Modern Pharmaceutical Analytical Techniques (CUTM2000)

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Dr. BIKASH RANJAN JENA, M.Pharm., Ph.D

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Modern Pharmaceutical Analytical Techniques

Course Code: [CUTM2000]

Course Type: Core course

Scope

This subject deals with various advanced analytical instrumental techniques for
identification, characterization and quantification of drugs. Instruments dealt are
NMR, Mass spectrometer, IR, HPLC, GC etc.

Course Objective

After completion of course student is able to know,
 Chemicals and Excipients
 The analysis of various drugs in single and combination dosage forms
 Theoretical and practical skills of the instruments

Course Outcome:

CO Statement Mapping with POs
CO-1 Understand the interaction of matter with electromagnetic radiations and its applications in drug analysis  PO1, PO2, PO8
CO-2 Understand the chromatographic separation and analysis of drugs. PO1, PO6, PO9
CO-3 Perform quantitative & qualitative analysis of drugs using various analytical instruments. PO1, PO2, PO8
CO-4 Able to separate and analyses drugs by chromatography Radioimmunoassay and Electrophoresis PO1, PO3, PO6, PO8
CO-5 student interpretation skills will be improve by the course content in terms of choice of analytical techniques to perform the estimation of different category drugs. PO1, PO2, PO6

SYLLABUS [THEORY]

1. a. UV-Visible spectroscopy: Introduction, Theory, Laws,
Instrumentation associated with UV-Visible spectroscopy, Choice of solvents and solvent effect and Applications of UV-Visible
spectroscopy.

b. IR spectroscopy: Theory, Modes of Molecular vibrations,
Sample handling, Instrumentation of Dispersive and Fourier -Transform IR Spectrometer, Factors affecting vibrational frequencies and Applications of IR spectroscopy
c. Spectroflourimetry: Theory of Fluorescence, Factors
affecting fluorescence, Quenchers, Instrumentation and Applications of fluorescence spectrophotometer.
d. Flame emission spectroscopy and Atomic absorption
spectroscopy: Principle, Instrumentation, Interferences and
Applications.
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.

4.Mass Spectroscopy: Principle, Theory, Instrumentation of Mass
Spectroscopy, Different types of ionization like electron impact, chemical, field, FAB and MALDI, APCI, ESI, APPI Analyzers of Quadrupole and Time of Flight, Mass fragmentation and its rules, Meta stable ions, Isotopic peaks and Applications of Mass spectroscopy

4. Chromatography: Principle, apparatus, instrumentation,
chromatographic parameters, factors affecting resolution and applications of the following:
a) Paper chromatography b) Thin Layer chromatography
c) Ion exchange chromatography d) Column chromatography
e) Gas chromatography f) High Performance Liquid
chromatography
g) Affinity chromatography

5. a. Electrophoresis: Principle, Instrumentation, Working
conditions, factors affecting separation and applications of the following:
a) Paper electrophoresis b) Gel electrophoresis c) Capillary electrophoresis d) Zone electrophoresis e) Moving boundary electrophoresis f) Iso-electric focusing
b. X ray Crystallography: Production of X rays, Different X ray diffraction methods, Bragg‘s law, Rotating crystal technique, X
ray powder technique, Types of crystals and applications of Xray diffraction.
6.Immunological assays: RIA (Radio immuno assay), ELISA, Bioluminescence assays.

REFERENCES:

1. Spectrometric Identification of Organic compounds - Robert M Silverstein,
Sixth edition, John Wiley & Sons, 2004.
2. Principles of Instrumental Analysis - Doglas A Skoog, F. James Holler,
Timothy A. Nieman, 5th edition, Eastern press, Bangalore, 1998.
3. Instrumental methods of analysis – Willards, 7th edition, CBS publishers.
4. Practical Pharmaceutical Chemistry – Beckett and Stenlake, Vol II, 4th
edition, CBS Publishers, New Delhi, 1997.
5. Organic Spectroscopy - William Kemp, 3rd edition, ELBS, 1991.
6. Quantitative Analysis of Drugs in Pharmaceutical formulation - P D Sethi, 3rd
Edition, CBS Publishers, New Delhi, 1997.
7. Pharmaceutical Analysis- Modern methods – Part B - J W Munson, Volume
11, Marcel Dekker Series

