Standard Operating Procedure for Retesting of Raw Material, Packaging Material and Semi-Finished Product
1.0 Purpose:
To lay down a procedure for Retesting of Raw Material, Packaging Material and Semi-Finished Product.
2.0 Scope:
The scope of this SOP is applicable for Retesting of all Raw Material (Active and Excipients), Packaging Material and Semi-Finished Product in quality control laboratory at [company name].
3.0 Responsibility:
3.1 Warehouse – Personnel: Arrangement of Raw Material and Packaging Material for sampling.
3.2 QC – Personnel:
- Sampling of Raw Material and Packaging Material due for Retesting.
- Analysis of Raw Material, Packaging Material and Semi-Finished Product.
3.3 QA – Personnel (IPQA): Sampling of Semi-Finished Product due for Retesting.
3.4 Section Head – QC / Designee: Planning for Analysis and review of reports.
3.5 Head- QC / Designee: Approval of Raw Material and Packaging Material.
3.6 Head – QA / Designee: Approval of Semi-Finished Product.
4.0 Definitions:
Definitions-Not Applicable
5.0 Procedure:
5.1 Common Retest parameters are mentioned in respective Formats.
5.2 For the Intermediate Granules retest shall be performed as per the respective specification except Identification test.
5.3 Retest Period for Raw Material shall be as follows;
| Raw Material (Active) | 12 Months (365 Days) |
| Raw Material (Excipient) | 12 Months (365 Days) |
| Raw Material (Active & Excipients) with Microbiological testing | 6 Months (183 Days) |
| Raw Material (Liquid) | 6 Months (183 Days) |
| Raw Material (Color’s) | 12 Months (365 Days) |
| Intermediate Granules and Intermediate Blend | 30 Days |
5.4 Retest Period for Packaging Material are mentioned in respective format. New material shall be added manually in respective format and subsequently revision in the SOP. On receipt of new Packaging Material or further new testing parameters needs to be added, the test parameters shall be amended in the respective Format manually and subsequently revision in the SOP.
5.5 Hold time period for Semi-Finished Product shall be as follows,
| Blend | 7 Days |
| Compressed Tablets (Core) | 30 Days |
| Coated Tablets | 30 Days |
| Filled Capsules | 30 Days |
5.6 Hold time period as mentioned above are not applicable for the Semi finish product whose Hold time study is established. Those are covered under the scope of SOP for conducting Hold Time study.
5.7 Hold time period is also fed in the SAP System.
5.8 On receipt of new Raw Material / Semi-Finished Product or further new testing parameters needs to be added, the test parameters shall be amended in the respective Format manually and subsequently revision in the SOP.
5.9 Retesting test parameter shall be selected from the respective specification and listed in respective Formats.
5.10 In case there is no immediate requirement of retesting of material, it shall be done prior to use.
5.11 Retesting of Raw Materials / Semi – Finished shall be done as per the retesting test parameters list.
5.12 The test to be performed during retest is not limited to the retesting test parameters list.
5.13 Retest of material shall be maintained and managed through SAP system.
5.14 In case the material is due for Retest, it must be used only after Retesting.
5.15 In Case material undergoes in retest within 7 working days (because of any reason) from date of material release, the results shall be out source from recent analysis of material.
5.16 For Raw Material and Packaging Material:
5.16.1 Retest Dates shall be given for Raw Material and Packaging Material from Usage Decision (UD) Approval date + inspection interval and the same shall be mentioned on the “Approved” Label & COA
5.16.2 Raw Material having 12 months Retest Period (i.e. Active and Excipients without microbiological testing and Colours), shall be retested three times (or less than 3 times) with the interval of 12 months from the date of release in LIMS and continued up to its expiry date.
5.16.3 Raw Material having 6 months retest period (i.e. Active and Excipients with microbiological testing and Liquids), shall be retested seven times (or less than 7 times) with the interval of 6 months from the date of release in LIMS and continued up to its expiry.
5.16.4 When a material attends its Retest Date, the balance quantity in SAP moves from “Un Restricted Zone” to “Quality Inspection” automatically. It signifies that the material cannot be issued without re-conforming (retesting) its quality parameters by Quality Control.
5.16.5 Physically, Warehouse – Personnel shall transfer the material from “Approved” area to “Quarantine” area and affix the “Quarantine” label as per respective SOP.
