COMMON PAPER (FIRST SEMESTER) (ALL BRANCHES) I/II M.PHARMACY ADVANCED INSTRUMENTAL METHODS OF ANALYSIS (THEORY)

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1 COMMON PAPER (FIRST SEMESTER) (ALL BRANCHES) MPH 101 (T) I/II M.PHARMACY ADVANCED INSTRUMENTAL METHODS OF ANALYSIS (THEORY) Unit : 1 : UV.VISIBLE SPECTROSCOPY : Brief review of electromagnetic spectrum and absorption of radiations. The chromophore concept, absorption law and limitations. Theory of electronic spectroscopy, absorption by organic molecules, choice of solvent and solvent effects, modern instrumentation - design and working principle. Applications of UV-Visible spectroscopy (qualitative and quantitative analysis), Woodward - Fischer rules for calculating absorption maximum. Unit : 2 : INFRARED SPECTROPHOTOMETRY ; Introduction, basic principles, vibrational frequency and factors influencing vibrational frequency, instrumentation and sampling techniques, interpretation of spectra, applications in Pharmacy. FT-IR-theory and applications, Attenuated Total Reflectance (ATR). Unit : 3 : NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY : Fundamental Principles and Theory, Instrumentation, solvents, chemical shift and factors affecting chemical shift, spin-spin coupling, coupling constant and factors influencing the value of coupling constant, spin-spin decoupling, proton exchange reactions, FT-NMR, 2D-NMR, NMDR, NOE, NOESY, COSY and applications in Pharmacy, interpretation of spectra, C13 NMR-Introduction, Natural abundance, C13 NMR Spectra and its structural applications. Unit : 4 : MASS SPECTROSCOPY: Basic principles and instrumentation, ion formation and types, fragmentation processes and fragmentation pattern, Chemical ionization mass spectroscopy (CIMS), Field Ionization Mass Spectrometry (FIMS), Fast Atom Bombardment MS(FAB MS), Matrix Assisted laser desorption/ionization MS (MALDI-MS), interpretation of spectra and applications in Pharmacy. :: 01 ::

2 Unit : 5 : CHROMATOGRAPHIC TECHNIQUES : a) Classification of chromatographic methods based on mechanism of separation; paper chromatography, thin layer chromatography, ion exchange chromatography, column chromatography and affinity chromatography - techniques and applications. b) Gas Chromatography : Theory and principle, column operation, instrumentation, derivatisation methods and applications in Pharmacy. c) High Performance Liquid Chromatography : Principle, instrumentation, solvents used, elution techniques, RP-HPLC and applications in pharmacy. d) HPTLC : Theory and Principle, instrumentation, elution techniques and pharmaceutical applications. Unit : 6 : X-RAY DIFFRACTION AND DSC, DTA METHODS : Introduction, Generation of X-Rays, Elementary crystallography; miller Indices, X-ray, diffraction Bragg s law, X-ray powder diffraction, X-ray powder diffractometer, obtaining and interpretation of X-ray powder diffraction data. Applications of XRD, DSC and DTA in the characterization of Pharmaceutical solids. Unit : 7 : STATISTICAL ANALYSIS : Introduction, significance of statistical methods, normal distribution, probability, degree of freedom, standard deviation, correlation, variance, accuracy, precision, classification of errors, reliability of results, confidence interval. Test for statistical significance - students T-test, F-test, Chi-square test, correlation and regression. :: 02 ::

3 I/II M.PHARMACY (1 st SEMESTER) ADVANCED INSTRUMENTAL METHODS OF ANALYSIS (PRACTICALS) 01. Determination of Isobestic point using bromocresol green. *02. Estimation of ranitidine hydro chloride in pharmaceutical formulation by PDAB reagent. *03. Estimation of aceclofenac in pharmaceutical formulation by FC reagent. 04. Estimation of ciprofloxacine in pharmaceutical formulation by ferric. *05. Estimation of sulphamethoxazole in pharmaceutical formulation by BM reagent. 06. Estimation of paracetamol (or) gatifloxacine (or) frusemide in pharmaceutical formulation by UV spectroscopy. 07. Simultaneous estimation of amoxicillin & dicloxacillin (or) paracetamol & nimesulide in pharmaceutical formulation by UV spectroscopy. 08. Estimation of Vit B1 & metformin (or) atorvastatin & ezetimib in pharmaceutical formulation by absorbance ratio method. 09. Estimation of paracetamol & diclofenac (or) ornidazole & ofloxacine in pharmaceutical formulation by derivative spectroscopy. 10. Estimation of moisture content by KFR 11. Estimation of sodium ions by flame photometer. 12. Estimation of potassium ionsby flame photometer *13. Estimation of paracetamol (or) aspirin (or) nimesulide in pharmaceutical formulation by HPLC. *14. Simultaneous estimation of paracetamol & nimesulide in pharmaceutical formulation by HPLC. *15. Estimation of paracetamol in pharmaceutical formulation by using caffeine as internal standard by HPLC. 16. Characterization of pharmaceutical solids by using recorded data of XRD and DSC. 17. Prediction of -max for different organic compounds by using woodward fischer rule. MPH 102 (P) 18. Interpretation of IR spectra s for different organic compounds. 19. Interpretation of NMR spectra s for different organic compounds. 20. Interpretation of MASS spectra s for different organic compounds. :: 03 ::

