Osmania University
Syllabus for M. Pharmacy
(Pharmaceutical Analysis and Quality Assurance)
(w.e.f. academic year 2013-14)
Faculty of Technology,
Hyderabad
Scheme of Instruction and Evaluation for M. Pharmacy
(Pharmaceutical Analysis and Quality Assurance)
I – Semester Revised-2013
Subject Code
M PAQ.T. 1.101
M PAQ.T. 1.102
M PAQ.T.1.103
M PAQ.T. 1.104
M PAQ.T. 1.105
M PAQ.P. 1.106
M PAQ.P. 1.107
M PAQ.T. 1.108
M PAQ .1.109
Subject / Paper
Pharmaceutical
Analytical Techniques
Instrumental Methods of
Analysis
Pharmaceutical Product
Development
Quality Control of Health
Related Products
Pharmaceutical Analysis
Pharmaceutical Analytical
Techniques
Pharmaceutical Product
Development
Scientific and Technical
Writing (SAIL)
Seminar
Theory /
Practical
Instruction Hours
per week
Evaluation
Duration of
External
Examination
Theory
Practical
Internal
External
Theory
4
---
30
70
3
Theory
4
---
30
70
3
Theory
4
---
30
70
3
Theory
4
---
30
70
3
Theory
4
---
30
70
3
Practical
-
4
30
70
6
Practical
--
4
30
70
6
Tutorial
2
-
A/B/C/D
-
-
18
8
20
60
240
420
Theory
Scheme of Instruction and Evaluation for M. Pharmacy
(Pharmaceutical Analysis and Quality Assurance)
II– Semester Revised-2013
Subject Code
M P Q.T. 1.201
M PAQ.T. 1.202
M PAQ.T. 1.203
M PAQ.T. 1.204
M PAQ.T. 1.205
M PAQ.P. 1.206
M PAQ.P. 1.207
M PAQ.T. 1.208
M PAQ. 1.209
Subject / Paper
IPR & Regulatory Affairs
Quality Control of Raw
Materials (RM) and Finished
Pharmaceutical Products (FPP)
Analytical Method Validation
Quality Assurance and
Management
Research Methodology
Quality Control of Raw
Materials (RM) and Finished
Pharmaceutical Products (FPP)
Analytical Method Validation
Entrepreneurship Management
(SAIL)
Seminar
SAIL: Self assess Interactive Learning
Theory /
Practical
Theory
Instruction Hours
per week
Theory Practical
4
---
Internal
30
External
70
Duration of
External
Examination
3
Evaluation
Theory
4
---
30
70
3
Theory
4
---
30
70
3
Theory
4
---
30
70
3
Theory
4
---
30
70
3
Practical
--
4
30
70
6
Practical
--
4
30
70
6
Tutorial
2
-
A/B/C/D
-
-
18
8
20
50
230
420
Theory
Scheme of Instruction and Evaluation for M. Pharmacy
(Pharmaceutical Analysis and Quality Assurance)
Semester III and IV
DISSERTATION – Original research work carried out by the candidate under the guidance
of regular teaching faculty/visiting faculty of the department should be submitted in a bound
form.
Evaluation of the dissertation shall be done by external and internal examiners appointed by
the university.
Dissertation viva-voce
Grade A/B/C/D/F
Dissertation report
Grade A/B/C/D/F
A. Excellent
B. Very good
C. Good
D. Fair
PHARMACEUTICAL ANALYTICAL TECHNIQUES
M PAQ. T.1.101
Sessional: 30
Examinations: 70
Period / Week: 4
Duration of Exam: 3 hrs
Nature of Exam: Theory
UNIT – I
UV-Visible Spectroscopy: Basic principles, interaction of electromagnetic radiation with
matter and its effects (electronic transitions). Concept of chromophore and auxochrome,
effect of conjugation, solvent and pH. Instrumentation (components and their significance).
Absorption spectra of organic compounds and complexes illustrating the phenomenon and its
utilization in qualitative and quantitative studies of drugs including multicomponent analysis.
Woodward-Fieser rules for caculating absortion maximum for unsaturated hydrocarbons.
Difference and derivative spectra.
Infra-Red Spectroscopy: Interaction of infrared radiation with organic molecules and it’s
effects on bonds. Instrumentation- Dispersive IR spectrophotometers and Fourier transform
spectrophotometers. Sample handling for IR spectroscopy. Interpretation of IR spectra. Brief
note on ATR. (Attenuated Total Reflectance).
