COURSE MODULE PHARMACEUTICAL ANALUSIS III (THEORY) 1
INDEX Sr. No. Particulars Page no. 1 Course specifications 3 2 Course objectives 3 3 Course outcomes 3 4 CO-PO matrix 4 5 Teaching and assessment methods 4 6 Course contents (Theory/Practicals) 4 7 Assignment & tutorials 7 8 Learning resources 8 9 Student support 8 10 Schedule of assessment 9 11 Facilities required 9 12 Course improvement process 9 13 Information of faculty member responsible for the course 10 2
1. COURSE SPECIFICATION: Course Identification and General Information a. Course Title: Pharmaceutical Analysis III (Theory) b. Course Number/ Code c. Credit Hours d. Study level/ semester at which this course is offered e. Pre-requisite f. Co-requisite 740 Theory Practical Total 4-4 Semester VII Subject code - 630 - g. Language of teaching the course English h. Prepared by i. Approved by Dr. Ms. Rana Zainuddin & Mr. Obaid Shaikh Dr. Ms. Rana Zainuddin 2. COURSE OBJECTIVES: o To provide the sound basis of advance analytical techniques like NMR, Mass, Chromatographic Techniques and Thermal analysis. o To develop the ability to solve simple spectroscopic problems involving NMR and Mass Spectrometry. o To emphasize the concept of advanced techniques of chromatography and Pharmaceutical importance of it. o To develop the basis for Quality assurance and Good Laboratory practice. o To study packaging materials and their testing. 3. COURSE OUTCOMES: Code Course outcome CO 740.01 Apply the theoretical principles for sophisticated methods such as NMR spectroscopy, mass spectrometry, chromatographic techniques, (GLC, HPLC, HPTLC, Flash, Ion chromatography and HPLC-MS) and thermal methods like TGA, DTA and DSC for drug analysis CO 740.02 Analyze and interpret data. CO 740.03 Plan and select lab experiments using appropriate analytical skills and generate a comprehensive analytical report on the findings. CO 740. CO 740.05 Contrast between activities of QC/QA and comprehend other quality management toolslike GMP, GLP, TQM and ISO 9000. Assess packaging material for different formulations. 3
4. CO-PO MATRIX: Course code (CO) Program Outcome (PO) PO1 PO2 PO3 PO4 PO5 PO6 PO7 PO8 PO9 PO10 PO11 CO 01 M S M H S CO 02 M S H H S CO 03 S H H M M S CO M S S H S CO 05 S S S S 5. TEACHING AND ASSESSMENT METHODS FOR ACHIEVING LEARNING Teaching Strategies /methods used Lectures Group Discussions Demonstrations Problem Solving Sessions Methods of Assessment Assignments Oral Presentations Written Examinations 6. COURSE CONTENT (THEORY/PRACTICALS): Order Topic list/units Subtopics list 01 Proton nuclear magnetic resonance spectrometry Principle involved in the technique. Knowledge about fundamental terms involved such as quantized absorption, flipping of nucleus, spin number, magnetic moment, magnetogyric ratio, relaxation, etc. Equations relating these terms to frequency of radiation & magnetic field [without derivation of the equations]. Types of relaxation processes. Low & high resolution instruments. A brief discussion on the low resolution instrumentation [60 MHz]. Quantitative knowledge of relationship between MHz & magnetic field. An introduction to superconductivity magnets.solvents & reference standards used. Setting up of a NMR scale. Samplepreparation. Shielding & deshielding of a proton & it s effect on chemical shift,discussion on & importance of equivalent & nonequivalent protons [number of signals], chemical shifts [position Number Contact of Hours Hours 10 4h/wk 4
of signal] & their calculation from the spectrum, chemical shifts of different H s, splitting [multiplicity] of a signal, coupling constants [J values], integration [area under the signal]. Importance of these terms in identification [or confirmation] of different functional groups should be covered. Significance & contribution of J value in stereochemistry should be emphasized. Prediction [expected theoretical values] of chemical shifts & multiplicities for all protons from simple structures containing up to 12-15 carbons. 02 Mass spectroscopy Different types of mass spectrometric techniques. Brief knowledge of Chemical Ionization mass spectrometry. Calculations of hydrogen deficiency index [HDI] or unsaturation index [UI]. Base or parent peak, molecular ion, M + 1, M + 2 peaks. Calculations of molecular weight based on M +1 & M + 2 peaks. Formation of molecular ion & further fragmentation. Rearrangements in mass spectrometry. Major modes of fragmentations of hydrocarbons, hydroxyl compounds, halogen compounds, aldehydes, ketones, carboxylic acids, and amines. Introduction [only] to recent advances in MS. 03 Advanced chromatography Introduction, Chemical equilibrium and the properties of the equilibrium constant, Thermodynamics and kinetics in Chromatographic separations, Band Broadening and its mechanism, Multiple Path Processes, Broadening by diffusion, Resistance to mass transfer (RTMT), Develoent of Chromatogram, Capacity Factor, Column resolution, optimization of column performance, Qualitative and quantitative analysis by chromatography. Concept of Normal and Reverse Phase Chromatography. Principle, rate & plate theory, Van Deemter equation 7 05 5
