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How to practice Pharmaceutical Analysis
course in Practice School model?

Jsk nagarajan
nagasaki2001@rediffmail.com

JSK NAGARAJAN
nagasaki2001@rediffmail.com
 PRACTICE SCHOOL - ANALYSIS
Gurukul system:Rich tradition -Europe, Middle East &
Portugal came to India -Quality education.

Residential schooling system - 5000 BC in

Indian subcontinent.
MODERN EDUCATION
Brought to India - 1835 by Lord Macauley
Rat race to be ahead of others. Total absence of
personality development, creation of moral conscience
and ethical training. Inte
Pliny teacher-developing speaking skills. Make
Roberto Nevilis (Italian pedagogi) invented-19
PUNISHING PURPOSE
 OSCE
Two types of clinical examination: cases and bell ringers.
case examinations: (LONG & SHORT)
• Candidate assigned a patient in clinical setting that
involved varying levels of simulations
• Given time to take patient’s history & physical examination
• Examiners ASKED ABOUT CASE TO THE candidate afterward
• Candidate was not observed in the patient interaction
• Entirely inconsistent examination experience
Bell-ringer examinations,
Candidates rotate from station to station – bones/specimens
under a microscope within a set amount of time.
OSCE - originally proposed in 1979 by Professor Ronald
Harden of the University of Dundee, Scotland
1995 - clinical assessment clearly moving away from written
examination formats.
 OSCE
Objective: Content & Scoring procedures are standardized.
Each station - designed to focus - area of clinical competence.
Standardized scoring tool is used to record what you do or do not do
well.

Structured: Every candidate experiences same problem, and asked to

perform same task, within same timeframe.
Exposed to same level of difficulty, & marked-same marking
scheme..

Clinical
Each OSCE station represent real-life clinical situations.
Assess ability to apply clinical knowledge & skills when, meeting with
a patient, writing an admission or discharge order, conferring with a
colleague, etc..

Examination
Enables a reliable assessment of a candidate’s competence.
Suitable for use in high-stakes assessments.
now used widely in UG, PG & licensing assessments..
EDUCATION : RECENT YEARS IN INDIA
 INDUSTRIAL TRAINING?

3 months (750 hours) in Pharma Company.

PASSION IN WORKING WITH
 PRACTICE SCHOOL – WHY & WHAT
“Learn By Practice“
“David H. Koch School of Chemical Engineering Pr
Anomaly at Massachusetts Institute of Technology
1915, Prof. William Walker’s desire to develop industrial chemistry as unique
School fulfillsdiscipline,
& necessary the visioncombined
of Institute’s
withfounder
alumnus inDr.
its emphasis on bringing
Arthur D. Little’s vision
scientific principles, & young people trained - to make useful goods.
for a practical component to univ. education in chemistry, resulted in the
School of Chemical Engineering Practice.

Concept was articulated in a report by the Visiting Committee to the Dept. of

Chemistry & Chemical Engineering, vigorously promoted by MIT President
Richard Maclaurin, and launched in 1916 with $300,000 in start-up funding
donated by George Eastman of Eastman Kodak Company. Professor Walker
was made Director of the School.

1917 Five stations established in the northeast US, covering industrial

operations in cement, dyes, abrasives, fuels, and paper.
1918 First year Resounding success & touted “an educational advance of the
first order” by Professor Walker. Program was suspended due to war.
1920 Reopened the Boston & Bangor Stations
1921 Opened - Buffalo Station.
1925 Enrollment soars after WW-1 with extraordinary development of
chemical industry. 3 stations in the northeast continue to thrive.

1943 WW-II causes suspension of School.

1950-80 Increasing costs, combined with the increased technical capabilities

resident in companies – and a new emphasis on “engineering science” in
university curricula – lead many to question the continuing relevance of the
Practice School.

1980-90 Alumni undertake fundraising to save PS & renamed in DAVID H.

KOCH.