UNIT – II
Nuclear Magnetic Resonance Spectroscopy: Fundamental principles of NMR,
instrumentation (components and their significance). Chemical shifts concept, spin- spin
coupling, spin-spin decoupling, shielding, deshielding, shift reagents and solvents. Signal
multiplicity phenomena in high resolution PMR. Interpretation of PMR spectra.
Brief introduction about Carbon-13 NMR and 2D NMR Spectroscopy.
UNIT – III
Mass Spectrometry: Basic principles and instrumentation (components and their
significance). Ionization techniques, mass spectrum and its characteristics, molecular ion,
metastable ions, fragment ions; fragmentation processes, fragmentation patterns and fragment
characteristics in relation to parent structure and functional groups. Relative abundances of
isotopes and their contribution to characteristic peaks.
UNIT – IV
Chromatographic Techniques: Classification of chromatographic methods based on
mechanism of separation and their basic principles. Gas chromatography: Instrumentation,
column efficiency parameters, derivatisation methods, applications in pharmaceutical
analysis. Liquid chromatography: Comparison of GC and HPLC, instrumentation in HPLC,
normal and reversed phase packing materials, column selection, mobile phase selection,
efficiency parameters, applications in pharmaceutical analysis. Instrumentation and
applications of HPTLC, ion exchange chromatography, gel permeation chromatography,
chiral chromatography, flash chromatography, and supercritical fluid chromatography (SFC).
Unit – V
Electrophoresis: Principles, instrumentation and applications of moving boundary
electrophoresis zone electrophoresis (ZE), isotachphoresis, isoelectric focusing (IEF),
Continuous electrophoresis (preparative) and capillary electrophoresis. SDS gel
electrophoresis and blotting techniques.
Radio immunoassay and ELISA: Principle, instrumentation, applications and limitations.
Recommended books:
1.
Skoog, DA, Holler, FJ, Crouch, SR. Principles of instrumental analysis. 6th ed., Baba
Barkha Nath printers, Haryana, 2007.
2.
Silverstein, RM, Webstar, FX. Spectrometric identification of organic compounds. 6th
ed., John Wiley & Sons (Asia) Pvt. Ltd., Singapore, 2005.
3.
William Kemp. Organic spectroscopy, 3rd ed., Palgrave, New York, 2006.
4.
Jag Mohan, Organic spectroscopy: Principles and Applications, 2nd ed., Narosa
publishing house Pvt Ltd., New Delhi, 2005.
5.
Conners KA. A Text book of pharmaceutical analysis, 3rd ed., John Wiley & Sons,
Singapore, 2004.
6.
Willard HH, Merritt LL, Dean JA, Settle FA. Instrumental methods of analysis, 7th
ed., CBS Publishers & Distributors, New Delhi, 1986.
7.
Pavia DL, Lampman GM, Kriz GS, Vyvyan JA. Introduction to spectroscopy. 4th ed.,
Brookescole publishers, California, 2008.
8.
Sharma BK. Instrumental methods of chemical analysis, 25th Ed., Goel Publishing
house, Meerut, 2006.
9.
Beckett, AH, Stenlake, JB. Practical pharmaceutical chemistry, Part I & II, 4 th ed.,
CBS Publishers & distributors, New Delhi, 2004.
10. Ewing, GW. Instrumental methods of chemical analysis, 5th ed., McGraw Hill Book
Company, New York, 1985.
11. Schirmer, RE. Modem methods of pharmaceutical analysis, Vol. I & II, 2nd ed., CRC
Press, Florida, 2000.
INSTRUMENTAL METHODS OF ANALYSIS
M PAQ. T.1.102
Sessional: 30
Examinations: 70
Period / Week: 4
Duration of Exam: 3 hrs
Nature of Exam: Theory
UNIT – I
Microscopy: General aspects, hot stage microscopy, scanning electron microscopy (SEM),
transmission electron microscopy (TEM): principle, instrumentation and applications.
Particles size analysis: Zetameter, Photon correlation spectroscopy, counter-counter
apparatus, atomic force microscopy and confocal.
UNIT – II
Emission Spectrophotometry: Principles, instrumentation and applications of raman, laser,
plasma, atomic absorption spectroscopy and flame spectroscopy.
Spectrofluorimetry: fluorescence, phosphorescence, chemiluminiscence: theory,
instrumentation and applications.
