Syllabus
Unit 1
Mass Spectroscopy: Principle, Theory, Instrumentation of Mass Spectroscopy, Different types of ionisation like electron impact, chemical, field, FAB and MALDI, APCI, ESI etc. Mass Analyzers of Quadrupole and Time of Flight, Mass fragmentation and its rules, Meta stable ions, Isotopic peaks and Applications of Mass Spectroscopy. Tandem MS, Hyphenation, MS Spectra.
Unit 2
NMR spectroscopy: Quantum numbers and their role in NMR, Principle, Instrumentation, Solvent requirement in NMR, Relaxation process, NMR signals in various compounds, Chemical shift, Factors influencing chemical shift, Spin-Spin coupling, Coupling constant, Nuclear magnetic double resonance, Brief outline of principles of FT-NMR and 13C NMR. Applications of NMR spectroscopy.
Unit 3
Preliminary reading: Basic Theory and Instrumentation of IR Spectroscopy
IR spectroscopy: Sample handling, Near IR, ATR. Instrumentation of Dispersive and Fourier- Transform IR Spectrometer, Factors affecting vibrational frequencies and Applications of IR spectroscopy. IR Spectra Interpretation.
Unit 4
Preliminary reading: Basic Theory and Instrumentation of UV-Visible Spectroscopy
UV-Visible spectroscopy: Choice of solvents and solvent effect. Multiple channel or Variable Channel Detectors, Derivative Spectroscopy, Difference Spectroscopy, Derivatisation technique. Application in Quantitative (Single component analysis) and Qualitative Analysis.
Unit 5
Preliminary reading: Basic Theory and Instrumentation of Spectro Fluorimetry Spectrofluorimetry: Factors affecting fluorescence, Quenching, Applications of Fluorescence Spectrophotometer. Fluorescence imaging and microscopic techniques.
Unit 6
Preliminary reading: Basic Theory and Instrumentation of Flame emission spectroscopy & Atomic absorption spectroscopy
Flame emission spectroscopy and Atomic absorption spectroscopy: Interferences and Applications.
Unit 7
Preliminary reading: Basic Theory and Instrumentation of the Theory and Principles of Chromatography, Planar & Columnar Chromatography
Chromatography: Instrumentation, chromatographic condition, factors affecting resolution, Hyphenation, data interpretation and applications of the following:
- High Performance Thin Layer Chromatography : Automated Instruments, Fingerprint Profiling ( 3 hrs)
- High Performance Liquid chromatography: Trouble Shooting, Quantitative (Single and Multicomponent analysis, Biological sample analysis) and Qualitative applications LCMS and its applications (6 hrs)
- Gas chromatography : Sample Handling, Temperature Programming Hyphenations- GCMS (3 hrs)
- Ion exchange chromatography (2 hrs)
- Gel Chromatography (2hrs)
Unit 8
Preliminary reading: Basic Theory and Instrumentation of Electrophoresis
Electrophoresis: factors affecting separation and applications of the following:
- Gel electrophoresis – SDS PAGE, Isoelectric focusing
- Capillary electrophoresis
Unit 9
Preliminary reading: Basic Theory and Instrumentation of X-ray Crystallography
X ray Crystallography: Different X ray diffraction methods, Bragg‘s law, Rotating crystal technique, X ray powder technique, Types of crystals and applications of Xray diffraction.
Unit 10
Preliminary reading: Basic Theory and Instrumentation of Thermogravimetry
Thermal Techniques:
Differential Scanning Calorimetry (DSC): Thermal transitions and Instrumentation (Heat flux and power-compensation and designs), Modulated DSC, Hyper DSC, experimental parameters (sample preparation, experimental conditions, calibration, heating and cooling rates, resolution, source of errors) and their influence, advantage and disadvantages, pharmaceutical applications. (2hrs)
Differential Thermal Analysis (DTA): Principle, instrumentation and advantages and disadvantages, pharmaceutical applications, derivative differential thermal analysis (DDTA). (1hr)
Thermo Gravimetric Analysis (TGA): Principle, instrumentation, factors affecting results, advantages and disadvantages, pharmaceutical applications. 1hr)
Assignments:
- Interpret different Organic compounds by IR, NMR & MS
- Case studies on HPLC troubleshooting
- Develop a procedure for the analysis of various drugs by HPLC & UV
- Determination of geometrical isomerism by spectroscopic
- Write down the MS Fragmentation pattern of selected drugs
Scope
The course provides students with comprehensive knowledge of analytical methods and instrumentation used in the pharmaceutical industry. Students will gain an understanding of how these analytical techniques are applied to address complex challenges in drug development, quality control, and pharmaceutical research. They will possess a strong foundation in modern pharmaceutical analytical techniques, enabling them to contribute effectively to the advancement of pharmaceutical science and drug discovery processes. Students will learn about drug quality assessment, adherence to regulatory standards, and the development of safe and effective pharmaceutical products.
