SOP Title: Retesting of Raw Materials and Packing Materials
- Objective:
To lay down the procedure for Retesting of Raw Materials and Packing Materials in Quality Control Department.
- Scope:
This procedure is applicable for Retesting of previously approved Raw Materials and Packing Materials on the due date of Retest in Quality Control Department .
- Responsibility:
- Quality Control Department: To prepare and review the SOP. To follow the procedures laid down for Retesting of Raw Materials and Packing Materials in Quality Control Department as per this SOP.
- Quality Assurance Department: To review and approve the SOP and Annexures.
- Warehouse Department: To intimate Quality Control Department for Sampling of Retest Raw Materials and Packing Materials.
- Accountability:
Head Quality Control Department, Head Quality Assurance Department
- Procedure:
| 5.1 | Precautions: | |
| 5.1.1 | Sampling analyst should wear safety nose mask, gloves at the time of sampling. | |
| 5.1.2 | Do not enter the sampling room when UV light is “ON”. | |
| 5.1.3 | Sample only one container at a time in a sampling booth. | |
| 5.1.4 | Do not expose hygroscopic materials for longer time in air as it will absorb the moisture. Cover the samples with double polybag. | |
| 5.1.5 | Do not expose light sensitive materials for longer time to light as it will degrade the sample. Cover the samples with black polybag. | |
| 5.2 | Assigning of Retest Date for Raw Materials and Packing Materials: | |
| 5.2.1 | On release of Raw Materials and Packing Materials enter the Retest Date on the approved labels and on respective COA as follows: | |
| 5.2.2 | For Active Raw Materials, Retest Date shall be one year from the date of release. | |
| 5.2.3 | For Inactive Raw Materials, Retest Date shall be two years from the date of release. | |
| 5.2.4 | For Packing Materials, Retest Date shall be two years from the date of release. | |
| 5.2.5 | Example: If the PVC foil is released on 20/08/2022 then the Retest Date shall be 19/08/2024. | |
| 5.2.6 | While assigning retest date, check that the expiry date of material is not less than the retest date. | |
| 5.2.7 | If the expiry date of the material is less than the retest due date then the Retest Date shall be same as expiry date. | |
| 5.2.8 | Example: If the material is released on 25/07/2022, expiry date is 04/2024 then the Retest Date shall be 30/04/2024. | |
| 5.2.9 | If any Raw Material is not possible to analyse as per Retest Date due to some reasons then material shall be analysed and released prior to taking into manufacturing. | |
| 5.3 | Sampling Procedure for Raw Materials due for Retest: | |
| 5.3.1 | Warehouse Head should give “Retest Intimation Slip” as per SOP “Management of Warehouse” prior to 15 day of the Retest Date as per approved label or Raw Material Stock Register. | |
| 5.3.2 | Warehouse Head should check available quantity of Raw Material in stock and expiry date before raising “Retest Intimation Slip”. | |
| 5.3.3 | If the quantity is less than 5% of total quantity required for batch or if the material is nearing to expiry in such cases it is discarded raising a deviation note with prior authorisation from Quality Assurance Department. | |
| 5.3.4 | For sampling containers, sampling devices and sampling procedure refer SOP “Sampling, Analysis and Release or Rejection of Raw Materials”. | |
| 5.3.5 | On receipt of the test requisition from Warehouse, the sampling analyst or supervisor shall enter all details in “Raw Material Inward Register” and assign the Analytical Reference Number as per SOP “Sampling, Analysis and Release or Rejection of Raw Materials” and plan for sampling. | |
| 5.3.6 | Sampling analyst should draw the sample as per sampling plan for respective raw materials. | |
| 5.3.7 | For Active Materials: 100% sampling should be done as per the specifications of the raw materials. | |
| 5.3.8 | Inactive Materials: Up to 03 containers, bags or drums, 100% sampling should be done and for consignments with 04 to 100 or more containers/bags/drums, sampling should be done by √n+1 method where ‘n’ is the number of containers/bags/drums received. | |
| 5.3.9 | For Retest Sample quantity refer the respective Raw Material Specifications. Mark the test on specification which has to be performed during retesting. | |
| 5.3.10 | During the retesting of raw material only Critical tests shall be carried out which can affects the stability of the material. Refer below test list but not limited to: –
A) Description B) Loss on drying / Water / Loss on Ignition C) Assay D) Related substances / Chromatographic purity E) Microbiological limit test / Test for Microbiological contamination
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| Note: Above test are just examples. It can be change as per respective specification. | ||