UNIT – III
Thermal Methods of Analysis: Principles, instrumentation and applications of
thermogravimetric analysis (TGA), differential thermal analysis (DTA), differential scanning
calorimetry (DSC), and thermo mechanical analysis (TMA).
UNIT – IV
Hyphenated Techniques: LC-MS, GC-MS, MS-MS and LC-NMR, principle and
applications in pharmacy
UNIT – V
X-Ray Spectroscopy: Origin of X-rays, basic aspects of crystals, X-ray crystallography,
miller indices, rotating crystal technique, single crystal diffraction, powder diffraction,
structural elucidation and applications.
Recommended Books:
1. Skoog DA, Holler FJ, Crouch SR. Principles of instrumental analysis. 6th ed., Baba
Barkha Nath printers, Haryana, 2007.
2. Silverstein RM, Webstar FX. Spectrometric identification of organic compounds. 6th
ed., John Wiley & Sons (Asia) Pvt, Ltd., Singapore, 2005.
3. Willard HR, Merritt LL, Dean JA, Settle FA. Instrumental methods of analysis, 7th
ed., CBS Publishers & distributors, New Delhi, 1986.
4. Ewing GW. Instrumental methods of chemical analysis, 5th ed., McGraw Hill Book
Company, New York, 1985.
5. Schirmer RE. Modem methods of pharmaceutical analysis, Vol. I & II, 2nd ed., CRC
Press, Florida, 2000.
6. Lee DC, Webb M. Pharmaceutical Analysis, Blackwell publishing, Australia, 2004.
7. Gurdeep R. Chatwal, Instrumental Methods of Chemical Analysis, Himalaya
Publishing House, 2006.
8. Ashutosh kar, Pharmaceutical Drug Analysis, New Age International Publishers.
9. Whoston C. X-ray methods, John Wiley & Sons, New York, 1987
PHARMACEUTICAL PRODUCT DEVELOPMENT
M PAQ.T.1.103
Sessional: 30
Examinations: 70
Period/Week: 4
Duration of Exam: 3 hrs
Nature of Exam: Theory
UNIT – I
Preformulation (API): Influence of melting point, dissociation constant, pharmaceutical
salts and hygroscopicity, physical forms of drugs, Methods of preparation and
characterization.
Design of Experiments: optimization, general principles (applications, advantages and
disadvantages, variables), strategies, classification, mathematical models and statistical tests,
simulation and search methods, factorial design of experiments, central composite design,
mixture and simplex design, fractional factorial design, Plackett Burman screening methods.
UNIT – II
Preformulation (Excipients Science): Tablet excipients, factors influencing selection of
excipients, directly compressible excipients, coprocessing of excipients, determination of
functionality tests of excipients, flow properties, compression properties, drug-excipient
compatibility, methods of evaluations, formulation development of hard gelatin capsules,
suspensions,
UNIT – III
Solubility: Importance, experimental determination, aqueous solubility aspects in
preformulation, intrinsic solubility, phase-solubility analysis, pH solubility profile,
UNIT – IV
Solubility Improvement: solubility techniques to improve solubility and utilization of
analytical methods-cosolvency, salt formation, complexation, solid dispersion, micellar
solubilization, hydrotropy.
UNIT – V
Dissolution: General principles, drug absorption, In-vitro dissolution testing kinetic modelssink and non-sink conditions, dissolution aspects in preformulation, intrinsic dissolution rate,
dissolution test apparatus- design, dissolution testing of conventional and controlled release
products, data handling and correction factors, in vitro-in vivo correlations, levels of
correlation.
Recommended books:
1. Lachman L, Lieberman HA, Kanig JL. The theory and practice of industrial
pharmacy, 3rd ed., Varghese Publishers, Mumbai 1991.
2. Sinko PJ. Martin's physical pharmacy and pharmaceutical sciences, 5th ed., B.I.
Publications Pvt. Ltd, Noida, 2006.
3. Lieberman HA, Lachman L, Schwartz JB. Pharmaceutical dosage forms: tablets Vol.
I-III, 2nd ed., CBS Publishers & distributors, New Delhi, 2005.
4. Conners KA. A Text book of pharmaceutical analysi Wells JI. Pharmaceutical
preformulation: The physicochemical properties of drug substances. Ellis Horwood
Ltd., England, 1998.
