SOP Title: Working Standard Preparation
- Objective:
To lay down the procedure for Working Standard Preparation.
- Scope:
This SOP is applicable for Working Standard Preparation in Quality Control Department.
- Responsibility:
- Quality Control Department: To prepare and review the SOP. To follow the procedures laid down for Working Standard Preparation in Quality Control Department as per this SOP.
- Quality Assurance Department: To review and approve the SOP and Annexures.
Accountability:
Head Quality Control Department, Head Quality Assurance Department.
- Procedure:
| 5.1 | Working Standard Preparation: | |
| 5.1.1 | Select the high purity material for Working Standard preparation. | |
| 5.1.2 | It should be indented from the raw material store or from API Manufacturer. | |
| 5.1.3 | Select a material of the latest passed batch having highest purity, lowest impurity. | |
| Note: In case of any manufacturer provides the working standard same shall be used and no further standardization required. | ||
| 5.1.4 | Give “Material Requisition for Working Standard Preparation” as per Annexure No. 01 to Warehouse Department. | |
| 5.1.5 | Take required quantity of material based on vial filling and analysis of working standard. | |
| 5.1.6 | In case of low dose materials take minimum required quantity of material based on vial filling and analysis of working standard. | |
| 5.1.7 | Supervisor/QC Head shall allocate the testing samples to the analysts as per their job responsibility and specialisation. | |
| 5.1.8 | Analyst should refer Standard Testing Procedure before initiating the testing. | |
| 5.1.9 | Analyst should give requisition for “Analytical Work Report” to the Quality Assurance Department as per the SOP “Control of Documents, Preparation, Approval, Issuance and Maintenance”. | |
| 5.1.10 | Analyst should refer Standard Testing Procedure to ensure that all required Reagents, Chemicals, Accessories, Equipment or Instruments are standardised or validated and available in the Laboratory. | |
| 5.1.11 | In case of non-availability of Chemicals, Impurities, Working Standard, Instruments or Equipment’s in the Laboratory for any specified test then the sample to be send to Government Approved Outside Testing Laboratory, by filling “Requisition for Analysis” form as per SOP “Approval of Outside Testing Laboratory and Analysis of Samples at Outside Testing Laboratory” with relevant necessary information. | |
| 5.1.12 | While preparation of working standard refer the Current reference standard lot number | |
| 5.1.13 | Analyst should fill in the necessary details on the Analytical Work Report and start the analysis as per Standard Testing Procedure and Specifications. | |
| 5.1.14 | If working standard qualified within the 3 months of original passed batch testing then, only critical test shall be performed again as mentioned below: | |
| 5.1.15 | Description: One time sufficient
Loss on drying / Water : Single preparation separately by two analyst Assay Test: Single preparation separately by two analyst (In-house Testing) Should be in single (External Testing) |
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| 5.1.16 | If working standard qualified after 3 months then perform full testing as per STP and qualify for the working standard. | |
| 5.1.17 | All the test and parameters should be followed as per Raw Material Specifications using Reference Standards or previously standardized Working Standard. | |
| 5.1.18 | In case of IR and UV Testing, Spectrum obtained shall be compared against the spectrum obtained by the reference standard. Analyze the material for Identification and related impurities (wherever applicable). | |
| 5.1.19 | LOD/Water value should not be vary more than 0.5 between two analysts. | |
| 5.1.20 | Assay value should not be vary more than 1.0 % between two analysts. | |
| 5.1.21 | If material tested from outside lab, perform all tests only single time. | |
| 5.1.22 | After completion of analysis, assign the Working Standard Number and prepare the “Certificate of Analysis (Working Standard)” as per SOP with details including Reference Standard Number used to prepare Working Standard.