1990s PS expands to international stations. A diversified suite of host

companies participate. Telecommunications and transportation allow projects
to be conducted at sites remote from the stations.
 Practice School (PS) - PHARMACY COUNCIL OF INDIA
PURPOSE OF PS
Shall undergo PS -150 hours throughout semester.
Shall opt any one-domains for PS as per program
committee.
Student shall submit report (in triplicate-25 pages) on
PS.
Evaluated by subject experts at college level.
Industrial training
Award: Grade (Desirable)
point shall be awarded.
Shall work for at least 150 hours (4 weeks) in Pharma Co./Hospital.
Production, QC, QA, R&D, Hospital Pharmacy, CRO, Community
Pharmacy, etc.
After the Semester – VI & before commencement of Semester – VII, &
shall submit satisfactory report of such work and certificate duly signed
by the authority of training organization to the head of the institute.

PREPARE THE PHARMACY

GRADUATES FOR THE PURPOSE
/USEFUL GOODS TO THE PHARMA
3 months (750 hours) in Pharma Company.
INDUSTRY
 CAREER OPPORTUNITIES IN PHARMA SECTOR
NO SKILLS - IT

MEDICAL CODING
MEDICAL BILLING
MEDICAL TRANSCRIPTION
MEDICAL WRITING
 PRACTICE SCHOOL
EARLIER 3 DEPT… NOW
• MFG • STORE
• QC
• MFG
• STORE
• QC
PHARMACEUTICAL CHEMISTRY • STORE
PHARMACEUTICS
• QA
PHARMACEUTICAL ANALYSIS
PHARMACOLOGY • RA
PHARMACEUTICAL BIOTECH • FR&D
PHARM. QA • AR&D
PHARM. RA
• Validation

STORE TO STORE
 PRACTICE SCHOOL - ANALYSIS

QMS ISO 9001:2015 • ISO – SAME

Scope
Normative References
Terms and Definitions
Context of the Organization
Leadership
Planning
Support
Operation
Performance Evaluation
Improvement

QUALITY IS NOT ACCIDENTAL ONE

 PRACTICE SCHOOL - ANALYSIS

QUALITY CONTROL & QUALITY ASSURANCE

DATA INTEGRITY
 PRACTICE SCHOOL - ANALYSIS

PREPARATION OF SOP
SOP
PREPARATION OF SOP
STRUCTURE OF SOP
INFORMATIONS AVAILABLE IN SOP
PREPARED BY WHOM
 PRACTICE SCHOOL - ANALYSIS

CLEANING – WHY SO IMPORTANT

CLEANING SOP
METHOD OF CLEANING
PREPARED BY WHOM
 PRACTICE SCHOOL - ANALYSIS

PREPARATION OF BUFFERS & STANDARD

SOLUTIONS

BUFFERS/ STANDARD SOLUTIONS

STORAGE CONDITIONS
LABELLING
DATE OF PREPARATION & EXPIRY
 PRACTICE SCHOOL - ANALYSIS

TESTING PROCEDURE -STP

 PRACTICE SCHOOL - ANALYSIS

TESTING PROCEDURE -STP

 PRACTICE SCHOOL - ANALYSIS
Calibration
Process by which ensure that an
instrument readings are accurate with
reference to established standards
Performed using primary reference
standards. Instruments need to be
calibrated before using.
Eg- Balance, pH meter, UV, IR, etc
Need for calibration
New instrument.
Specified time period is elapsed.
Specified usage (operating hours) has
elapsed.
Instrument has had a shock/vibration
which potentially may have put it out of
calibration.
sudden changes in weather. whenever
observations appear questionable.
Validation
.
Process of providing documented
evidence that something does what it
is intended to do Process, system,
method (performing without error)
Field of validation is divided into No. of
subsections as follows-
Cleaning, Process, Analytical method,
Computer system validation
Equipment validation - demonstrate that
equipment used in validation studies is suitable
for use & is comparable to equipment used for
routine analysis. Qualification Action of proving
and documenting that equipment or ancillary
systems are properly installed, work correctly,
& actually lead to the expected results.
Qualification is part of validation , but individual
qualification steps alone do not constitute
process validation
 UV-Vis SPECTROPHOTOMETER
PARAMETER
Wavelength accuracy:-
Defined as the deviation of the
wavelength reading at an
absorption band/emission band
from the WL of the band.
TEST
Checked by comparing recorded WL
of peak against the value of ref. std.
Commonly used WL standards such
as Deuterium, Hg vapor lamp,
Holmium oxide filter & Holmium
oxide solution (4% holmium oxide in
10% HClO4 in 1-cm cell)
RESULT
±1nm in UV range (200 - 380
nm) & ±3 nm in the visible
range (380 to 800nm). 3
repeated scans of same
peak should be within ±0.5
nm