4 REFERENCE BOOKS : 01. Spectrometric identification of Organic Compounds, Robert, M.Silverstein et al, 7th edition, Fundamentals of Mathematical Statistics, S.C.Gupta and V.K.Kapoor. 03. Principles of Instrumental Analysis by Donglas A.Skoog, James, J.Leary, 4th Edition. 04. Pharmaceutical Analysis - Modern Methods - Part A, Part B, James W. Munson Vogel s Text Book of Quantitative Chemical Analysis, 6th Edition, Chromatographic Analysis of Pharmaceuticals, John A.Adamovics, 2nd Edition. 07. Practical Pharmaceutical Chemistry, Part two, A.H.Beckett & J.B.Stenlake - 4th Edition. 08. Instrumental Methods of Chemical Analysis - B.K.Sharma - 9th Edition. 09. Instrumental Methods ofanalysis - Hobert H.Willard, 7th Edition. 10. Organic Spectroscopy - William Kemp, 3rd Edition. 11. Techniques and Practice of Chromatography - Raymond P.W.Scott, Vol Identification of Drugs and Pharmaceutical Formulations by Thin Layer Chromatography - P.D.Sethi, Dilip Charegaonkar, 2nd Edition. 13. HPTLC-Quantitative Analysis of Pharmaceutical Formulations - P.D.Sethi, 14. Liquid Chromatography - Mass Spectrometry, W.M.A.Niessen, J.Van Der Greef, Vol Stereo Chemistry - Conformation and Mechanism by P.S.Kalsi, 2nd Edition. 16. Spectroscopy of Organic Compounds by P.S.Kalsi. 17. Organic Chemistry by I.L.Finar Vol. II - 5th Edition. :: 04 ::

5 I/II M.PHARMACY (1 ST SEMESTER) ADVANCED INSTRUMENTAL METHODS OF ANALYSIS (THEORY) MODEL QUESTION PAPER TIME: 3HOURS MAX MARKS: 70 ALL QUESTIONS CARRY EQUAL MARKS ANSWER ANY FIVE QUESTIONS 1. (a) Explain Beer-Lamberts law and discuss about the deviations from beer s law. (b) What are the most frequent electronic transitions during absorption of electromagnetic Radiation? Which results is more intense absorption? Give examples of compounds that exhibit each. 2. (a) Explain the different detectors used in gas chromatography with (b) a neat diagram. Distinguish between packed columns and capillary columns in GC. Add note on Van deemter equation. 3. Explain the following terms: a) Reverse-phase chromatography. b) Normal phase chromatography. c) Column efficiency parameters. 4. a) Explain the term chemical shift and discuss the factors influencing chemical shift. b) Write a short note on the following: (i) Longitudinal relaxation (ii) Transverse relaxation 5. (a) What is the necessary criterion for absorption to occur in the IR region? What types of molecular vibration are associated with IR absorption? (b) MPH 101 (T) Name the functional groups that are present in a molecule for the corresponding wave numbers in an IR spectrum. (i) 3300 cm -1 (ii) 1690 cm -1 (iii) Band at 1600, 1490 and cm -1 (iv) 3000 cm a) Explain the principal involved in FAB-Mass spectrometry with example. b) Describe briefly the instrumentation of a quadruple mass spectrometer and write its advantage. 7. a) Write the principle involved and working of X-ray power diffracto meter. Add note on Application of X-ray diffractometer in pharmacy with example. b) Explain with example how DSC and DTA studies are useful in preformulation and formulation Development studies. c) C 13 NMR :: 05 ::

6 I/II M.PHARMACY (1 ST SEMESTER) MODEL QUESTION PAPER (PRACTICALS) Time: 6 hrs Max Marks: Synopsis : 15 Marks *2. Major Experiment : 25 Marks 3. Minor Experiment : 15 Marks 4. Viva-voce : 15 Marks MPH 102 (P) Note : Total sessional marks is 30 (20 for practical sessional plus 10 marks for regularity, promptness, viva-voce and record maintenance). :: 06 ::

MODERN PHARMACEUTICAL ANALYSIS

MODERN PHARMACEUTICAL ANALYSIS THEORY GOALS: The important goals of this course are to give through understanding of the spectroscopy, Mass and chromatographic techniques so that the post graduate students