SOP for Sampling Frequency and Criteria for Raw Materials in Quarantine – V 2.0

Standard Operating Procedure for Sampling Frequency and Criteria for Raw Materials in Quarantine

Department	Quality Control / Quality Assurance / Warehouse
SOP No.	SOP/RM/078/2025
Supersedes	SOP/RM/078/2022
Page No.	Page 1 of 15
Issue Date	01/02/2025
Effective Date	05/02/2025
Review Date	01/02/2026

1. Purpose

This Standard Operating Procedure (SOP) defines the frequency and criteria for sampling raw materials stored in the quarantine area. It ensures that materials are sampled correctly to maintain quality, safety, and compliance with Good Manufacturing Practices (GMP).

2. Scope

This SOP applies to all raw materials, including Active Pharmaceutical Ingredients (APIs), excipients, solvents, and temperature-sensitive materials received and stored in the quarantine area before Quality Control (QC) testing and Quality Assurance (QA) approval.

3. Responsibilities

Quality Control (QC) Personnel: Perform sampling as per defined frequencies and criteria, and maintain sampling records.
Warehouse Personnel: Facilitate access to quarantined materials and ensure proper labeling and segregation.
Quality Assurance (QA): Review sampling procedures, verify compliance, and approve sampling plans.

4. Accountability

The QC Manager is responsible for ensuring that sampling is conducted per this SOP. The QA Manager ensures compliance with regulatory standards, and the Warehouse Manager ensures

proper storage and segregation of sampled materials.

5. Procedure

5.1 General Sampling Guidelines

Sampling Environment:
- Conduct sampling in designated sampling areas under controlled environmental conditions to prevent contamination.
- Ensure all sampling equipment is clean, calibrated, and sanitized before use.
Personnel Requirements:
- Only trained and authorized personnel are permitted to perform sampling.
- Personnel must wear appropriate personal protective equipment (PPE) as per SOP for handling quarantined materials.

5.2 Sampling Frequency

New Materials:
- For new suppliers or materials, sample every batch received until a consistent quality record is established (minimum of 5 consecutive conforming batches).
Routine Sampling:
- For approved suppliers, sample each batch received.
- For materials with extended shelf life and stable history, sampling frequency may be reduced based on risk assessment and QA approval.
Re-Test or Re-Evaluation:
- Materials stored in quarantine for more than 6 months must undergo re-sampling and testing.
- Materials approaching expiry should be sampled for re-evaluation based on the material’s stability data.

5.3 Sampling Criteria

Sampling Quantity:
- The quantity to be sampled is based on the type of material, container size, and specific test requirements.
- Refer to the Sampling Quantity Chart (Annexure-1) for standard sampling amounts.
Sampling Methodology:
- Follow random sampling techniques to ensure representative samples.
- For solids, use sampling thieves or scoops. For liquids, use pipettes or sampling bottles.
- For hazardous materials, follow additional safety protocols and use specialized equipment.
Container Selection:
- For batches with fewer than 5 containers, sample from all containers.
- For batches with 5-10 containers, sample from at least 50% of the containers.
- For batches with more than 10 containers, sample from a minimum of 10 containers or as specified by QA.

5.4 Documentation of Sampling

Sampling Records:
- Document all sampling activities in the Sampling Log (Annexure-2), including:
  - Date and time of sampling
  - Material name and batch number
  - Quantity sampled
  - Sampling method and equipment used
  - Personnel involved in sampling
Sample Labeling:
- Label samples with:
  - Material name
  - Batch number
  - Sampled by (name and signature)
  - Date of sampling
- Ensure samples are transported to the QC lab in sealed, contamination-free containers.

5.5 Handling Deviations in Sampling

Deviation Reporting:
- Report any deviations from the sampling procedure to the QA Manager immediately.
- Document deviations in the Sampling Deviation Report (Annexure-3).
Corrective Actions:
- Investigate the root cause of the deviation and implement corrective actions.
- Document corrective actions in the Corrective Action Log (Annexure-4).

6. Abbreviations

SOP: Standard Operating Procedure
GMP: Good Manufacturing Practice
QA: Quality Assurance
QC: Quality Control
PPE: Personal Protective Equipment

7. Documents

Sampling Quantity Chart (Annexure-1)
Sampling Log (Annexure-2)
Sampling Deviation Report (Annexure-3)
Corrective Action Log (Annexure-4)

8. References

21 CFR Part 211 – Current Good Manufacturing Practice for Finished Pharmaceuticals
ICH Q7 – Good Manufacturing Practice for Active Pharmaceutical Ingredients
EU Guidelines on Good Distribution Practices (GDP)

9. SOP Version

Version: 2.0

10. Approval Section

	Prepared By	Checked By	Approved By
Signature
Date
Name
Designation
Department

11. Annexures

Annexure-1: Sampling Quantity Chart

Material Type	Container Size	Sampling Quantity	Sampling Equipment
API	25 kg Drum	200 g	Sampling Thief
Solvent	50 L Drum	500 ml	Sampling Bottle

Annexure-2: Sampling Log

Date	Material Name	Batch Number	Quantity Sampled	Sampled By	Verified By (QA)
01/02/2025	API-X	X-2025-001	200 g	Ravi Kumar	Anjali Mehta
01/02/2025	Solvent-Y	Y-2025-002	500 ml	Sunita Sharma	Ajay Singh

Annexure-3: Sampling Deviation Report

Date	Material Name	Batch Number	Deviation Description	Reported By	Corrective Action Taken
02/02/2025	API-X	X-2025-001	Incorrect Quantity Sampled	Ravi Kumar	Resampled Correct Quantity

Annexure-4: Corrective Action Log

Date	Deviation Description	Corrective Action	Implemented By	Verified By (QA)
03/02/2025	Incorrect Sampling Method	Re-trained Sampling Personnel	Ajay Singh	Anjali Mehta

Revision History:

Revision Date	Revision No.	Revision Details	Reason for Revision	Approved By
01/01/2024	1.0	Initial Version	New SOP	QA Head
01/02/2025	2.0	Updated Sampling Frequency and Criteria Procedures	Regulatory Compliance	QA Head