Gas Chromatography 05 High Performance Liquid Chromatography (HPLC) 06 Advanced chromatographic methods [no derivation] & the parameters affecting separation/band broadening. Classification of chromatography, retention factor Introduction to Theory and Principle, Instrumentation, types of columns and detectors. Advantages and limitations. Pharmaceutical and other Applications Introduction to Theory and Principle, importance of column purging. Instrumentation and types of columns and detectors. Concept of silinization and bonded-phases LC-MS. Introduction to UPLC and its applications Ion Pair Chromatography, Ion suppression and Ion Exchange Chromatography, Introduction to Theory and Principle, Instrumentation. Advantages and limitations. Pharmaceutical and other Applications. Size exclusion chromatography: Introduction, principle, instrument. Column packing, Applications. 07 HPTLC Instrumentation, Importance of automation, Pharmaceutical and other Applications.Chiral Chromatography, Flash chromatography,supercritical fluid chromatography 08 Thermal Methods or analysis Introduction to thermal analysis. Thermogravimetry; Isothermal/Static Thermogravimetry, Quasistatic Thermogravimetry, Factors affecting Thermogravimetric curve, Instrumentation, Applications. Differential Thermal Analysis and Differential Scanning Calorimetry; Comparison of DTA and DSC, Types of DSC analysis, Instrumentation, DTA and DSC Curves and their interpretation and Applications 09 Quality Assurance Concept of Quality control and Quality Assurance, Quality Assurance and Quality Management in the Pharma industry, ISO 9000, TQM Functions & advantages of QC & QA, Organizational structure Introduction- History of GLP, QA in 06 08 6
GLP 10 Validation Introduction to Validation of analytical methods as per ICH guidelines 11 Packaging materials Test of packaging materials, cartons, aluminum foils, strip packing, blister packing, ampoules, vials, etc. 7. ASSIGNMENT & TUTORIALS: SCHEDULE OF ASSESSMENT TASKS DURING THE SEMESTER: Sr. No. Assessment Method Week due Marks 01 02 03 Assignments, Exercises & tutorials Sessional ( Internal Theory exam) Continuous Practical Assessment (Sessional Practical exam) Weekly during practicals Proportion of Final Assessment 10 10% 20 20% 10 5% Final exam (theory) As per 80 40% University at 05 Final exam( practical) end of course 80 40% Total 100 100% 7
8. LEARNING RESOURCES: Sr. No. 01 Text books Title of Learning Material Details Willard, Merrit, Dean & Settle, Instrumental methods of analysis Van Nostrand. Silverstein, spectrometric identification of organic compounds, Willey. Beckett & Stenlake, Practical Pharmaceutical chemistry, CBS publisher, New Dehli. KempWilliam, Organic spectroscopy, Pal Grav, N. Y. Kalsi P. S., Spectroscopy of organic compounds, New age publishers, New Delhi. Sinder, Text book of HPLC. Chromatographic Analysis of Pharmaceuticals, John A. Adamovics, 2nd Edition. Techniques and Practice of Chromatography Raymond P. W. Scott, Vol. 70. Identification of Drugs and Pharmaceutical Formulations by Thin Layer Chromatography P. D. Sethi, Dilip Charegaonkar, 2nd Edition. HPTLC Quantitative Analysis of Pharmaceutical Formulations P. D. Sethi. Remington: The Science And Practice Of Pharmacy Edited By David B. Troy, Paul Beringer 02 Essential references (as per syllabus) Principles Of Instrumental Analysis 6th Edition, Doughlas Skoog cgmp For Pharmaceuticals By Manohar A Potdar, Pharmamed Press 03 Reference material WHO and ICH guidelines E-materials and websites 05 Other learning material - www.ich.org/products/guidelines.html https://en.wikipedia.org/wiki/quality_management_system http://apps.who.int/medicinedocs/en/d/js5517e/ 9. STUDENT SUPPORT: Office Hours/Week Two hours minimum Other Procedures e-mail, etc Days Monday Tuesday Wednesday Thursday Friday Saturday Time 8
10. SCHEDULE OF ASSESSMENT: Sr. No. Assessment Method Week due Marks 01 02 03 Assignments, Exercises & tutorials Sessional ( Internal Theory exam) Continuous Practical Assessment (Sessional Practical exam) Weekly during practicals Proportion of Final Assessment 10 10% 20 20% 10 5% Final exam (theory) As per 80 40% University at 05 Final exam( practical) end of course 80 40% Total 100 100% 11. FACILITIES REQUIRED: Sr. No. Particular of Facility Required 01 Lecture Rooms (capacity for 60 students) 02 Computing resources: P-IV-PCs with recent hardware/ utilization of open source and licensed application software 12. COURSE IMPROVEMENT PROCESS: Strategies for obtaining student feedback on effectiveness of teaching: Course delivery evaluation by students using: questionnaires Questionnaire forms and online Other strategies for evaluation of teaching by the instructor or by the department: Periodic review by Academic Planning & Monitoring Committee and departmental review committee, Observations and assistance of colleagues, External assessments by advisors/ examiners and auditors. Periodic review by departmental review committee, Review of course delivery and outcome through assessment and feedback from all stake holders. Process for improvement of teaching: Use of ICT tools, teaching aids, Simultaneous practical orientation and theory classes (SPOT), Adoption of reflective teaching. Course develoent plans: 9
Provide inputs for course improvement and update to University Course develoent Committees (Board of Studies) 13. INFORMATION OF FACULTY MEMBER RESPONSIBLE FOR THE COURSE Name Dr. Rana Zainuddin Office hours 10: 00 am 5:00 Location Contact Details Department of Quality Assurance and Pharmaceutical Analysis Mobile +918668215030 +919028914908 Email: ranazainy@gmail.com Weekdays including Saturdays. Mon Tue Wed Thurs Fri Sat Name Shaikh Obaid Alhilali Office hours 9.30am - 4.30 Location Pharmaceutical Analysis Lab. Contact Details Department of Quality Assurance and Pharmaceutical Analysis Mobile +917020854793 +919370512274 Email: obaidshaikh5342@gmail.com obaidshaikh5342@live.com Weekdays including Saturdays. Mon Tue Wed Thu Fri Sat 10