This course fosters an attitude of curiosity and openness to explore cutting-edge analytical methods and emerging technologies in the pharmaceutical industry. Graduates will develop a proactive and problem-solving attitude to address challenges in drug quality assessment and ensure the development of safe and effective pharmaceutical products. They will also be instilled with a sense of responsibility and commitment to contributing to the advancement of pharmaceutical science for the benefit of society and patient health.
In conclusion, the scope of the course on Modern Pharmaceutical Analytical Techniques encompasses a wide array of knowledge, skills, and attitudes that prepare students to excel in the dynamic and critical field of pharmaceutical analysis. Graduates will be equipped to meet the demands of the pharmaceutical industry, contribute to scientific advancements, and uphold ethical standards, ensuring the well-being of society and the enhancement of patient health.
Objectives and Outcomes
COURSE LEARNING OUTCOMES:
After successful completion of the course, the student shall be able to;
KNOWLEDGE
K1: Demonstrate a comprehensive understanding of various modern analytical methods and instrumentation commonly employed in the pharmaceutical industry.
K2: Explain the significance of specific analytical techniques in addressing complex challenges related to drug development, quality control, and pharmaceutical research.
K3: Familiar with the regulatory guidelines and ethical practices governing pharmaceutical analysis
K4: Gain insights into the principles and applications of stability testing and dissolution studies K5: Acquire knowledge of emerging analytical technologies and advancements in the pharmaceutical industry.
K6: Analyse scientific literature and research papers related to modern pharmaceutical analytical techniques, informing them about recent advancements.
SKILL
S1: Optimise analytical methods for the qualitative and quantitative analysis of pharmaceutical compounds.
S2: Apply knowledge of regulatory requirements and guidelines in the execution of analytical techniques in the pharmaceutical industry
S3: Interpret data obtained from various analytical techniques to ensure accurate and reliable results.
S4: Analyse troubleshooting strategies for resolving common issues encountered in analytical testing,
S5: Develop a fundamental skill in selecting suitable analytical techniques for analysing drugs in dosage forms and biological fluids.
S6: Evaluate the validity and reliability of analytical methods
ATTITUDE
A1: Demonstrate a receptive attitude.
A2: Value the importance of adhering to regulatory guidelines and ethical practices.
A3: Develop a proactive and problem-solving attitude.
A4: Exhibit a strong commitment to upholding the highest standards of quality and accuracy.
A5: Demonstrate a willingness to collaborate with peers and professionals.
A6: Display a sense of responsibility and commitment
Text Books / References
Reference Books:
Robert M Silverstein, Spectrometric Identification of Organic Compounds, Sixth edition, John Wiley & Sons, 2004Becket A.H. & Stenlake J.B. Practical Pharmaceutical Chemistry I and II, 4th edn, The Athlon Press of the University of London. 1998.Doglas A Skoog, James Holler, Timothy A. Nieman, Principles of Instrumental Analysis, 5th edition, Eastern press, Bangalore, 1998.Hobart H. Willard, Lynne L. Merritt, Jr., and John A. Dean, Instrumental methods of analysis, 7th edition, CBS publishers, 1986.William Kemp, Organic Spectroscopy, 3rd edition, PAlGRAVE,P D Sethi, Sethi’s HPTLC High Performance Thin Layer Chromatography- Quantitative Analysis of Pharmaceutical Formulations, Volume 3, CBS Publishers, 2013.D Sethi, Sethi’s HPLC High Performance Liquid Chromatography: Quantitative Analysis of Pharmaceutical Formulations, Volume 8. India: CBS Publishers & Distributors. 2015James Munson, Quantitative Analysis of Pharmaceutical Formulations Pharmaceutical Analysis- Modern methods, Volume 11, Marcel Dekker Series, 2001Journals:Journal of Pharmaceutical Analysis (Elsevier) https://www.com/journal/journal-of-pharmaceutical-analysisCurrent Pharmaceutical Analysis (Bentham Science) https://benthamscience.com/public/journals/current-pharmaceutical-analysisJournal of Chromatography A Elsevier https://www.com/journal/journal-of-chromatography-aJournal of Chromatography B Elsevier https://www.com/journal/journal-of-chromatography-b