Standard Operating Procedure for Raw Material Sampling Procedure in API Manufacturing
| Department | API Manufacturing |
|---|---|
| SOP No. | SOP/API/003/2025 |
| Supersedes | SOP/API/003/2022 |
| Page No. | Page 1 of 10 |
| Issue Date | 13/04/2025 |
| Effective Date | 15/04/2025 |
| Review Date | 13/04/2026 |
1. Purpose
To describe the procedure for sampling of raw materials such as APIs, excipients, and solvents in a GMP-compliant manner to ensure samples taken for analysis are representative of the entire batch or lot.
2. Scope
This procedure applies to all personnel involved in raw material sampling in the warehouse sampling booth or designated sampling area in the API manufacturing facility.
3. Responsibilities
- QC Analyst: Perform the sampling activity using validated tools and techniques as per the sampling plan.
- Warehouse Personnel: Present quarantined material in the correct sequence and assist during sampling.
- QA Officer: Review sampling records and ensure GMP and gowning practices are followed.
4. Accountability
The Head of Quality Control is accountable for ensuring proper implementation of sampling procedures and compliance with GMP requirements.
5. Procedure
5.1 Preparation for Sampling
- Ensure sampling is performed in a dedicated, validated sampling booth with differential pressure and HEPA filtration.
- Check environmental conditions and log temperature, humidity, and pressure differentials before starting.
- Wear appropriate personal protective equipment (PPE) as per gowning SOP.
- Verify cleanliness of sampling tools and containers; sterilize if required.
5.2 Sampling Plan and Strategy
- Follow the sampling plan as per ICH Q7 or √n+1 approach:
- √n+1, where n = total number of containers
- Minimum of 10% of total containers must be sampled
- Sample randomly from different positions – top, middle, bottom – using a thief sampler, scoop, or zone sampler.
- Prepare both individual samples (if required) and a composite sample for routine analysis.
- Use clean and inert sampling containers labeled with:
- Material name
- Batch number
- Date of sampling
- Sampled by (initials)
5.3 Sampling Procedure
- Place containers on a designated platform and inspect physical condition before opening.
- Use pre-sanitized tools and avoid contamination during sampling.
- Open each selected container under LAF and take sample volume as specified in the material specification file.
- Record the sample weight and seal containers properly after sampling.
- Affix “Sampled” labels on all containers from which samples were drawn.
5.4 Sample Transfer and Documentation
- Transfer samples to the QC lab with the “Sample Transfer Form” (Annexure-2).
- Document all details in the “Raw Material Sampling Log” (Annexure-1), including number of containers sampled, tool used, sample quantity, and sampling personnel.
- If a sample shows any unusual appearance or odor, notify QA and record it in the deviation register.
5.5 Cleaning and Closure
- After sampling, clean the sampling booth and disinfect all used tools.
- Update the cleaning log and leave the area ready for the next activity.
6. Abbreviations
- SOP: Standard Operating Procedure
- QC: Quality Control
- QA: Quality Assurance
- LAF: Laminar Airflow
- PPE: Personal Protective Equipment
7. Documents
- Raw Material Sampling Log (Annexure-1)
- Sample Transfer Form (Annexure-2)
- Sampling Plan Template (Annexure-3)
8. References
- ICH Q7: Good Manufacturing Practice Guide for Active Pharmaceutical Ingredients
- WHO TRS 986 Annex 2
- 21 CFR Part 211.84 – Testing and approval of components
9. SOP Version
Version: 2.0
10. Approval Section
| Prepared By | Checked By | Approved By | |
|---|---|---|---|
| Signature | |||
| Date | |||
| Name | Rajesh Kumar | Sunita Reddy | Manoj Verma |
| Designation | QC Officer | QA Executive | QA Manager |
| Department | API Manufacturing | Quality Assurance | Quality Assurance |
11. Annexures
Annexure-1: Raw Material Sampling Log
| Date | Material | Batch No. | No. of Containers | Qty Sampled | Sampled By |
|---|---|---|---|---|---|
| 13/04/2025 | Citric Acid | CA20250413 | 10 | 500g | Rajesh Kumar |
Annexure-2: Sample Transfer Form
| Date | Material | Batch No. | Transferred To | Transferred By |
|---|---|---|---|---|
| 13/04/2025 | Citric Acid | CA20250413 | QC Laboratory | Sunita Reddy |
Annexure-3: Sampling Plan Template
| Total Containers | Sampling Plan Used | No. of Containers Sampled | Approach |
|---|---|---|---|
| 10 | √n+1 | 4 | Random + Stratified |
Revision History:
| Revision Date | Revision No. | Revision Details | Reason for Revision | Approved By |
|---|---|---|---|---|
| 01/01/2022 | 1.0 | Initial Release | New SOP | QA Head |
| 13/04/2025 | 2.0 | Added Sample Plan and Transfer Protocol | Annual SOP Review | QA Head |