Session 1: Introduction to UV visibile spectroscoopy

uv (Theory, laws and instrumentations of UV)

Session 2:  UV visibile spectroscoopy, instrumentation and Applications

UV instrumentation

Session 3: Theory, Modes of Molecular vibrations,
Sample handling,

Infrared spectroscopy _ FTIR

Session 4: Instrumentation and Applications of IR spectroscopy

Infrared spectroscopy _ (Instrumentation, Different types of Sample handlings)

Session 5: Molecular vibrations and  Applications of IR spectroscopy

IR spectroscopy (Multivariate Applications)

Session 6: Flame emission spectroscopy: Principle, Instrumentation, Interferences

Flame phtometry (Principle, Theories)

Session 7: Spectroflourimetry: Theory of Fluorescence, Factors
affecting fluorescence, Quenchers,

Spectro-flourimetry (Principle, Theory, Instrumentations, Applications)

Session 8:  Instrumentation, Interferences and
Applications.

flamephotometery (Interferences, Applications)

Session 9:  

NMR spectroscopy: Quantum numbers and their role in NMR,
Principle, Instrumentation, Solvent requirement in NMR,
Relaxation process.

c 13 NMR and its applications

FT-NMR and its configurations

Session 10:  

NMR spectroscopy: Nuclear magnetic double resonance,
Brief outline of principles of FT-NMR and 13C NMR. Applications
of NMR spectroscopy.

(H1, C13, FT NMR )

Session 11:  

Chemical shift, Factors influencing chemical shift, Spin-Spin coupling, Coupling constant in NMR spectroscopy

https://chem.libretexts.org/Courses/Providence_College/Organic_Chemistry_I/05%3A_Analytical_Methods_for_Structure_Elucidation/5.03%3A_Factors_That_Influence_NMR_Chemical_Shift

chemical shift

Session 12

Principle, instrumentation, applications of FTNMR

FTNMR principles & Applications

Session 15

Mass Spectroscopy: Principle, Theory of Mass spectroscopy.

https://yunus.hacettepe.edu.tr/~selis/teaching/WEBkmu396/ppt/KMU396Presentations2011/MS.pdf

 

 

Session 17

Different types of ionization like electron impact, chemical ionization.

Ionization-techniquesmass-spectrometry-a-review.

Session 18

FAB and  APCI, ESI, APPI Analyzers of Quadrupole and Time of Flight, Mass fragmentation and its rules, Meta stable ions, Isotopic peaks and Applications of Mass spectroscopy.

FAST ATOM BOMBARDMENT

Electrospray_Ionisation_Mass_Spectrometry_Principl

Ionization-techniquesmass-spectrometry-a-review

MALDI-TOF-MASS

Session 19

Principle and instrumentation of Paper chromatography.

Paper Chromatography-

Session 20

Principle and instrumentation of TLC.

Thin-layer-chromatography (TLC)

Session 21

Principle and instrumentation of Ion exchange chromatography .

ION EXCHANGE CHROMATOGRAPHY NEW

Session 22

Principle and instrumentation of High Performance Liquid chromatography. (HPLC).

HPLC NEW

Session 23

Principle and instrumentation of Affinity Chromatography

Affinity Chromatography new

Session 24

Principle and instrumentation of Column chromatography

column chromatography

Session 25

Principle and instrumentation of Fluorimetry

flourimetry

Session 26

Principle and instrumentation and Application's of Electrophoresis

electrophoresis

Session 27

Principle and instrumentation and Application's of Moving boundary electrophoresis and Iso electric focusing.

https://www.youtube.com/watch?v=B-z8rKpI58k

Session 29

Application's of X ray crystallography and Bragg's law of X ray diffraction

x-raydiffraction-_2

Session 30

Principle and instrumentation and Application's of Potentiometry

Potentiometry PDF

Our Main Teachers

Dr. BIKASH RANJAN JENA, M.Pharm., Ph.D

Associate Professor, M.Pharm., Ph.D.
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About Me My self Dr.Bikash Ranjan Jena currently working in Pharmaceutical Analysis & Research Division, School of Pharmacy and Life Sciences (SoPLS), Centurion University, Bhubaneswar since Jan 2021.  I have successfully awarded my Ph.D  degree at KLEF Deemed to be University, Vaddeswaram, Guntur, A.P on 22nd June 2023. Expertised in Analytical Quality by Design (AQbD), […]