5. Yalkowsky SH. Techniques of solubilization of drugs. Vol-12. Marcel Dekker Inc.,
New York, 1981.
6. Dressman J, Kramer J. Pharmaceutical dissolution testing. Saurah printer pvt. Ltd.,
New Delhi, 2005..
7. Sethi PD. Quantitative analysis of drugs in pharmaceutical formulations, 3rd ed., CBS
publications, New Delhi, 2008.
8. Carstensen JT, Rhodes CT. Drug stability principles and practices, 3rd ed., CBS
Publishers & distributors, New Delhi, 2005.
9. Yoshioka S, Stella VJ. Stability of drugs and dosage forms, Springer (India) Pvt. Ltd.,
New Delhi, 2006.
10. Banker GS, Rhodes CT. Modern Pharmaceutics, 4th ed., Marcel Dekker Inc, New
York, 2005.
11. W. Grimm - Stability testing of drug products.
12. Mazzo DJ. International stability testing. Eastern Press Pvt. Ltd., Bangalore, 1999.
13. Beckett AH, Stenlake JB. Practical pharmaceutical chemistry, Part I & II., 4 th ed.,
CBS Publishers & distributors, New Delhi, 2004.
14. Indian Pharmacopoeia. Controller of Publication. Delhi, 1996.
15. British Pharmacopoeia. British Pharmacopoeia Commission Office, London, 2008.
16. United States Pharmacopoeia. United States Pharmacopeial Convention, Inc, USA,
2003.
QUALITY CONTROL OF HEALTH RELATED PRODUCTS
M PAQ. T.1.104
Sessional: 30
Examinations: 70
Period / Week: 4
Duration of Exam: 3 hrs
Nature of Exam: Theory
UNIT – I
Quality Control of Cosmeceuticals: Hair care products (shampoo and hair dyes), baby care
products (oils, creams, powders and shampoos), personal hygiene products (shaving creams,
after shave lotions and soaps), eye care products (eye shadows, eye liners, and eye brow
pencils)
UNIT – II
Quality Control of Herbal Products: WHO guidelines for the quality control of raw
materials used in herbal formulations. Quality control of crude drugs: proximate analysis,
including ash and extractive values, crude fiber content, UV and fluorescence analysis of
powdered drugs, quantitative microscopy and micro-chemical tests. Analysis of official
formulations derived from crude drugs including some herbal preparations, alkaloids
(ephedrine, reserpine and ergotamine).
UNIT – III
Quality control of Biological Products: Biological assays of the following.
1. Vaccines: diphtheria, tetanus, rabies.
2. Enzymes: streptokinase, urokinase.
3. Antitoxins: diphtheria, tetanus.
4. Hormones: chronic gonadotropin, oxytoxin, insulin.
UNIT – IV
Quality Control of Nutraceuticals: Vitamins (A, B1, B2, B12, C, D, E and K), micro
nutrients and health supplements including free radical scavengers.
UNIT – V
Quality Control of Food Constituents: Carbohydrates, proteins and fats with special
emphasis in the determination of moisture, ash, nitrogen and physical constituents. General
analytical methods for milk and milk constituents (milk powder and margarine).
Recommended books:
1. Commercial’s manual on drugs & cosmetics. 2nd ed., Commercial Law Publishers
(India) Pvt. Ltd., Delhi, 2004.
2. Sharma PP. Cosmetics-formulation, manufacturing and quality control. 3rd ed.,
Vandana Publications Pvt. Ltd., Delhi, 2005.
3. Kokare CR. Pharmaceutical microbiology and biotechnology. 2nd ed., Nirali
Prakashan, Pune, 2006.
4. Nanda S, Nanda A, Khar RK. Cosmetic technology. Birla Publications Pvt. Ltd.,
Delhi, 2007.
5. Mukherjee PK. Quality control of herbal drugs: an approach to evaluation of
botanicals. Business horizons, New Delhi, 2007.
6. Evans WC. Trease and evans pharmacognosy. 15th ed., Saunders, China, 2004.
7. Lachman L, Lieberman HA, Kanig JL. The theory and practice of industrial
pharmacy, 3rd ed., Varghese Publishers, Bombay, 1991.
8. Remington: The science and practice of pharmacy. 21st ed., vol. I & II, Lippincott
Willams & Wilkings, Noida, 2006.
9. Agrawal SS, Paridhavi M. Herbal drug technology. Universities Press (India) Pvt.
Ltd., Hyderabad, 2007.
