m.pharm analysis, pharmaceutical analysis, food analysis, cosmetic analysis and evaluation, modern bio analytical techniques, advanced pharmaceutical analysis, phamaceutical validation

1. SUBJECT: PHARMACEUTICAL VALIDATION
KARNATAKA COLLEGE OF PHARMACY
TOPIC:QULIFICATION OF GAS CHROMATOGARPHY
SUBMITTED BY: SUBMITTED TO:
ABHISHEK DR. C. SREEDHAR
M. PHARM 1ST SEMESTER PROF. AND HOD
DEPT. OF PHARMACEUTICAL ANALYSIS DEPT. OF PHARMACEUTICAL ANALYSIS
KARNATAKA COLLEGE OF PHARMACY KARNATAKA COLLEGE OF PHARMCY
BANGALURU BANGALURU
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2. Contents
• INTRODUCTION
• Principle of HPTLC
• Qualification of HPTLC
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3. VALIDATION
 Validation is a documented act of proving that any procedure, process or
system actually leads to expected result.
QUALIFICATION
 Qualification of analytical instruments is the process of ensuring that the
instrument meets the specified requirements and performs reliably and
accurately for its intended use. :
Design Qualification (DQ) : is the documented verification that the proposed
design of the facilities, systems and equipment is suitable for the intended
purpose.
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4. Installation Qualification (IQ): This step verifies that the instrument is properly
installed, including verifying that all components are present .
Operational Qualification (OQ): This step verifies that the instrument is operating
within its specified parameters, including testing the accuracy and precision of the
measurements.
Performance Qualification(PQ): This step verifies that the instrument consistently
performs within its specified parameters over time.
Maintenance Qualification : The instrument must be maintained to ensure that it
continues to operate within its specified parameters.
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5. GAS CHROMATOGRAPHY
 It is a process of separating compounds in a mixture by injecting a gaseous or liquid
sample into a mobile phase, typically called the carrier gas, and passing the gas
through a stationary phase.
 There are two types:-
1. GSC
2. GLC
Principle: The sample solution injected into the instrument enters a gas stream which
transports the sample into a separation tube known as the column. The various
components are separated inside the column.
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6. INSTRUMENTATION OF GAS CHROMATOGRAPHY
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7. QUALIFICATION OF GAS CHROMATOGRAPHY
A. Design Qualification
• Supplier must provide documented evidence that the product has been
designed, developed and manufactured in a quality environment.
• Supplier must provide on-site support in case of defects.
• Supplier must provide information through the internet on availability of
new firmware upgrades.
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8. B. Installation Qualification
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Check
Check documentation for completeness (operating manuals, maintenance
instruction, standard operating procedure for testing, safety and validation
certificate).
Compare
Compare equipment as received, with purchase order (including software,
accessories, spare parts).
Allow
Allow sufficient shelf space for the equipment, SOPs, operating
manual and software.
Check
Check the site for the fulfilment of the manufacturer's recommendation (utilities
such as electricity and environment condition such as humidity and temperature)
Obtain Obtain manufacturers recommendations for installation site requirements.

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Prepare Prepare an installation report.
Run
Run test sample and compare chromatogram print out with reference
chromatogram.
Identify
Identify and a make a list with a description of all hardware, include drawings
where necessary.
Switch on
Switch on the instrument and ensure that all modules power up and perform an
electronic self test.
Install
Install hardware( computer, equipment, fittings and tubing's, for fluid connection,
column in HPLC, power cables, data flow and instrument control table).
Check Check equipment for any damage

10. C. Operational Qualification
Precision of peak retention times
Precision of peak areas
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11. Accuracy of the temperature of the column oven
precision of heating zone temperature
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12. Carryover of Injection
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13. D. Performance Qualification
INJECTOR LEAK TEST:-
 Disconnect the column from the injector and close the injector outlet with
a sealed cap.
 Close the septum purge and the bypass.
 Adjust the flow and pressure controller to the maximal possible value of
the pressure gauge.
 Adjust the flow controller to zero.
 Read the pressure after 1 minute and record the value.
 Record the pressure after 5 minutes.
Limits:-
 Pressure drop < 15 kPa within 5 minutes.
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14. INLET PRESSURE/FLOW RATE ACCURACY:-
• The digital flow meter is connected to the detector outlet port.
• The carrier gas flow is set and wait till it reaches the set flow.
• The observed flow in replicate is noted.
• The procedure is repeated for other carrier gases such as hydrogen
or helium air.
• The flow rate of carrier gas should be 10% of set flow.
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15. System precision:-
• 20ml of methanol, ethanol and acetone is transferred into
100mlvolumetric flask and made up with ethyl acetate.
• Blank is injected followed by standard preparation in six replicates.
• The areas and retention times are noted down.
• The %RSD (Relative standard deviation) of retention time should not
be more than 1.0% and peak area not more than 5.0%.
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16. Detector noise and Drift test
• After GC is ready, the system is run up to 15 minutes through single
run.
• When the run is completed noise and drift is calculated through
software.
• The acceptance values are:
a) Noise not more than 100uV.
b) Drift not more than 2500uV/hr.
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17. REFERENCE
1. Textbook of pharmaceutical analysis 4th edition Dr. Ravi Shankar
2. Google source https://pharmaguidesline.com/performance-
qualification-document-of-gc-with-head-space-on-chromeleon-
software/
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18. THANK YOU
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