SOP Title: Sampling, Handling and Analysis of Stability Study Samples
- Objective:
To lay down the procedure for Sampling, Handling and Analysis of Stability Study Samples.
- Scope:
This procedure is applicable for Sampling , Handling and Analysis of Stability Study Samples.
- Responsibility:
- Quality Control Department: To prepare and review the SOP. To follow the procedure for Sampling and Handling of Stability Study Samples as per this SOP.
- Quality Assurance Department: To review and approve the SOP and Annexure.
- Accountability:
Head Quality Control Department, Head Quality Assurance Department
- Procedure:
| 5.1 | Sampling and Handling of Samples: | |
| 5.1.1 | Stability Sample study shall be carried out for first three consecutive batches of Finished Product of every new product. | |
| 5.1.2 | Quality Assurance Associate shall collect the Finished Product sample for stability study analysis as per approved stability study protocol. | |
| 5.1.3 | Finished Product should be sampled for Stability Study in a intact pack size. | |
| 5.1.4 | The real time study shall be carried out for 3 months, 6 months, 9 months,
12 months, 18, months, 24, months and 36 months or as per stability study protocol at 30°C ± 2°C / 65% RH ± 5% RH. |
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| 5.1.5 | The Accelerated studies shall be carried out for 3 months and 6 months at
40°C ± 2°C / 75% RH ± 5% RH. |
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| 5.1.6 | Sample quantity should be calculated as per stability period and type of analysis requirement. | |
| 5.1.7 | For example: For complete physico-chemical single analysis, number of Tablets /Capsules required is 40 and for microbial analysis 40 then total number of units to be sampled for single analysis is 80. | |
| 5.1.8 | If stability to be performed for 36 month for Real time and 3 and 6 month for Accelerated, total of analysis will be 7+2= 9 and quantity of sample to be withdrawn for Stability Study will be 9 x 80 units =720 nos. | |
| 5.1.9 | 1. If packing style is not 10 tablets/Capsules per strip, then sample quantity may be slightly more than as above; but any stage it cannot be less than required quantity. | |
| 5.1.10 | 2. Label the Stability samples as per define Annexure. | |
| 5.1.11 | 3. Incubate Stability Study Samples to respective stability chambers as per stability protocol and fill up the respective Stability sample Entry Register. | |
| 5.1.12 | After incubation of stability sample, prepare stability scheduler for respective batches as per define Annexure. | |
| 5.1.13 | Real time Stability Study Samples details are entered in ‘Finished Product Real Time Stability Sample Entry Register’. | |
| 5.1.14 | 4. Accelerated Stability Study Samples details are entered in ‘Finished Product Accelerated Stability Sample Entry Register’. | |
| 5.1.15 | Supervisor shall prepare the “Stability Sample Monthly pull out log” at initial of the respective month, according to the “stability scheduler”. | |
| 5.1.16 | The Samples shall be withdrawn from the respective chambers at stated interval within + 5 working days of the due day. If the stability period is shorter than 3 months then withdrawn should be completed within + 2 working days from the due date. | |
| 5.1.17 | As per the stability scheduler, samples shall be pull out at regular intervals and withdrawn quantities shall entered in respective registers. | |
| 5.1.18 | The samples shall be stored at specified condition until the completion of analysis. | |
| 5.1.19 | On receipt of sample, Analyst should give requisition for “Analytical Work Report” to the quality assurance department. | |
| 5.1.20 | Assign Analytical Reference Number (A. R. No.) as “SS/XX/NNN”
Where, ‘SS’ stands for ‘Stability Study’ ‘XX’ stands for ‘Last two digits of the current year’. ‘NNN’ stands for ‘Serial number i.e. 001, 002 and so on’. |
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| 5.1.21 | Analyst should fill in the necessary details on the Analytical work report according to ‘Stability Sample Inward Register’. | |
| 5.1.22 | Stability Samples shall be tested as per respective specification. Analyst shall refer standard testing procedure and analyse the sample accordingly. | |
| 5.1.23 | The testing of the stability samples should be completed within 30 days from the due date. If the stability period is shorter than 3 months then testing should be completed within 15 days from the due date. If for some reason, it is not possible to analyse the sample within specified testing window then deviation shall be raised with proper justification and impact shall be assessed.
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| 5.1.24 | After the analysis, analyst should hand over the Analytical Work Report to Supervisor/Reviewer 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. | |
| 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 “Stability Summary Report” as per define Annexure. | |
| 5.1.27 | Quality Control Head shall verify Stability Summary Report. | |
| 5.1.28 | After verification of Stability Summary Report, Supervisor/QC Head shall hand over the Stability Summary Report to Quality Assurance Department for approval. | |
| 5.1.29 | Leftover samples should be destroyed as per SOP “Destruction of Laboratory Waste”. | |
| 5.1.30 | During analysis if analyst observes the results out of specification (OOS) or out of limits, he / she should report to the Supervisor or Head of the Department. | |
| 5.1.31 | Supervisor shall initiate investigation as per SOP “Out of Specification” by filling OOS form. | |
| 5.1.32 | After completion of investigation, categorise the observation as analyst error, reagent error, instrument error or material defect. | |
| 5.1.33 | Based on detailed investigation and type of error decision shall be taken for further course of action or recall of the product. | |
| 5.1.34 | Update the Stability Sample Inward Register after completion. | |
| 5.1.35 | If long-term studies are conducted at 25°C ±2°C/60% RH ±5% RH and “significant change” occurs at any time during 6 months testing at the accelerated storage condition, additional testing at the intermediate storage condition should be conducted.
In general, “significant change” for a drug product is defined as: · A 5% change in assay from its initial value; or failure to meet the acceptance criteria for potency when using biological or immunological procedures. · Any degradation product’s exceeding its acceptance criterion.
· Failure to meet the acceptance criteria for appearance, physical attributes, and functionality test (e.g., color, phase separation, re-suspendability, caking, hardness, dose delivery per actuation); however, some changes in physical attributes (e.g. melting of creams) may be expected under accelerated conditions; and, as appropriate for the dosage form. · Failure to meet the acceptance criterion for pH. · Failure to meet the acceptance criteria for dissolution testing at 12 dosage unit. |
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| 5.1.36 | Incubation shall be maintained at ± 2° C of the Specified temperature and ± 5% of the Specified Relative Humidity.
Any deviation as mentioned below must be assessed for impact and reported to the Head of QA Department. Deviation of > ±2° C to ± 5°C from the set point for 48Hours. Deviation of > ±5% RH to ± 10% from the set point for 48Hours. Deviation of > ±5° C from the set point for 24Hours. Deviation of > ± 10% RH from the set point for 24Hours. |
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- Definitions / Abbreviations :
- Abbreviations :
| Abbreviation | Expansion |
| SOP | Standard Operating Procedure |
| QC | Quality Control |
| QA | Quality Assurance |
| °C | Degree Centigrade |
| RH | Relative Humidity |
| Nos. | numbers |
| ± | Plus or minus |
| % | Percentage |
*Note – Ready to use SOP available in “DOWNLOAD” Section.