorimetric Analysis: Theory, luminescence, factors affecting fluorescence, quenching. Instru- mentation, Applications, fluorescent indicators, study of pharmaceutically important compounds estimated by fluorimetry.
   2. Flame Photometry: Theory, nebulisation, flame and flame temperature, interferences, flame spectrometric techniques and instrumentation and pharmaceutical applications.
   3. Atomic Absorption Spectrometry: Introduction, Theory, types of electrodes, instrumentation and applications.
   4. Atomic Emission Spectroscopy: Spectroscopic sources, atomic emission spectrometers, photographic and photoelectric detection.
   5. NMR & ESR (introduction only): Introduction, theoretical aspects and applications.
   6. Mass Spectroscopy: (Introduction only) – Fragmentation, types of ions produced mass spectrum and applications.
   7. Polarimetry: (Introduction only) – Introduction to optical rotatory dispersion, circular dichroism, polarimeter.
   8. X-RAY Diffraction: (Introduction only) – Theory, reciprocal lattice concept, diffraction patterns and applications.
   9. Thermal Analysis: Introduction, instrumentation, applications, and DSC and DTA.