Checklist / Check points of Laboratory preliminary Investigation (OOS Phase I) for find out the root cause for out of specification (OOS) test results.
Laboratory Investigation Check Points / Report
OOS Number | : | OOS login Date | : | |||||||||
Name of Product | : | |||||||||||
Batch No. | : | Market | : | |||||||||
Batch Size / Qty | : | Mfg. Date | : | |||||||||
Test | : | G.R. No. / A.R. No. | : | |||||||||
Name of Analyst | : | Date of the Analysis | : | |||||||||
Stage |
: | RM FP | Exp. Date / Retesting Date | :
| ||||||||
Others (specify) | ||||||||||||
Release | Stability | |||||||||||
Raw Material/Packing Material/Finished Product/Stability/In process (Laboratory Investigation) | ||||||||||||
Sr. No. | A.R. No. | Batch No. | Pack Code & Packing details | Condition | Observation | |||||||
Details of OOS Result [Relevant code of product (Finished Product/RM/PM) shall be maintained]: | |
Related : SOP for Handling Out of Specification (OOS) Results | |
Whether the OOS is Re-occurrence (Yes/No) If Yes OOS No.: ____________ | |
Name of Analyst/Initiator : | Name of Reviewer : |
Sign / Date : | Sign / Date : |
Section A:
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Laboratory Investigation (Phase 1a):-
Date of Laboratory Investigation :- | |||||
Method/ Analyst Verification | Observation | Yes | No | Suspected | |
1. | Was analyst trained in the particular test / techniques? | ||||
2. | Was corrected standard test procedure used for the analysis? (Specify the number with current version) | ||||
3. | Was analytical method adequate and followed properly? | ||||
4. | Was evident from the discussion that the analyst has understood Analytical Method and the operation SOP of the equipment/ instrument used? | ||||
5. | Was there evidence that the system suitability requirements of the analytical method met? | ||||
6. | Had the analyst calculated that results correctly as mentioned in standard test procedure? | ||||
7. | Had the analyst calculated the results using correct potency of the working / reference standard? | ||||
8. | Was there any similar history with the product / material? | ||||
9. | Was any past incident done by the same analyst and what was the conclusion? | ||||
10. | Was any past incident happened in test parameters in same product and what was the final conclusion? | ||||
11. | Was stock solution of standard, system suitability, sample and or any other solution available? |
Laboratory Glassware Verification / Investigation | |||||
12. | Were proper volumetric glassware used for analysis? | ||||
13. | Were correct volumetric pipettes / burettes used for analysis? | ||||
14. | Was there any obvious evidence of glassware contamination? (Visual) | ||||
15. | Was there any evidence or probability that the glass ware not washed or dried properly? | ||||
16. | Were the glassware used for analysis properly and legibly labeled? | ||||
Analysis Process Verification (Laboratory Investigation) | |||||
17. | Was there any evidence that the sample was not stored properly? | ||||
18. | Were the dilutions made in sample / standard preparation as per standard test procedure? | ||||
19. | Were the environmental conditions (temperature, Relative humidity, light) during analysis appropriate? | ||||
20. | Were there any instrument related problem noticed? | ||||
21. | Were the regents / chemicals used of recommended grade and prepared as per the standard test procedure? | ||||
22. | Were used volumetric solutions standardized as per procedure? | ||||
23. | Were the correct working / reference standard used for analysis? (specify the number with validity) | ||||
24. | Were the standards, reagents, used, properly stored? | ||||
25. | Was there evidence that the reagents, standards or other materials used for test were contaminated? | ||||
Equipments / Instruments | |||||
26. | Was the instrument used for analysis with in the calibration period? For example HPLC, GC, UV, Dissolution etc. (specify the ID number & next calibration due date) | ||||
27. | Was Instrument Set-up according to standard test procedure? | ||||
28. | Was the possibility of any leakage or air bubble in the system? | ||||
29. | Was the correct system parameters used during analysis? | ||||
30. | Was the proper electrical and tubing connections given to the system? | ||||
31. | Was the correct volume of dissolution medium used for analysis? | ||||
32. | Dose any physical observation noted during dissolution testing? | ||||
33. | Was there any power failure during analysis? | ||||
Chromatographic related parameters (Laboratory Investigation) |
Mobile Phase | |||||
34. | Was the pH of the Mobile Phase adjusted correctly as per standard test procedure? (specify if any) | ||||
35. | Was the mobile phase filtered by using proper filters specified in standard test procedure? | ||||
36. | Was the mobile phase degassed properly before usage? | ||||
Column | |||||
37. | Was the corrected column used as specified in standard test procedure? (specify the column number) | ||||
38. | Was any leakage observed in column fittings? | ||||
39. | Was the column flushed properly before usage? | ||||
40. | Was the correctness of raw data peak shape, system suitability criteria, retention time matching? | ||||
Heating Equipment (LOD Oven and muffle furnace) | |||||
41. | Were the temperature indicators within calibration range? (specify the next calibration due date) | ||||
42. | Was the heating equipment malfunctioning observed during operation? | ||||
Weighing Verification (Laboratory Investigation) | |||||
43. | Balance I.D. No.: | ||||
44. | Was the balance used for weighing, within calibration date? (specify next calibration date) | ||||
45. | Were weights taken accurately, without spillage? | ||||
46. | Was the weighing as per standard test procedure? | ||||
47. | Was the malfunctioning of balance observed during weighing? | ||||
Karl Fisher / Auto titrator | |||||
48. | Was the instrument calibrated before use? (specify the identification number & next calibration due date) | ||||