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| 5.1.23 | Use the mean value of replicate results during data presentation on “Certificate of Analysis (Working Standard)”. Assign the validity of Working Standard up to one year from the date of approval or Expiry given by manufacturer, whichever is earlier. | |
| 5.1.24 | After the analysis, analyst should hand over the Analytical Work Report to Supervisor/Reviewer analyst for data checking. | |
| 5.1.25 | If Supervisor/Reviewer observed any discrepancy with analysis or analytical data, he / she should consult to Head of the Department for investigation by filling incident or OOS as per SOP “Out of Specification” depending on discrepancies. | |
| 5.1.26 | If all the relevant data on Analytical Work Report complies as per Pharmacopoeia or IHS requirement or both, Supervisor/Analyst should prepare “Certificate of Analysis (Working Standard)”as per specified format. | |
| 5.1.27 | In case of any raw material having two pharmacopoeia grades material shall be standardized for both the pharmacopoeias procedures and both pharmacopoeias potency shall be mentioned on the label. | |
| 5.1.28 | Quality Control Head shall verify and approve the COA. | |
| 5.1.29 | Pharmacopoeia grade Reference Standards or Impurity Standards shall be procured from Authorised Agency. | |
| 5.1.30 | Assign Working Standard Number as follows:
If the Working Standard prepared as per IP, number should be given as: WS/IP/XXX/YY/NN. If the Working Standard prepared as per BP, number should be given as: WS/BP/XXX/YY/NN. If the Working Standard prepared as per USP, number should be given as WS/USP/XXX/YY/NN. where:- WS: Working Standard IP: Indian Pharmacopoeia BP: British Pharmacopoeia USP: United State Pharmacopoeia XXX : Material Code YY: Last two digits of the current year NN: Serial number of that particular Working Standard |
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| 5.1.31 | Prepare the 13 vials of the Working Standards in same quantity. | |
| 5.1.32 | Keep 12 vial for one year i.e. each vial per month and keep One vial as a Reserve Working Standard. | |
| 5.1.33 | In case of low dose materials prepare Five vials of the Working Standards in same quantity. Keep 4 vial for one year i.e. every 3 month one vial and keep One vial as a Reserve Working Standard. | |
| 5.1.34 | Store the Working Standards in Refrigerator at 2°C to 8°C or as per respective material storage condition in glass vials with butyl rubber plugs and tightly closed with aluminium seal. | |
| 5.1.35 | For light sensitive material use amber coloured glass vials. | |
| 5.1.36 | Label the vials with detailed information and vial number also as 1/ 13, 2 /13 and so on. | |
| 5.1.37 | Issue the first vial for first months and next for coming months as per serial number. Opened vial is valid for one month from the date of opening. | |
| 5.1.38 | Discard the each opened vial after use or within 3 days of respective month end.
Example: If an Paracetamol (API) working standard vial no.1 is opened on 15/05/2023, then it should be discard within 3 days i.e. from 14/06/2023 to 16/06/2023. |
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| 5.1.39 | Allow the Working Standard to equilibrate to room temperature in the original container before it is weighed for a test. | |
| 5.1.40 | Care should be taken to minimise the exposure of Working Standards to atmospheric condition for longer time. After use, immediately close the vial with cap and keep it as per respective storage condition. Update ‘Working Standard Usage Log Book’’. | |
| 5.1.41 | Dispensing equipment such as Spatula, butter paper etc. should not be inserted into the Working Standards vials as this may contaminate the material. | |
| 5.1.42 | Material taken out for weighing that is in excess should not be transferred back to the vial. | |
| 5.1.43 | All unused vials shall be destroyed at end of one year. | |
| 5.1.44 | In-case, for any reason new material is not available in stock to prepare new working standard, then unused working standard vials shall be retested as per working standard qualification criteria and shall be used for next one year provided that it should be within the expiry period assigned by manufacturer.
Example: If the Paracetamol (API) working standard vial retested on 10/05/2023 and Manufacturer expiry period of Paracetamol is 04/2024 then it cannot be used beyond 30/04/2024. |
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| 5.1.45 | For destruction of any Working Standards, refer current SOP of “Destruction of Laboratory Waste”. | |
- Definitions / Abbreviations:
- Definitions :
- Abbreviations :
| Abbreviation | Expansion |
| SOP | Standard Operating Procedure |
| QC | Quality Control |
| QA | Quality Assurance |
| AR | Analytical Reagent |
| No. | Number |
| RSD | Relative Standard Deviation |
| % | Percentage |
*Note – Ready to use SOP available in “DOWNLOAD” Section.