10. Nelson DL, Cox MM. Lehninger principles of biochemistry. 4th ed., Replika Press
Pvt. Ltd., India, 2006.
11. Murray RK, Granner DK, Rodwell VW. Harper’s illustrated biochemistry, 27th ed.,
McGraw-Hill, New Delhi, 2006.
12. David Pearson. The chemical analysis of foods, 7th ed., Churchill Livingstone,
Edinburgh, 1976.
13. Nielsen S. Introduction to chemical analysis of foods. Jones & Barlett Publishers,
Boston, 1974
PHARMACEUTICAL ANALYSIS
M PAQ. T.1.105
Sessional: 30
Examinations: 70
Period / Week: 4
Duration of Exam: 3 hrs
Nature of Exam: Theory
UNIT – I
Potentiometry and pH metry: Principles and theoretical aspects – electrodes, representation
of electrodes and cells, measurement of cell potential, measurement of pH, end point
evaluation methods, null point Potentiometry and applications.
Conductometry: Principles and theoretical aspects – conductance, equivalent and molar
conductance, instrumentation, measurement of conductivity, wheatstone bridge principle and
conductometric applications
UNIT – II
Polarography: Principle and theoretical aspects – instrumentation, factors effecting limiting
current, cells, form of waves, half wave potentials and applications.
Amperometry: Principle and theoretical aspects-instrumentation, different types of
amperometric titrations with dropping mercury electrode, rotating platinum electrode and
applications.
UNIT – III
Optical Methods: Principle, instrumentation and applications of refractometry, polarimetry,
nephelometry and turbidometry
Optical Rotatory Dispersion (ORD) and Circular Dichroism (CD): Principles and
theoretical aspects – instrumentation, sample handling and applications.
UNIT – IV
In-process quality control : Importance, inspection, IPQC tests for tablets (weight
variation, hardness, thickness, friability, disintegration tests and content uniformity),
suspensions and emulsions (appearance and feel, volume check, viscosity, particle size
distribution, electrical conductivity and content uniformity) and parenterals (pH, volume
check, clarity, content uniformity, integrity of seals and particulate matter). Problems
encountered and trouble shooting.
UNIT – V
Impurity Profile: Sources of impurities, their effect on drug stability and therapeutic action.
Determination of impurities in bulk drugs and formulation - Isolation, characterization,
analytical methods and guidelines as per ICH and WHO for impurity and related substances
in the drugs, concept of purity angle, purity threshold and purity flag
Recommended books:
1. Ahuja S, Alsante KM. Handbook of isolation and characterization of impurities in
pharmaceuticals. Academic press, California, 2003
2. Skoog DA, Holler FJ, Crouch SR. Principles of instrumental analysis. 6th ed., Baba
Barkha Nath printers, Haryana, 2007.
3. Silverstein RM, Webstar FX. Spectrometric identification of organic compounds. 6th
ed., John Wiley & Sons (Asia) Pvt, Ltd., Singapore, 2005.
4. Willard HR, Merritt LL, Dean JA, Settle FA. Instrumental methods of analysis, 7th
ed., CBS Publishers & distributors, New Delhi, 1986.
5. Ewing GW. Instrumental methods of chemical analysis, 5th ed., McGraw Hill Book
Company, New York, 1985.
6. Schirmer RE. Modem methods of pharmaceutical analysis, Vol. I & II, 2nd ed., CRC
Press, Florida, 2000.
7. Lee DC, Webb M. Pharmaceutical Analysis, Blackwell publishing, Australia, 2004.
8. Gurdeep R. Chatwal, Instrumental Methods of Chemical Analysis, Himalaya
Publishing House, 2006.
9. Ashutosh kar, Pharmaceutical Drug Analysis, New Age International Publishers.
INTELLECTUAL PROPERTY RIGHTS & REGULATORY AFFAIRS
M PAQ.T.1.201
Sessional: 30
Examinations: 70
Period/Week: 4
Duration of Exam: 3 hrs
Nature of Exam: Theory
UNIT – I
Intellectual Property Rights (IPR): Objectives, types of IPR, Patents-advantages, types,
criteria, inventions – patentable, Impact on Pharmaceutical Industry, copyrights-types rights,
trademarks-functions, types, geographical indications-significance, types, industrial designs,
integrated circuits, trade secrets.