5.16.6 QC Person will get the list of materials to be retested by accessing the “Quality Inspection” lot under “09” (Lot 09 in SAP is for materials to be retested).
5.16.7 QC Personnel shall take printout of “Under Test” labels as per respective SOP.
5.16.8 QC Personnel shall sample the retesting material as per the respective SOPs.
5.16.9 For retest procedure perform a set test parameter separately for respective Raw Material and Packaging Material as per respective Format.
5.16.10 In case where the vendor or supplier of any raw material provides an expiry date on the Certificate of Analysis (CoA), the material is considered expired beyond that date and retest is continued up to that date.
5.16.11 In case where the vendor or supplier of any raw material doesn’t provide an expiry date , retest date and re-evaluation date on the Certificate of Analysis (CoA), the material shall be considered expired only after 48 months from the date of manufacturing of that particular raw material, provided by the vendor or supplier.
5.16.12 In case the vendor or supplier of any raw material has mentioned retest date and or re-evaluation date on the Certificate of Analysis (CoA), that date shall be considered as an expiry date of that particular raw material and consider 48 months as expiry from the manufacturing date if retest date and re-evaluation is not given.
5.16.13 For Pre-sterilize material retesting shall be done at the frequency of 2 years and Sterility test shall be performed along with Description test.
5.16.14 QC – Person shall release the Raw Material as per respective SOP and Packaging Material as per respective SOP.
5.16.15 QC – Personnel shall take printout of “Approved” or “Rejected” label as per respective SOP.
5.16.16 Physically, Warehouse – Personnel shall transfer the material from “Under Test” area to “Approved” area.
5.17 For Semi-Finished Product:
5.17.1 Hold time period and valid up to date shall be given for Semi-Finished Product from the date of its sampling & posting date (lot initiated date + inspection interval) and the same shall be mentioned on the “Approved” Label.
5.17.2 QA – Personnel shall check the Certificate of Analysis (CoA) at the time of giving line clearance for the next step. During this period he /she will come to know the material retest status (whether the retest is due or not).
5.17.3 QA – Personnel shall collect the sample as per respective SOP and hand over it to QC department. QC Person shall make necessary entries in “Semi-Finished Retest Sample Inward” register.
5.17.4 QC – Personnel shall perform the analysis as per the respective Format No. and also compare the test parameters with respective Specification.
5.17.5 On completion of analysis, QC – Personnel shall hand over the Sampling Sheet to QA – Personnel.
5.17.6 Head-QA / Designee shall approve the Semi-Finished Product. QA – Personnel shall enclose the Certificate of Analysis (CoA) in Batch Manufacturing Record (BMR) and affix “Approved” status label.
6.0 Frequency:
As applicable
7.0 Format for recording:
7.1 Retesting Test Parameters of Raw Material
7.2 Retesting Test Parameters of Packaging Material
7.3 Retesting Test Parameters of Semi-Finished Product
7.4 Retesting Frequency for Packaging Material
7.5 Distribution list of SOP and Formats/Annexures
Retesting Test Parameters of Raw Material
| Sr. No. | Test parameters | Updated By Sign and Date | Verified By Sign and Date |
| 01. | Description / Appearance | ||
| 02. | Assay | ||
| 03. | Related Substance (By TLC, By HPLC, By GC) | ||
| 04. | pH | ||
| 05. | Conductivity | ||
| 06. | Specific Optical Rotation and Optical Rotation | ||