49. | Was the corrected factor used for analysis? | ||||
Stability Chambers | |||||
50. | Was the instrument / equipment within calibrated period? (specify the ID number & next calibration due date) | ||||
51. | Was the temperature & humidity mapping within the specified acceptance criteria for the particular temperature and humidity condition? | ||||
52. | Was the temperature & humidity within the acceptance criteria? | ||||
53. | Was the breakdown/malfunctioning /excursion observed for the particular stability chambers? | ||||
pH Meter | |||||
54. | Was the pH meter within the calibration period? (specify the calibration date) | ||||
55. | Was the standard buffer used for calibration within validity period? | ||||
Related Substances Analysis (Laboratory Investigation) | |||||
56. | Was system, purged before start of the analysis? | ||||
57. | Was blank solution (Diluent / mobile phase) injected to identify any unknown peaks? | ||||
58. | Was standard, system suitability, placebo and sample solution injected within the solution stability period? | ||||
59. | Was the peak of concern is an unknown impurity? | ||||
60. | Was the peak of concern is degradation product? | ||||
61. | Was peak of concern found in blank / mobile phase / placebo? | ||||
Laboratory Condition (Investigation) | |||||
62. | Was the laboratory environment satisfactory during the testing of the samples? |
Details of the interview of the Analyst:
Name of Analyst: ___________________________
Name of Interviewer :_________________________
Analyst Sign/Date: Interviewer Sign/Date :
Summery / Conclusion of Laboratory Investigation: Prepared By Sign / Date: QC Head Sign / Date: |
Laboratory Hypothesis Analysis / Investigation (Phase 1b)
S.No. | Repeat Analysis (Re-Analysis) | Yes | No | Comments | Annexure |
1. | Re-injection from the same vial (original preparation) for verification to identify injection error or programming error | ||||
2. | Re-filtration from the same final dilution of the sample to verify the usage of inappropriate filter paper, insufficiently saturated filter or contaminated vials, septum’s / filters. | ||||
3. | Re-dilution from the stock solution to investigate if the incident is due to dilution error. If yes, then the same stock solution shall be re-diluted, wherever applicable and analyzed. | ||||
4. | Re-sonication / Re-shaking due to incomplete solubilization of the analyze in the test preparation due to inadequate shaking and / or sonication or improper grinding of the test sample, wherever applicable. | ||||
5. | Any other (if) | ||||
Summery of Laboratory investigation from hypothesis: Prepared by Sign / Date: Reviewed By Sign/Date: |
Conclusion with justification: | |||
Recommended Corrective & Preventive Action (From Phase Ia and Ib): | |||
QA Comments | |||
Section B: Phase-IIa Investigate checklist related to manufacturing process | |||
OOS number:- | |||
Sr. No. | Check Points | Observations | Remarks |
Process: | |||
1. | Is the right and approved procedure used in processing? | ||
2. | Whether approved BMR is used? (Mention MFR and BMR number) | ||
3. | Whether all steps of processing followed properly as per BMR? | ||
4. | Whether the process is validated? | ||
5. | Whether each process steps is checked by the concerned department supervisor? | ||
6. | Whether yield reconciliation carried out and yield is within the limits as per BMR/BPR? | ||
7. | Whether change control or deviation is proposed for this batch? (Mention Change control or Deviation number) | ||
Personnel: | |||
1. | Is the operator adequately trained and followed BMR/BPR? | ||
2. | Whether the SOPs followed properly? | ||
3. | Whether the hygienic practices followed? | ||
Equipment: | |||
1. | Whether right equipments used as per BPR and details recorded in equipment logbook? | ||
2. | Whether all equipment used in the process have been qualified? | ||
3. | Whether the manufacturing equipments operated as per SOP? | ||
4. | Whether critical gauges and manufacturing devices are calibrated and used within calibration due date? | ||
5. | Whether all the equipments are cleaned before use? | ||
6. | Whether preventive maintenance carried out for all equipments used in processing? | ||
Material: | |||
1. | Whether the right materials dispensed for the batch? | ||
2. | Whether API and excipients used for the batch are approved? | ||
3. | Whether exact quantity of the material is dispensed as per BPR? | ||
4. | Whether the right material used during processing? | ||
5. | Were there any changes of contamination? | ||
Area: | |||
1. | Whether area cleaning and sanitation carried out as per SOP? | ||
2. | Whether environmental conditions are monitored and recorded as per BPR? | ||
Others: | |||
1. | Product contamination (give details) | ||
2. | Any other observation made by the operator during operation | ||
Sampling: | |||
1. | Whether correct material / product are sampled? | ||
2. | Whether appropriate SOP followed for sampling? | ||
3. | Whether sample was properly stored and handled? | ||
4. | Whether correct sampling tools are used? | ||
5. | Whether sampling personnel trained as per SOP? | ||
6. | Whether sampling personnel understood the procedure? | ||
7. | Whether hygiene practices are followed throughout sampling? | ||
8. | Whether any other contamination sources observed? | ||
9. | Error in sampling: Handling Error: Error in storage of sample: | ||
10. | Any abnormal observation(s) in environmental monitoring records | ||
11. | Error in labeling details in the container to be sampled & product name, manufacturing details, etc. | ||
Re-Sampling | |||
12. | Whether re-sampling performed only when original sample is proved an unrepresentative? | ||
13. | Whether re-sampling performed only when original sample quantity was not sufficient? | ||
14. | Whether re-sampling performed as per method used for initial sample? | ||
15. | Whether new-sampling method is developed only when initial sampling method found faulty (error)? | ||
Phase – IIa Investigation Details:
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