Standard Operating Procedure on Withdrawal, Storage, Observation & Destruction of Control/Retention Sample in Pharmaceuticals.
1.0 Objective: This SOP applies to the withdrawal, storage, observation, and destruction of control samples from production (OSD & Injectable) and Quality control (R.M. Retention) in the pharmaceutical formulation plant.
2.0 Scope: This Standard Operating Procedure applies to the withdrawal, storage, observation, and destruction of control samples from production (OSD & Injectable) and Quality Control (R.M. Retention) in the pharmaceutical formulation plant.
3.0 Responsibility
3.1 QA/QC officer is responsible for the implementation of this SOP.
4.0 Accountability
The QA Head shall be accountable for the Overall compliance with this SOP.
6.0 Procedure
6.1 Withdrawal of Control Sample
6.1.1 Control samples of drug products shall be withdrawn from each batch of products that is under manufacturing.
6.1.2 The quantity of the sample shall be withdrawn as per Table-I.
| S.No. | Sample | Quantity of Sample Drawn (in Units) |
|---|---|---|
| 01 | Tablets | 200 |
| 02 | Capsules | 200 |
| 03 | Dry Syrup (Bottles) | 44 |
| 04 | Dry Powder injection | 128 |
6.1.3 The QA Officer shall collect the finished product control sample from each batch during the packing operation as per the quantity mentioned in Table-I. The entry shall be made in the finished product control sample logbook as per Annexure No.-I.
6.1.4 For Raw Material retention samples, the QC personnel shall collect the sample and make the entry in the raw material retention sample logbook as per Annexure No.-II.
6.1.5 Control Sample sticker labels shall be affixed to each pack as per Annexure No.-III.
6.1.6 The control sample shall proportionately represent all different pack sizes in the same batch sales/Physician sample.
6.1.7 Liquid and solvent are not retained in the control sample room.
6.2 Storage of Control Sample
6.2.1 The control sample shall be stored at a temperature not exceeding 25°C.
6.2.2 Temperature monitoring records of the control sample room shall be maintained as per the “SOP on Monitoring of Temperature and Relative Humidity.”
6.3 Physical Observation of Control Sample
6.3.1 Physical observation will be conducted every six months, and the observation records shall be maintained as per Annexure No.-V.
6.3.2 During physical observation, the following points shall be considered, wherever applicable:
- Appearance/Description
- Packing Quality
- Imprinting
- Overprinting
- Intactness of the package
- Delamination
- Peeling/Motting of coated tablets
6.3.3 If a specific amount of control sample or retention sample is needed for testing or reference purposes, it will only be provided once the request is approved, in accordance with Annexure No.-IV. Such withdrawals shall be recorded in the ‘Finished Product Control Sample Logbook’ and ‘Raw Material Retention Sample Logbook’ as per Annexure No.-I and Annexure No.-II, respectively.
6.4 Destruction of Control Sample
6.4.1 Control samples and retention samples shall be destroyed after one year from the expiry date. Refer to the ‘SOP on Handling Scrap and Disposal‘ for the destruction process.
6.4.2 Destruction records of finished product control samples and raw material retention samples shall be maintained in the ‘Finished Product Control Sample Logbook’ as per Annexure No.-I and ‘Raw Material Retention Sample Logbook’ as per Annexure No.-II.
7.0 Forms and Records (Annexures)
Annexure-I: Finished Product Control Sample Logbook
Annexure-II: Raw Material Retention Sample Logbook
Annexure-III: Control Sample Sticker Label
Annexure-IV: Control Sample/Retention Sample Requisition Slip
Annexure-V: Physical Observation of Control Sample
Related: Quality Control Test for Secondary Packing Materials
8.0 Distribution
Master copy: Quality Assurance
Controlled copies: Quality Assurance, Production, Quality Control & Warehouses RM.
5.0 Abbreviations and Definitions
SOP: Standard Operating Procedure
QA: Quality Assurance
Annexure-I: Finished Product Control Sample Logbook
| Batch No. | Product Name | Date of Sample Withdrawal | Quantity Drawn (Units) | Remarks |
Annexure-II: Raw Material Retention Sample Logbook
| Batch No. | Raw Material Name | Date of Sample Collection | Quantity Drawn (g/kg) | Remarks |
Annexure-III: Control Sample Sticker Label
Annexure-IV: Control Sample/Retention Sample Requisition Slip
| Requested By | Date of Request | Purpose of Request | Quantity Requested (Units/g/kg) | Approved By | Date of Approval |
Annexure-V: Physical Observation of Control Sample
| Batch No. | Product Name | Date of Observation | Observations | Remarks |
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