| 07. | Film Formation and Dispersion Test | ||
| 08. | Physical Parameter of EHG Capsule | ||
| 09. | Microbial Limit Test (MLT) | ||
| 10. | Bacterial Endotoxin Test (BET) | ||
| 11. | % Water Content | ||
| 12. | % Loss on Drying (LOD) | ||
| 13. | Specific Gravity | ||
| 14. | Refractive Index | ||
| 15. | Melting Point | ||
| 16. | Boiling Point | ||
| 17. | Ordinary Impurities | ||
| 18. | Protein & Light Absorbing Impurities | ||
| 19. | Vinyl Pyrrolindine | ||
| 20. | 2-Pyrrolidone | ||
| 21. | Formic Acid | ||
| 23. | Relative Content of Stearic Acid & Palmitic test | ||
| 24. | Any Impurity Test | ||
| 25. | Extraneous Matter | ||
| 26. | Phosphate Binding Capacity |
| Sr. No. | Test parameters | Updated By Sign and Date | Verified By Sign and Date |
Retesting Test Parameters of Packaging Material
| Sr. No. | Test parameters | Updated By Sign and Date | Verified By Sign and Date |
| 01. | Description / Appearance | ||
| 02. | Sterility Test (For Sterile Packaging Material) | ||
Retesting Test Parameters of Semi-Finished Product
| Sr. No. | Test parameters | Updated By Sign and Date | Verified By Sign and Date |
| 01. | Description / Appearance | ||
| 02. | Assay | ||
| 03. | Related Substance | ||
| 04. | Loss on Drying | ||
| 05. | Water Content | ||
| 06. | Microbial Limit Test (MLT) | ||
Retesting Frequency for Packaging Material
| Sr. No. | Material Name | Retest Period |
| 01. | Film PVC, PVC-PVdC, PVC-PE-PVdC | 6 Month |
| 02. | Film PVC – Aclar | 6 Month |
| 03. | Silica Gel Bag (Blue and White) | 6 Month |
| 04. | Silica Gel Sachet | 6 Month |
| 05. | Silica Gel Canister | 6 Month |
| 06. | Molecular Sieve Sachets | 6 Month |
| 07. | Oxygen Absorber Canister | 6 Month |
| 08. | Pallets | 6 Month |
| 09. | 5 and 10 ml HDPE / LDPE Bottle | 6 Month |
| 10. | LDPE / HDPE Nozzles (Eye dropper) | 6 Month |
| 11. | Tamper HDPE Cap (Injectable) | 6 Month |
| 12. | Foil Blister & Stripe Aluminum (Plain and Printed) | 1 Year |
| 13. | Foil Alu-Alu. | 1 Year |
| 14. | Plain / Printed Peelable Foil | 1 Year |
| 15. | Carton (Plain and Printed) | 2 Year |
| 16. | Catch Cover | 2 Year |
| 17. | Leaflets (Outserts /Inserts) | 2 Year |
| 18. | Label (Plain and Printed) | 2 Year |
| 19. | Film Stretch | 2 Year |
| 20. | Cotton, Polyester, Rayon | 2 Year |
| 21. | Container With Cap (Jar) | 2 Year |
| 22. | Outserts (Leaflets) | 2 Year |
| 23. | Booklet | 2 Year |
| 24. | HDPE Bottle / Container | 2 Year |
| 25. | HDPE/Polypropylene Closure | 2 Year |
| 26. | Rubber Stoppers | 2 Year |
| 27. | BOPP & Cello Tape (Plain and Printed) | 2 Year |
| 28. | Shipper & 3 Ply Box (Corrugated Box) | 2 Year |
| 29. | LDPE Air Bubble Bag | 2 Year |
| 30. | Trilaminate High Barrier (THB) Bag | 2 Year |
| 31. | Grey Board Box | 2 Year |
| 32. | Polyethylene Bag | 2 Year |
| 33. | Transparent Stickers | 2 Year |
| 34. | Polyethylene Bag (Heat Shrink) | 2 Year |
| 35. | Plastic Seal (Plain and Printed) | 2 Year |
| 36. | Vial 2 ml, 5 ml, 10 ml and 25 ml | 2 Year |
| 37. | Seal Alu Flip-Off | 2 Year |
| 38. | Plastic Tray | 2 Year |
| 39. | Thermocole Box | 2 Year |
| 40. | Alcohol Swab | 2 Year |
| 41. | Needles | 2 Year |
| 42. | Syringes | 2 Year |
| 43. | Pad Seal | 2 Year |
| 44. | Drum (HDPE and Fibre) | 2 Year |
| 45. | 5 and 10 ml HDPE / LDPE Bottle (Other than BPREX) | 2 Year |
| 46. | LDPE / HDPE Nozzles (Eye dropper) (Other than BPREX) | 2 Year |
| 47. | Tamper HDPE Cap (Injectable) (Other than BPREX) | 2 Year |
| 48. | Pre Filled Syringe | 2 Year |
| 49. | Stopper Plunger | 2 Year |
| 50. | Plunger Rod | 2 Year |
| 51. | Safety guard for needle | 2 Year |