| 5.3.11 | Put the container/bag/drum number on the sample polybag and deface the previously approved label on the container/bag/drum by making cross mark with black marker and affix “UNDER RETEST” (yellow colour) label as per Annexure on the container with a stamp “SAMPLED” for those container/bag/drum from which the sample is removed along with container number on each “UNDER RETEST” label. | |
| 5.3.12 | Move all the container/bag/drum of the consignment to the under test area. Affix the “UNDER RETEST” label on all the containers/bags/drums. | |
| 5.3.13 | If Microbiology testing is required then divide the sample quantity in two polybags i.e. Microbiology sample and Chemical analysis sample as per respective Raw Material Specification. | |
| 5.3.14 | Sampling analyst should visually take note of physical appearance of material while drawing the sample. | |
| 5.3.15 | If any discrepancy observed in physical appearance i.e. foreign particles, lumps, colour variation etc. then immediately bring it to the notice of the supervisor. | |
| 5.3.16 | Keep the analysis sample with “Raw Material Sample for Analysis’ label as per SOP “Sampling, Analysis and Release or Rejection of Raw Materials” in a designated place in Quality Control Laboratory. | |
| 5.3.17 | Fill up the log entries and affix “To be cleaned” label on sampling accessories as well as on sampling booth. | |
| 5.3.18 | For cleaning of sampling booth refer to the SOP “Cleaning and Operation of Sampling Booth”. | |
| 5.4 | Sampling procedure for Packing Materials due for retest: | |
| 5.4.1 | Warehouse head should give “Retest Intimation Slip” as per SOP “Management of Warehouse” prior to 15 days of the Retest Date as per approved label or Packing Material Stock Register. | |
| 5.4.2 | On receipt of the “Retest Intimation Slip” from Warehouse, Quality Control Department makes plan for sampling. | |
| 5.4.3 | For sampling procedure refer SOP “Sampling, Analysis and Release or Rejection of Packing Materials”. | |
| 5.4.4 | The sampling analyst or Supervisor shall enter all details in “Packing Material Inward Register” and assign the analytical reference number as per “Sampling, Analysis and Release or Rejection of Packing Materials” and plan for sampling. | |
| 5.4.5 | Sample quantity drawn should be sufficient for single analysis and as per respective Packing Material Specifications. Mark the test on specification which has to be performed during retesting. | |
| During the retesting of Packing material Critical tests shall be carried out which affects the quality of the Packing material. Refer below test list but not limited to: –
1-Description 2-Printed Text 3-VMCH coating 4-Pin hole Test 5-Colour scheme 6-Peel Test 7-Printing 8-Adhesive property 9- Sealing |
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| Note: Above test are just examples. It can be change as per respective specification. | ||
| 5.4.6 | Check the consignment as per Retest note for Batch or Lot no, Quantity and any external damages. | |
| 5.4.7 | Put the rolls/containers/boxes number on the sample polybag and deface the previously approved label on the rolls/containers/boxes by making cross mark with black marker and affix “UNDER RETEST” (yellow colour) label as per Annexure on the container with a stamp “SAMPLED” for those rolls/containers/boxes from which the sample is removed along with container number on each “UNDER RETEST” label. |
| 5.4.8 | Sampling analyst should visually take note of physical appearance of material while drawing the sample. | |
| 5.4.9 | If any discrepancy observed in physical appearance then immediately bring it to the notice of the Supervisor. | |
| 5.4.10 | Keep the analysis sample with “Packing Material Sample for Analysis” label as per SOP “Sampling, Analysis and Release or Rejection of Packing Materials” in a designated place in Quality Control Laboratory. | |
| 5.5 | Analysis, Release or Rejection of Retest Raw Materials and Packing Materials: | |
| 5.5.1 | Supervisor/QC Head shall allocate the testing samples to the analysts as per their job responsibility and specialisation. | |
| 5.5.2 | Analyst should refer respective specification to check the test parameters for retest Raw Materials and Packing Materials and also refer Standard Testing Procedure before initiating the testing. | |
| 5.5.3 | Carry out retesting for those tests which can demonstrate change in product quality by storing over a period or stability indicating tests which are capable to show material degradation. | |
| 5.5.4 | 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”. | |
| 5.5.5 | 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. | |
| 5.5.6 | In case of non-availability of Chemicals, Impurities, Working Standard, Instruments or Equipments 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 “Outside