3 test solutions prepared &

Stray light:- Stray light is
Defined as the detected light of
any wavelength that is outside
the bandwidth of WL selected.
measured the stray light @ 200,
220 &340 nm Acceptance:- The
transmittance of the solution in a 1
cm cell should be < 0.01 or
absorbance value should be >2.
At 1% transmittance, stray
light at 1% of the incident
light intensity can cause a
15% drop in absorbance

Resolution power:- Resolution of

a UV-VIS spectrophotometer is
related to its spectral band
width(SBW). Smaller the spectral
width-finer the resolution. SBW
depends on slit width &dispersive
power of monochromator
Linearity:- Linear dynamic range of
the measurement is limited by stray
light at high absorbance & by noise
at low absorbance. Accuracy of the
quantification of the sample
depends on the precision & linearity
of the measurements.
0.02%v/v toluene in hexane is
Ratio of the absorbance at
used to test resolution power of
269 nm & absorbance at
the spectrophotometer. The
266 nm should be grater
absorbance measured @ 269 &
than 1.5
266 nm.
Series of K2Cr2O7solution of conc.
20,40,60,80 & 100mg/L in 0.005M
H2SO4. Absorption of various WL Correlation coefficient r≥
are plotted against the concn of the 0.999
solution and the correlation
coefficients are calculated
 UV-Vis SPECTROPHOTOMETER
PARAMETER
Noise:- Noise in the measurement
affects accuracy at both ends of
absorbance scale. Photon noise
from the light source affects the
accuracy of the measurements
leads to low absorbance.
Baseline flatness:- Flat baseline
test demonstrates the ability of the
instrument to normalize light
intensity measurement & spectral
output at different wavelengths
through out the spectral range.
Stability:- Lamp intensity is a
function of the age of the lamp,
temp. fluctuation & WL of the
measurement. These changes
can lead to errors in the value of
the measurements, over an
extended period of time
Photometric accuracy:-
Determined by comparing the
difference between the measured
absorbance of the reference
materials & established value.
TEST RESULT
Air is scanned in absorbance
mode for 10 min. peak to noise
The RMS noise should be
is recorded @ 500nm.Root
less than 0.001 AU
mean square noise is then
calculated.
Air is scanned in absorbance
mode. The highest & lowest The deflection is typically
deflections in the absorbance unit less than 0.01AU
are recorded
Air is scanned in the absorbance
mode for 60 min at specific
The deflection is less than
wavelength(340nm).Highest &
0.002 AU/h
Lowest deflections in the
absorbance unit are recorded
6 replicate measurements
of 0.006%w/v K2Cr2O7
Either neutral density filters or
solution at 235, 257, 313 &
K2Cr2O7 solutions are used.
350 nm should be less
than 0.5% RSD
 PRACTICE SCHOOL - ANALYSIS
IR SPECTROPHOTOMETER
Calibration of IR spectrophotometer:
i)Wave number verification ii)Resolution performance

Wave number verification:-

The wave number scale may be verified using a polystyrene
film which has maxima at the wavenumbers (in cm–1 ):

3027.1(±0.3), 2924 (±2), 2850.7(±0.3), 1944 (±1),

1871.0(±0.3), 1801.6(±0.3), 1801.6(±0.3), 1583.1 (±0.3),
1181.4(±0.3), 1154.3(±0.3), 1069.1(±0.3), 1028.0 (±0.3),
906.7 (±0.3), 698.9 (±0.5).

Resolution performance:-
Record the spectrum of polystyrene film. Depth of the trough
between 2851 - 2870 cm–1 >6 % T for prism & <18 %T for grating instruments &
Between 1583 -1589 cm–1 >6 %T for prism & <12 %T for grating instruments.
PRACTICE SCHOOL - ANALYSIS

INTERPRETATION

RECALL OF RANITIDINE

RECALL OF 344 DRUGS

DRUG COMBINATIONS
VISIT/LIKE