SOP for Recording of Analytical Data

1.0 OBJECTIVE

To lay down a procedure for recording analytical data.
2.0 SCOPE This SOP is applicable to record the analytical data in the raw data sheets.

3.0 RESPONSIBILITY

Officer / Executive - Quality Control

4.0 ACCOUNTABILITY

Manager - Quality Control

5.0 PROCEDURE

5.1 Ensure that all data related to analysis are recorded in Record of Analysis (Raw data sheet) and any attachments referenced therein.
5.1.1 Use following Raw data sheet for recording the analytical data.
a) In-process
b) Raw Materials Testing
c) Finished Product Testing
d) Stability Testing
e) Validation
5.1.2 Each Raw data sheet is a controlled document bearing serial no. on the counterfoil as well as on the raw data sheet identification number.
5.1.3 The pad will be issued for each type of analysis by the analyst and a record of issuance shall be maintained in issuance register.
5.1.4 Prior to the start of any analysis the QC Supervisor/officer shall verify the required number of raw data sheets.
5.1.5 Sample withdrawn date (from the respective condition) shall be recorded on the raw data sheet and all analytical observations/data shall be recorded online while performing the analysis (like Description, Water by KF & foreign particle etc)
5.1.6 Product Names shall be written in full (Generic/Trade/Brand) against Product. Correct abbreviations (Alphabets/Alphanumerical) shall be mentioned in brackets only.
5.1.7 Columns of Batch no, Date of Mfg., Date of Exp. shall be written as per the product pack and Protocol.
5.1.8 Other details like strength/ Specification number, market shall be written as per sample request/ Protocol and Specification (as applicable).
5.1.9 Description: The actual product description shall be recorded using the text as per the Protocol Specification in case of exhibit batches and Product Release Specification in case of the commercial batch.
5.1.10 The average fill weight/ average fill volume shall be recorded at the time of analysis. In another case ‘NA’ (Not applicable) shall be written where there is no requirement of average fill weight and average fill volume.
5.1.11 Water by KF: Results shall be recorded as per the Printout. The rounding off shall be done as per specification/ protocol.
5.1.12 Loss on Drying (LOD): Recording shall be done after filling the relevant information. The rounding off shall be done according to specification.
5.1.13 pH shall be measured and recorded from digital pH meter without rounding off. Prior to this, the instrument shall be calibrated. The observation of calibration shall also be recorded.
5.1.14 Fill Volume / Fill weight shall be recorded in units as per the Protocol /Product Release Specification as applicable.
5.1.15 Foreign particle shall be recorded after filling the relevant entries. The result should be recorded.
5.1.16 Particulate Matter Shall be recorded after filling the relevant entries.
5.1.17 Viscosity shall be recorded & calculated after making relevant entries.
5.1.18 Endotoxin test results shall be recorded in the respective raw data sheet.
5.1.19 Sterility test record shall be recorded in the respective raw data sheet.

5.2 Assay

5.2.1 All relevant entries regarding instrument number shall be recorded along with Working Standard, Batch No., and Potency. The correct potency shall be filled.
5.2.2 Mobile Phase preparation shall be written recording the actual weight of salt and volume of solvents used. The actual pH of mobile phase shall be recorded. Prior to this pH meter calibration shall also be recorded.
5.2.3 The preparation of diluent shall be recorded. In case the STP mentions the use of solvents other than diluent, it shall be recorded.
5.2.4 All weight of Resolution Solution, Internal Standard, Working Standard and Test Preparation shall be recorded in the table only. The recording of weights shall be done along with entries of relevant factors like Batch Number, Strength. In the case where the STP mentions the intact liquid injection/ Dry powder injection to be taken for assay, the weight of pooled (number as per STP) shall be recorded in the table only.
5.2.5 Average Peak Area of Working Standard and Test (for which sheet) is issued shall be recorded ditto from the chromatogram. The RSD of Working Standard Peak Area shall be recorded from the chromatogram up to 1 decimal place. Rounding of peak area shall not be done.
5.2.6 Calculation of assay shall be according to the STP. The result shall be recorded up to 2nd decimal place without rounding off. The rounding off shall be done according to Specification, Release Specification, Regulatory Specification as the case may be.
5.2.7 In case of STP mentions to calculate the area ratio between 2 peaks then, the peak area ratio up to the 4th decimal place for each injection (without rounding off) shall be calculated.
5.2.8 Then the average peak ratio shall be calculated rounding off to 4 decimals.
5.2.9 Reference for weight slip, UV printout or chromatogram shall be mentioned as per the Product, Batch No. Sheet number shall not be mentioned. Product abbreviation can be used.
5.2.10 The reference of Mobile Phase Preparation / Diluent Preparation, Working Standard potency and Batch No shall be mentioned on all sheets. 5.2.11 Only validated calculation sheet shall be used and the same shall be attached to each and every sheet.

5.3 Sterility test

5.3.1 Details of the sample shall be mentioned on Raw data sheet of sample i.e. Product Name, B. No. , sampling date. Analysis date, Date of completion. Media details. Detail of Autoclave load must be given on raw data sheet.
5.3.2 Growth of microbial culture /Sterility test will be observed and recorded, every day.
5.3.3 Each observation has to be recorded in the raw data sheet.
5.3.4 Result of stasis test shall be recorded in the raw data sheet.
5.3.5 Environmental monitoring data shall be recorded in the raw data sheet.

5.4 Endotoxin test

5.4.1 Raw data of endotoxin test shall be recorded.
5.4.2 Lot No of LAL Reagent/ control endotoxin standard shall be recorded.
5.4.3 Product name, B.No. shall be recorded.
5.4.4 Refer SOP for documentation of supporting analytical documents, recording results of review documents in the Raw data sheet.
5.4.5 Continuation Raw data bearing a different control No. of a different serial no. shall be used to record data in case space is not available to capture data on Green Sheet. Attach the continuation sheet along with original sheet wherever possible giving a link of original Green Sheet No. in the continuation sheet.
5.4.6 If the data is to be kept as a separate bunch in the continuation sheet, cross-reference to the sheets shall be given to show tractability of data recorded.
5.4.7 All raw data sheet should be reviewed after completion of analysis and shall bear reviewers signature and date on the bottom of each raw data sheet and continuation sheet.
5.4.8 All supporting documents which are raw data such as chromatograms, spreadsheets, printouts from PLC controlled instruments shall be attached and referenced appropriately in Green Sheet.

6.0 ABBREVIATIONS

6.1 SOP - Standard Operating Procedure
6.2 No. - Number
6.3 QA - Quality Assurance
6.4 QC - Quality Control
6.5 LAL - Limulus Amebocyte Lysate
6.6 PLC - Program Logic Controller

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