Laboratory Testing” with relevant necessary information. |
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| 5.5.7 | If tests to be carried out as per IHS, copy of the protocol to be enclosed or scan copy to be mailed. | |
| 5.5.8 | Analyst should fill in the necessary details on the Analytical Work Report according to ‘Raw Material Inward Register’ or ‘Packing Material Inward Register’ and start the analysis as per Standard Testing Procedure and Specification. | |
| 5.5.9 | Ensure that all the Instruments are calibrated before use. | |
| 5.5.10 | Analyst should refer to the SOP of Instrument before operation and update the Instrument operation logs immediately after use. | |
| 5.5.11 | Analyst should refer to the SOP of Instrument before operation and update the Instrument operation logs immediately after use. | |
| 5.5.12 | After the analysis, analyst should hand over the Analytical Work Report to Supervisor/Reviewer analyst for data checking. | |
| 5.5.13 | If Supervisor/Reviewer observed any discrepancy with analysis or analytical data, he / she should consult to Head of the Department for investigation. | |
| 5.5.14 | 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” as per SOP “Preparation of Certificate of Analysis”. | |
| 5.5.15 | Quality Control Head shall verify and approve the COA and release the retest materials. | |
| 5.5.16 | Incase of Raw Materials, after approval of COA, analyst should prepare “APPROVED” labels (green colour) as per SOP “Sampling, Analysis and Release or Rejection of Raw Materials” with approved by signature on it. | |
| 5.5.17 | Incase of Packing Materials, after approval of COA, analyst should prepare “APPROVED” labels (green colour) as per SOP “Sampling, Analysis and Release or Rejection of Packing Materials” with approved by signature on it.
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| 5.5.18 | Affix “APPROVED” labels on top of the “UNDER RETEST” label on all containers in such a way that the “UNDER RETEST” word on the label should be covered but the details on the Under Retest label should be seen. | |
| 5.5.19 | No need to mention potency/Assay and Water/LOD/LOI on approved label in case of Inactive Materials. | |
| 5.5.20 | Photocopy of the approved COA shall be provided to the Warehouse Department if required. | |
| 5.5.21 | Leftover samples should be destroyed as per SOP “Destruction of Laboratory Waste”. | |
| 5.5.22 | During analysis if analyst observes the results Out of Specification or out of limits, he / she should report to the Supervisor or Head of the Department. | |
| 5.5.23 | Supervisor shall initiate investigation as per SOP “Out of Specification” by filling OOS form. | |
| 5.5.24 | After completion of investigation, categorise the observation as analyst error, reagent error, Instrument error or material defect. | |
| 5.5.25 | If material has major defect that can affect product quality or out of respective Pharmacopoeial monograph or IHS then material should be rejected. | |
| 5.5.26
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After detailed investigation prepare a COA for rejected material with a remark as “Material does not complies with the prescribed standards’’ and affix the labels on the material as “REJECTED” (Red Colour) with rejected by signature and the reason for rejection as per SOP . | |
| 5.5.27 | Photocopy of Rejected COA shall be provided to Warehouse. Photocopy is not necessary if software (ERP) is used for material inventory or control. | |
| 5.5.28 | Rejected Material shall be disposed as per SOP “Destruction of residues and line rejects”. | |
- Definitions / Abbreviations:
- Definitions:
- Retest Period: Retest Period is the period of time during which the Raw Materials and Packing Materials can be considered to remain within specifications, and therefore acceptable for use in the manufacture of a given drug product, provided that it has been stored under defined conditions. After this period, these should be retested for compliance with the specifications before use.
- Expiry Date: The date at which a product is no longer potent or of therapeutic value, determined by The date for a drug estimated for its shelf life with proper storage in sealed containers away from harmful and variable factors like heat and humidity.
- Abbreviations:
| Abbreviation | Expansion |
| SOP | Standard Operating Procedure |
| QC | Quality Control |
| QA | Quality Assurance |
| WH | Warehouse |
| UV | Ultra Violet |
| √n+1 | Under route of n = numbers of containers, bags, drums |
| COA | Certificate of Analysis |
| % | Percentage |
| i.e. | That is |
| A. R. No | Analytical Reference Number |
| IHS | Inhouse Specification |
| OOS | Out Of Specification |
| ERP | Enterprise Resource Procedures |
| PVC | Poly Vinyl Chloride |
| PVDC | Poly Vinyl Dichloride |
*Note – Ready to use SOP available in “DOWNLOAD” Section.