UNIT – II
India Patents Act, 1970, Amendments, 1999, 2002, 2005, stages of patenting, patent
opposition (Post Grant), maintaining the patent rights – Conditions, patent information –
search and sources
International Organizations and Agreements – IPR: General Agreement on Tariffs and
Trade (GATT)- Historical perspectives, objectives and impact, World Trade Organization
(WTO)- scope, functions, structure, withdrawal of membership, dispute settlement, World
Intellectual Property Organization (WIPO) - objectives and programs, Paris Convention –
background, scope, impact, Berne Convention, TRIPS Agreement-scope general features,
specific features, The Doha Declaration, Patent Cooperation Treaty (PCT), Madrid Protocol.
UNIT – III
Related Quality Systems: ISO- quality concepts, quality management – vocabulary, ISO
9000 series- standards, guidelines and selection, quality management systems – requirements,
ISO - certification procedure, ISO 14000.
ICH - stability guidelines, harmonization efforts, basic principles, testing of new drug
substance, new drug products, photostability, containers, WHO stability guideline. ICH Q11
(Quality management systems).
Total Quality Management (TQM): Principles, elements of TQM, continuous improvement
and learning, management tools, tools and techniques of quality, new quality tools and
techniques
UNIT – IV
Regulatory Affairs: Indian context-Requirements and guidelines of GMP understanding of
drugs and Cosmetics Act 1940 and Rules 1945 with reference to schedule M, U and Y.
USFDA, orange book, FDA guidelines on investigational new drugs (IND), New drug
applications (NDA).
Unit – V
Documentation: CTD dealing with post approval changes, SUPAC, handling and
maintenance including electronic documentation.
Generic Drug Products: General principles, categories of OUT of patent pharmaceuticals,
Hatch - Waxman Act, Bolar amendment, principles of exclusivity, drug regulations – ANDA,
generic drug product development, generic drug product approval.
Documentation: (CGMP - Subpart J)
File exclusives (NCL, NS, NP, NDF, PED, ODE, PC exclusivity).
Recommended books:
1. Guarino RA. New drug approval process, 4th ed., vol 139, Marcel Dekker Inc., New
York, 2004.
2. Willing SH. Good manufacturing practices for pharmaceuticals. 5th ed., vol 109,
Marcel Dekker Inc., New York, 2001.
3. Das P, Das G. Protection of industrial property rights.
4. Katju SN. Laws and drugs. Law Publishers.
5. Original Laws published by Government of India.
6. Hussain. Law of drugs in India.
7. Websites: www.fda.org; www.wipo.int, www.ich.org, www.cder.org.
8. Subrahmanyam CVS, Thimma Setty JPharmaceutical Regulatory Affairs, Vallabha
Prakashan, Delhi 2012.
QUALITY CONTROL OF RAW MATERIALS (RM) AND FINISHED
PHARMACEUTICAL PRODUCTS (FPP)
M PAQ. T.1.202
Sessional: 30
Examinations: 70
Period / Week: 4
Duration of Exam: 3 hrs
Nature of Exam: Theory
UNIT – I
Reagent Based and Functional Group Based Analysis of APIs: Analytical principles,
procedures and applications involved in the use of the following reagents.
a) MBTH (3-methyl-2-benzothiazoline hydrazone).
b) Folin – Ciocalteu (FC) reagent.
c) 2,6- Dichloroquinone chlorimide.
d) 2,3,5- Triphenyl tetrazolium salt.
e) 1,2- naptho quininone -4- sulfonate.
f) Bratton-Marshall reagent.
g) PDAC (P-Dimethyl amino cinnamaldehyde) .
h) PDAB (P-Dimethyl amino benzaldehyde)
UNIT – II
Principles and procedures involved in quantitative determination of the following functional
groups:
A) Hydroxy
B) Aldehyde
C) Ketone
D) Amine
E) Methoxyl
F) Ester
G) Carboxyl
UNIT – III
Quality Control of Excipients: Tests related to excipients (disintegrating agents, binders,
emulsifiers, viscosity modifiers and preservatives) such as bulk density, tapped density,
particle size distribution, pH, moisture content, viscosity (dynamic), gelling temperature,
swelling temperature, loss on drying, residue on ignition, conductivity, congealing range,
readily carbonizable substances and readily oxidizable substances, melting point and melting
range, including preservative challenge test.
