Qualification of Gas Chromatography
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The document presents a seminar on the qualification of gas chromatography as part of the M.Pharm curriculum at Raghavendra Institute of Pharmaceutical Education and Research. It outlines the four stages of qualification: design qualification, installation qualification, operational qualification, and performance qualification, emphasizing the importance of validation in ensuring equipment reliability. Additionally, it provides detailed procedures and acceptance criteria for various qualification tests related to gas chromatography.
Qualification of Gas Chromatography
- 1. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 1 A Seminar as a part of curricular requirement for I year M.Pharm II Semester Presented by Ms. T.Jayasree (Reg.No 20L81S0709) Pharmaceutical Analysis QUALIFICATION OF GAS CHROMATOGRAPHY
- 2. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 2 Qualification Gas Chromatography (GC) Design Qualification (DQ) Installation Qualification (IQ) Operational Qualification (OQ) Performance Qualification (PQ) References Contents
- 3. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 3 • Qualification- It is defined as the “action of proving that any equipment works correctly and leads to the expected results”. Qualification is also part of validation and is product specific. • Qualification is often a part (the intial stage) of validation ,but the individual qualification steps alone do not constitute process validation. Qualification
- 4. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 4 • There are four stages of qualification 1) Design Qualification (DQ) 2) Installation Qualification (IQ) 3) Operational Qualification (OQ) 4) Performance Qualification (PQ)
- 5. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 5 • validation and qualification are essentially components of the same concept. • The term qualification is normally used for equipment , utilities and systems. • Validation is used for processes. • In this sense, qualification is part of validation. Relationship between validation and qualification
- 6. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 6 GAS CHROMATOGRAPHY (GC)
- 7. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 7 • Supplier must provide documented evidence that the product has been designed, developed and manufactured in a quality environment e.g. ISO 9001:2000 certification. • Supplier must provide phone and on-site support in case of defects. • Supplier must provide information through the internet on availability of new firmware upgrades. Design Qualification
- 8. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 8 • Equipment is compared as received with purchase order, including software, accessories, spare parts and consumables. • Documentation checked for completeness of operating, maintenance instructions, standard operating procedures for testing and safety, validation certificates and health and safety instruments. • Equipment is checked for any damage. • The supplier’s instruction for installation is read. Installation Qualification
- 9. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 9 • The supplier’s safety instructions are read, if there are any. • Hardware (computer, equipment, fittings and tubings for fluid connections, power cable, data flow and instrument control cables) is installed following the manufacturer’s recommendation. • The instruments are switched on and ensured that all modules power up and an electronic self test is performed. • Any deviations are recorded.
- 10. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 10 • Software is installed on computer following the manufacturer’s recommendation. • Correct software installation is verified. • A backup copy of software is made.
- 11. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 11 Precision of peak retention times Precision of peak areas Operational Qualification Test procedure Acceptance limits Test frequency Five injections of a standard. Calculation of relative standard deviation. <1% RSD (Relative Standard Deviation) Yearly Test procedure Acceptance limits Test frequency Five injections of a standard. Calculation of relative standard deviation. <2% RSD Yearly
- 12. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 12 Test procedure Acceptance limits Test frequency Remarks Temperature in column oven is measured and compared with set point. ±1°C Yearly The temperature measurement device should be calibrated and traceable to a national standard. Accuracy of the temperature of the column oven
- 13. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 13 Precision of heated zone temperature Test procedure Acceptance Limits Test frequency Remarks Actual temperature is measured and compared with set points at 50,70 and 90°C. 2°C Yearly The temperature measurement device should be calibrated and traceable to a national standard.
- 14. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 14 Precision of injection Test procedure Acceptance limits Test frequency Five injections of a standard. Calculation of relative Standard deviation. <2% RSD Yearly
- 15. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 15 Test procedure Acceptance limits Test frequency Blank solvent is injected after standard. Peak ratio is measured between blank and standard injection. <5% Yearly Carryover of Injection
- 16. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 16 Solution A 10 ml of methanol, ethanol, acetone make upto 100ml with ethyl acetate. Solution B 15ml of methanol, ethanol, acetone make upto 100ml with ethyl acetate. Solution C 20 ml of methanol, ethanol, acetone make upto 100ml with ethyl acetate. Solution D 25 ml of methanol, ethanol, acetone make upto 100ml with ethyl acetate. Solution E 30 ml of methanol, ethanol, acetone make upto 100ml with ethyl acetate. Performance Qualification Detector Linearity Detector linearity solutions:
- 17. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 17 Procedure Acceptance Criteria Blank is injected followed by detector linearity solutions and the peak responses are recorded. A standard plot is drawn between the concentrations vs the peak responses. The plot should be linear and regression coefficient (R2) should not be less than 0.9999.
- 18. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 18 • 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 and air. • The flow rate of carrier gas should be ±10% of set flow. Flow rate accuracy
- 19. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 19 • 20ml of methanol, ethanol and acetone is transferred into 100ml volumetric 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%. System precision
- 20. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 20 • 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 100µV. b) Drift not more than 2500µV/hr. Detector noise and Drift test
- 21. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 21 1. D. Gowrisankar, K. Abbulu , O. Bala souri, K. Sujana, Validation and Calibration of Analytical instruments. 2010;2(2). 2. McDowall RD. Method validation in gas chromatography. Gas chromatographic techniques and applications, 2001:201-2. 3. USP 30 NF 25 “The official compendia of standards”, Asian edition, 2007, vol: 1. References
- 22. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 22 4. Chan CC, Lam H, Zhang XM. Practical approaches to method validation and essential instrument qualification. John Wiley & Sons; 2011 Mar 1. 5. A.H.Beckett, J.B.Stenlake, Practical Pharmaceutical chemistry, CBS Publishers and distributors, IV-Edition, part two, 2004, p.no.326. 6. Y.Anjaneyulu ,R.Marayya ,Quality Assurance and Quality Management in Pharmaceutical industry , Pharmabook Syndicate , 2005.
- 23. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 23