SOP for Chromatographic Analysis and Documentation

To lay down the procedure to be followed in HPLC & GC analysis and documentation.

This SOP is applicable for the procedure to be followed for assay, dissolution, uniformity of dosage units and related substances/impurity by HPLC and for assay & residual solvents by GC.

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.

4.1 Head of Quality.

5.1 Make sure the audit trail is always on.
5.2 Use parafilm to close the mobile phase bottles.

6.1 Mobile phase
6.1.1 The mobile phase shall be prepared as per the composition describe in the Standard Test Procedure.
6.1.2 The mobile phase shall not be used after 48 hours of its date of preparation.
6.1.3 The mobile phase shall be discarded if any haziness or precipitation is found upon visual examination.
6.1.4 Mobile phase container shall be labeled with FQC/104.

6.2 Resolution Solution/System Suitability Solution
6.2.1 For quantitative analysis resolution solution/system suitability solution shall be prepared freshly.
6.2.2 For qualitative analysis, prepared resolution solution/system suitability solution can be used within 6 months of its date of preparation.

6.3 Standard Preparation
6.3.1 The standard solution shall be prepared as per the STP, taking in consideration them stability and storage requirement.

6.4 Analysis
6.4.1 Test sample trial injection shall be prohibited. Only blank, resolution solution or system suitability standard solution can be used for trial injection.
6.4.2 Trial injection shall be in separate sample set and to be processed and documented.
6.4.3 Analyst shall check previous chromatographic data if necessary.
6.4.4 The system suitability shall be established as per the STP, before proceeding with the analysis.
6.4.5 Injection sequence/sample set shall be captured from the system as per the STP of respective product/material and shall be recorded.
6.4.6 The system suitability shall be valid for a maximum period of 24 hours.
6.4.7 Process validation/method validation analysis must be in separate validation project since validation documents are for life time.

6.5 Acceptance Criteria
6.5.1 The stored resolution mixture if used, shall meet the system suitability criteria on all the day of its use. Otherwise a freshly prepared resolution solution shall be used.
6.5.2 During assay and related substance analysis involving isocratic runs. The flow rate of mobile phase shall be kept constant for the entire run, after the system suitability is established. If the flow rate of the system is changed fresh system suitability shall be established.
6.5.3 During assay and related substance analysis involving gradient run, if there is delay (exceeding the run time) in injection the next sample, the blank run with gradient operation shall be continued. The chromatogram for blank injection shall be recorded.
6.5.4 Manual integration can be done in case of related substance analysis.
6.5.5 The analyst will seek the permission of the lab in-charge / supervisor for manual integration.

6.6 Recording Chromatogram
6.6.1 All chromatogram before establishment of system suitability and up to entire run shall be recorded and documented.
6.6.2 In case where the chromatogram needs disregarding the analyst shall show it to the supervisor/reviewer for review and approval.
6.6.3 The disregarded chromatogram shall be checked by supervisor/reviewer.
6.6.4 The chromatogram, which is disregarded and not considered for calculation, shall be written as “DISREGRADED”. The reason for disregarding the chromatogram could be variation in the area count/ inconsistent area, faulty integration, abnormal drift in baseline, ghost peak or any other reason.
6.6.5 The analyst performing the analysis shall assign the reason of disregarding a chromatogram on the chromatogram itself. The disregarded chromatogram shall be filled along with the test chromatogram.
6.6.6 All electronic data must be reviewed by the supervisor/reviewer.
6.6.7 Reprocessing of chromatogram if necessary shall be documented with reason for reprocessing.
6.6.8 For the system generated chromatogram, the necessary information shall be printed on each chromatogram.
6.6.9 The integrating parameter such as peak width, peak threshold, minimum peak area and height shall be recorded, as used for integration of chromatogram.
6.6.10 Instrument method and processing method shall be documented.
6.6.11 Audit trial report shall be reviewed by Sr.Officer/supervisor and documented

6.7 Calculation
6.7.1 The calculation shall be performed as per respective STP using Empower-3 software, Lab Solution software or Excel spread sheet. In case where Empower-3 or Lab Solution software will be used for calculation then an established multiplication factor or appropriate dilution shall be used.

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