UNIT – IV
Quality Control of Packaging Materials: Containers – Glass: light transmission, chemical
resistance – glass containers, powdered glass test, water attack test. Biological tests – plastics
and other polymers: physicochemical tests – plastics, polyethylene containers, single unit
containers and unit dose containers for non sterile solids and liquid dosage forms, customized
patient medication packages, containers – permeation, metal containers, and rubber closures.
UNIT – V
Analysis of Drugs in Dosage Forms: Principles and procedures involved in the analysis of
drugs in dosage forms: A) Antibacterials (penicillins, erythromycin) and fluoroquinolones B)
steroids (cholesterol, progesterone, and androsterone); C) Anti-inflammatory drugs
(nimusuline, diclofenac. Ibuprofen and indomethacin); D) Antihypertensive drugs
(propranolol, levodopa); and E) antidiarrhoeals (metronidazole, tinidazole).
Recommended books:
1. Hiaguchi T, Brochmann E, Hanssen H, Hanseen H. Pharmaceutical analysis, CBS
publishers & distributors, New Delhi, 2004.
2. Rowe RC, Sheskey PJ, Owen SC. Handbook of Pharmaceutical excipients. 5th ed.,
Pharmaceutical press, Britain, 2006.
3. Lachman L, Lieberman HA, Kanig JL. The theory and practice of industrial
pharmacy, 3rd ed., Varghese Publishers, Mumbai 1987.
4. Sethi PD. Quantitative analysis of drugs in pharmaceutical formulations, 3rd ed., CBS
publishers & distributors, New Delhi, 2008.
5. Beckett AH, Stenlake JB. Practical pharmaceutical chemistry, Part I & II., 4 th ed.,
CBS publishers & distributors, New Delhi, 2004.
6. Remington: The science and practice of pharmacy. 21st ed., vol. I & II, Lippincatt
WilIams & Wilkings, New Delhi, 2005.
7. Indian Pharmacopoeia. Controller of Publication. Delhi, 2007.
8. British Pharmacopoeia. British Pharmacopoeia Commission Office, London, 2008.
9. United States Pharmacopoeia. United States Pharmacoepial Convention, Inc, USA
ANALYTICAL METHOD VALIDATION
M PAQ. T.1.203
Sessional: 30
Examination: 70
Period/week: 4
Duration of Exam: 3 hrs
Nature of Exam: Theory
UNIT – I
Analytical Method Development: Introduction, calibration and validation of various
analytical instruments such as UV and visible spectrophotometer, FT-IR and HPLC for drug
analysis and maintenance of instruments.
UNIT – II
Analytical Procedures Validation: Needs, types, accuracy, precision, linearity, robustness,
specificity, ruggedness, system suitability parameters, LOQ, and LOD. Sources of errors,
use of significant figures and their correct usage, importance of revalidation
UNIT – III
Development of Analytical Methods and Validation: The instruments include UV-visible
spectrophotometer, FT-IR spectrometer, HPLC and GC-MS.
UNIT – IV
Drug Analysis in Biological Matrices: Selection of biological sample, extraction of drugs
by various methods as LLE, SPE and membrane filtration, factors affecting extraction of
drugs, bio analytical method validation.
UNIT – V
Validation Methods: Methods of validation for the following – pharmaceutical water
systems, cleaning validation, HVAC system and vendor qualification. Validation master plan
and validation protocol.
Process validation (PV): (prospective, retrospective and concurrent).
Recommended books:
1. Nash RA, Wachter AH. Pharmaceutical process validation, 3rded., CBS publications
& Distributors, New Delhi, 2005.
2. Carleton FJ, Apalloco JP. Validation of pharmaceutical processes-sterile products.
Marcel Dekker Inc., New York, 2006.
3. Haider Si. Pharmaceutical master validation plan. St.Lucie Press, Noida, 2006.
4. Ahuja S, Alasante KM. Handbook of isolation and characterization of impurities in
pharmaceuticals. Elsevier Publications, New Delhi, 2005.
5. Parker M. Quality Assurance and TQM for analytical laboratories, The Royal Society
of chemistry publications.
6. Shah DH. SOP Guidelines. Business Horizons, New Delhi, 2004.
7. Mehra ML. Good manufacturing practices (GMP), University Book Agency.
8. Maitra K, Ghosh SK. A Guide to total quality management.
9. Snyder,Kirkland & Glajch, Practical HPLC Method development,2nd ed, 1997,Wiley
Interscience,New York.
