1.0 OBJECTIVE
To provide a general guideline for the system suitability test for chromatographic (High Performance Liquid Chromatography & Gas Chromatography) & Spectroscopic (UV) analysis.
2.0 SCOPE
This SOP is applicable to tests like Assay, Related substances, Content Uniformity, Dissolution, Deposition (for MDI & DPI), Particle size distribution (for MDI) and Residual solvents. The System Suitability Tests are to be carried out to verify that the chromatographic / spectroscopic system is adequate for the intended analysis.
3.0 RESPONSIBILITY
3.1 QC Officer/analyst shall be responsible to follow the procedure during HPLC and GC analysis.
3.2 Overall responsibility for training, implementation & follow-up shall be with the QC Manager or His/Her Nominee.
4.0 ACCOUNTABILITY
4.1 Head of Quality.
5.0 PRECAUTIONS
5.1 System suitability must be checked during performing analysis by chromatographic & spectroscopic techniques.
5.2 Do not proceed with the sample analysis until the system suitability requirements are met.
6.0 PROCEDURE
6.1 Each chromatographic & spectroscopic method must have appropriately set system suitability criteria to evident the suitability of the analytical method as well as the equipment.
6.2 For a chromatographic procedure, at least one of the following or a combination of more than one parameters are to be set as system suitability criteria in the STP:
• % RSD of repeated injections (3 – 6 injections as described in the respective procedure).
• Reproducibility of standard solutions (between two different preparations of the standard solution).
• Theoretical plates.
• Tailing Factor (Asymmetry).
• Resolution between peaks.
• Peak-to-valley ratio.
• Signal to noise ratio.
For spectroscopic procedure, % RSD of repeated measurements is usually set as the system suitability requirement.
6.3 The acceptance limit of the above system suitability parameters are to be set as per general or individual pharmacopoeial monograph (as applicable) or as per method validation output. Also it can be set as per supplier’s method.
6.4 The sequence of testing system suitability, standards and samples shall be done as per the respective test procedure.
6.5 Perform the required system suitability test (s) before proceeding with the analysis of the sample (s) and at the end of the analysis (bracketing) as described in the respective testing procedures.
6.6 The criteria of all the system suitability parameters must meet prior to proceeding with the sample analysis and also in a defined interval (i.e every after 14th injections etc.) and at the end (bracketing) of the analysis (if applicable).
6.7 After completion of an analysis, attach all the chromatograms & respective data of system suitability with the batch record.
6.8 In case there is a system suitability failure at the start of an analysis, the analysis has to be stopped immediately and the root cause of the failure has to be identified.
6.9 The incidence to be recorded as Incidence on SST Failure (Annexure-I) and appropriate corrective actions to be taken. The analysis shall be continued if the system suitability criteria met after implementing the corrective actions.
6.10 The initially prepared standard solutions shall be used as bracketing standard but shall be injected from separate intact vials than the initially injected vials.
6.11 When solution stability is not adequate for prepared standard solution as per the individual test procedure to check the bracketing SST, then prepare fresh standard solution for bracketing SST. In this case reproducibility is to be checked instead of %RSD.The acceptance criteria for reproducibility is NMT 2%.
6.12 If any measured bracketing SST is not meeting the acceptance criteria, raise an incidence on SST Failure and determine the status of result based on the disposition comments made by supervisor or Head of QC.
6.13 Data obtained even though the chromatography system suitability requirements are not met shall not be released without retesting using chromatographic systems that meet the STP’s SST requirements regardless of the intended market for the product.
6.14 Data obtained prior to the last successful check or bracketing standard shall only be accepted , and retesting the solutions obtained after the last successful check standard or bracketing standard to be done with properly justified and documented.