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Course Detail

Course Name Pharmaceutical Analysis Practical
Campus

Syllabus

UNIT-I  Chromatography                                                                                      30 Hours

Principles and tecniques of Chromatography, Planar and Columnar chromatography, theories of chromatography. Choice of chromatographic condition. Concept and need for derivatization in pharmaceutical analysis (5 hrs)

Introduction to chromatographic techniques

  • Paper Chromatography (1 hr)
  • Thin Layer Chromatography (1 hr)
  • High Performance Thin Layer Chromatography (2 hr)
  • Column Chromatography: (1 hr)
  • Gas Chromatography (2 hrs)
  • Ion-exchange chromatography (1 hr)
  • Gel filtration and affinity chromatography (1 hr)
  • Chiral Chromatography(1 hr)
  • High Performance Liquid Chromatography (10 hrs)

Introduction, theory, instrumentation, selection of mobile phase, stationary phase, detectors, analytical and bioanalytical applications. Sample preparation of non-biological and biological samples. HPLC- method development, Data interpretation, HPLC in Bioavailability and Equivalence Studies. Hyphenation techniques, Ultra and nano-HPLC. AI technologies used in hyphenated instruments for data interpretation, method optimization, and decision support.

  • Electrophoresis (5 hrs)

Principles of separation, gel electrophoresis, SDS PAGE, Clinical and Pharmaceutical Applications. Quality control of protein-based drugs. Identifying and characterizing biomarker proteins. Studying protein-protein or DNA-protein interactions. Genomic and proteomic studies for novel drug targets.

UNIT-II  Spectroscopy                                                                                       21 Hours

  • Absorption Spectroscopy: (7 hrs) Introduction to Spectroscopy, Theory of electronic, atomic and molecular spectra, Fundamental laws of photometry, Beer-Lambert’s Law, Principle and Application, Deviations and Limitations, Chromophores and Auxochromes in Biomolecules, Spectral Shifts and Solvent Effects, Instrumentation, Types of Spectrophotometers: Single-beam and double-beam spectrophotometers, Radiation Sources

and Monochromators, Detectors, Advanced Techniques like Derivative Spectroscopy, Derivatisation and Difference Spectroscopy, Applications in Pharmacy: Quality Control in Pharmaceuticals Single and Multi-Component Analysis: Spectroscopy in Biochemical and Pharmacokinetic Studies Equilibrium and Kinetics,Spectroscopic methods in Diagnosis and Monitoring glucose, cholesterol, and other critical parameters in clinical labs,

  • Fluoresence Spectroscopy (7 hrs)

Introduction to Fluorescence Spectroscopy, Theory of Luminescence, Factors Affecting Fluorescence and Quenching, Instrumentation, Applications of Fluorescence Spectroscopy in Pharmacy and Clinical Settings, study of pharmaceutically important compounds estimated by fluorimetry. Fluorescence techniques employed for DNA/RNA quantification and enzyme activity assays. Fluorescence imaging and microscopic techniques: imaging tissues and monitoring drug absorption and distribution, deep tissue imaging with minimal damage using NIR. Application of NIR fluorophores in robotic surgery.

Inroduction to structural elucidation techniques and its clinical relevance

  • Infrared Spectroscopy (3 hrs)
  • NMR & ESR (2 hrs)
  • X-RAY Diffraction (2 hrs)

UNIT-III SpectrometricTechniques                                       12 Hours

  • Mass Spectrometry: (8 hrs)

Basic principles of Mass Spectrometry Instrumentation: Ionization techniques: Electron ionization, Chemical ionization, Atmospheric pressure ionization (Electrospray ionization, APCI, and APPI), other sources: MALDI, ICP, etc. Mass Analyzers: Quadrupole, Time of flight, Orbitrap, High Resolution Mass Spectrometry, Hyphenated Mass Spectrometry: GC/MS, HPLC/UPLC-MS and Tandem Mass Spectrometry, Mass spectrum and applications. Over view of LCMS as an analytical technicque. A brief outline of omics study using hyphenated tandem MS including the scope of biomarkers study. AI-driven advancements in mass spectrometry, including machine learning models for enhancing spectral clarity, optimizing analytical methods, improving peak identification accuracy, and providing intelligent decision support in data interpretation.

  • Flame Photometry (2 hrs)

Theory, nebulisation, flame and flame temperature, interferences, flame spectrometric techniques instrumentation and pharmaceutical applications.

  • Atomic Absorption Spectrometry: (2 hrs)

Introduction, Theory, types of electrodes, instrumentation and applications.

UNIT-IV Quality Assurance                                                                               12 hours

  • Concept of Quality Control and Quality assurance (2 hr)
  • Total quality management, quality review and (2 hr)
  • GLP, NABL, ISO (2 hrs)
  • ICH- international conference for harmonisation (4hrs)
  • Qualification of equipment, validation of analytical instruments and (2 hrs)

Text Books / References

TEXT BOOKS:

  1. Willard, H.H., Merritt, L.L., Dean, J.A., & Settle, F.A. Instrumental methods of analysis, 7th edition. EWP, East West Press Ltd., Delhi/Madras;1988.
  2. Skoog, A., Heller, F.J., Nieman, T.A., Principles of Instrumental Analysis, WBSaunders;1997
  3. Becket H. & Stenlake J.B. Practical Pharmaceutical Chemistry Vol. I and II, 4th edition, the Athlone Press of the University of London;1988.
  4. Kenneth A. Connors. A Textbook Of Pharmaceutical Analysis, 3rd Edition. Wiley India Pvt. Limited; 2007.
  5. Silverstein, M., Webster, F. X., Kiemle, D. J. Spectrometric Identification of Organic Compounds. 6th edition. Wiley India Pvt. Limited; 2006
  6. Sethi, D. Quantitative Analysis of Drugs in Pharmaceutical Formulations. India: CBS Publishers & Distributors; 2015
  7. Kemp, Organic Spectroscopy. United States: Palgrave Macmillan; 1991
  8. Vogels Textbook Of Quantitative Chemical India: Pearson Education; 2006.

REFERENCE BOOKS:

  1. Indian Pharmacopoeia, Indian Pharmacopoeia Commission.The Controller of Publications, New Delhi; 2018.
  2. BPC- of Health, U.K. for HMSO.
  3. USP – Mack Publishing , Easton, PA.
  4. The Extra Pharmacopoeia – The Press, London.
  5. Sethi, D. Sethi’s HPLC High Performance Liquid Chromatography: Quantitative Analysis of Pharmaceutical Formulations, Volume 8. India: CBS Publishers & Distributors; 2015
  6. Clarke, G. C. Clarke’s Analysis of Drugs and Poisons: In Pharmaceuticals, Body Fluids and Postmortem Material. United Kingdom: Pharmaceutical Press; 2004
  7. Remington, P. Remington: The Science and Practice of Pharmacy. United Kingdom: Lippincott Williams & Wilkins; 2006
  8. Stahl, Thin-Layer Chromatography: A Laboratory Handbook. Germany: Springer Berlin Heidelberg. Higuchi. T and Hasen. E. B. Text Book of Pharm. Analysis. New York Inter Science Publishers; 2013

JOURNALS:

Biomedical Chromatography. https://analyticalsciencejournals.onlinelibrary.wiley.com/journal/10990801

Journal of Pharmaceutical and Biomedical Analysis. https://www.sciencedirect.com/journal/journal-of-pharmaceutical-and-biomedical- analysis

Clinical Chemistry and Laboratory Medicine (CCLM) https://www.degruyter.com/journal/key/cclm/html#overview

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