QUALITY ASSURANCE AND MANAGEMENT
M PAQ. T.1.204
Sessional: 30
Examination: 70
Period/week: 4
Duration of Exam: 3 hrs
Nature of Exam: Theory
UNIT – I
Basic Concepts of Quality Assurance: concept of quality control & quality assurance,
functions, sources of variation, quality assurance for raw materials, APIs, packing materials
& finished products (specifications, receipt, testing, sampling and certificate of analysis),
production (change control, aseptic process control, temperature, pressure & humidity control
tests, tests for air flow pattern, microbiological monitoring) buildings & facilities (design and
construction features, construction materials, lighting, air handling systems, sanitation &
maintenance) equipments (construction, cleaning and maintenance, calibration & handling).
UNIT – II
Good Laboratory Practices: Scope, organization, personnel – desirable qualities of analyst,
responsibilities of key personnel in the QC lab. Facilities, equipments, testing facilities
operation – systems and procedures in QC lab, analytical worksheet, test methods, evaluation
of test results. Test and control articles – incoming samples, retention samples, reference
materials, reagents, specification reportory. Safety guidelines in QC lab
UNIT – III
Equipment qualification: (DQ, IQ, OQ &PQ)
Audits: GMP compliance audit, Definition Summary, Audit policy, Internal and External
Audits, Second Party Audits, External third party audits
Standard operating procedures: operations like cleaning, filling, drying, compression,
coating, disinfection, sterilization, membrane filtration etc.
UNIT – IV
Statistical Quality Control: Scope, sampling – importance, sampling plans, sample size,
statistical consideration - probability, frequency distribution. Sampling procedures,handling,
labeling & preservation. Analysis of data, Control charts – X charts, R charts, applications.
NABL certification and accreditation procedure
UNIT – V
Environment Health and Safety (EHS): Hazards- Fire, mechanical, chemical and
pharmaceutical, monitoring and prevention systems, industrial effluents testing and treatment,
control of environmental pollution.
Recommended books:
1. Gupta SC. Fundamentals of statistics. 6th ed., Himalaya publishing house, Hyderabad,
2004.
2. Sharma PP. How to practice GMPs, 4th ed., Vandhana publications Pvt. Ltd., Delhi,
2004.
3. Sharma PP. How to practice GLP, Vandhana publications, Delhi, 2000.
4. Quality assurance of pharmaceutical (A compendium of guidelines and selected
materials) Vol. I & II, WHO, Geneva, Pharma book syndicate, Hyderabad, 2002.
5. Basic tests for pharmaceutical substances, WHO, Geneva, All India traveler book
seller, India, 1990.
6. The International Pharmacopoeia, Vol. I-II, 3rd ed., WHO, Geneva, 1981.
7. Mehra ML. Good manufacturing practices (GMP), University Book Agency.
8. Subrahmanyam.CVS, Pharmaceutical Production and Management, 2005, Vallabh
Prakashan, NewDelhi.
9. Statistical design and analysis in pharmaceutical sciences, Marcel Dekker, NY.
10. Statistical Methodology in Pharmaceutical Science, D.A. Berry, Marcel Dekker, NY.
11. Quality assurance Manual, DH Shah, Business horizons, New Delhi.
12. Quality assurance and quality management in pharmaceutical industry, Y.
Anjaneyulu, R. Marayya. Pharma book Syndicate, Hyderabad
Research Methodology
Unit-I:
Developing a research question, Resources for research question,
Literature Review: Traditional Qualitative Review
Meta-Analysis—A Quantitative Review
Preparation of Research Proposal
Unit-II:
Non-experimental Research:
Part 1—Observational, Archival and Case-Study Research: The Hermeneutic Approach.
Observational Research: Naturalistic Observation, Participant-Observer Research.
Archival Research: Archival Data Collection and Compilation.
Case Studies: Characteristic of Case Studies.
Non-experimental Research: Survey Research—Designing of Questionnaire, Methods of
Administration, Response Rates. Types of Samples—Haphazard Samples, Purposive
Samples, Convenience Samples and Probability Samples.
Unit III:
Single-Subject Experiments: Advantages and Disadvantages.
Quasi Experiments: The differences between Quasi and True Experiments.
Design without Control Groups—Interrupted Time Series Designs and Repeated Treatment
Designs.
Unit IV:
Small scale industries, creativity, innovation, entrepreneurship