API Manufacturing: SOP for Sampling and Testing of Raw Materials – V 2.0

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API Manufacturing: SOP for Sampling and Testing of Raw Materials – V 2.0

Standard Operating Procedure for Sampling and Testing of Raw Materials in API Manufacturing

Department API Manufacturing
SOP No. SOP/API/129/2025
Supersedes SOP/API/129/2022
Page No. Page 1 of 9
Issue Date 13/04/2025
Effective Date 15/04/2025
Review Date 13/04/2026

1. Purpose

To establish a standardized procedure for the sampling and testing of raw materials used in API manufacturing to ensure quality, identity, and compliance with approved specifications before use in production.

2. Scope

This SOP applies to Quality Control (QC) personnel responsible for sampling, testing, and approving raw materials received for use in the API manufacturing process, including active ingredients, excipients, and solvents.

3. Responsibilities

  • QC Sampler: Collect samples using clean tools and label containers properly.
  • QC Analyst: Test samples as per STP and record results in logbooks and reports.
  • QC Reviewer: Review and approve the results; determine compliance with specifications.
  • QA Officer: Ensure raw materials are not used before approval; verify traceability.
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4. Accountability

The Head – QC is accountable for ensuring raw materials are sampled and tested according to validated methods and GMP standards.

5. Procedure

5.1 Material Receipt and Quarantine

  1. Upon receipt, store raw materials in the quarantine area with a “To Be Sampled” status label.
  2. Verify material against invoice, delivery challan, and purchase order.

5.2 Sampling Plan

  1. Use appropriate sampling techniques based on material category:
    • Random sampling (for general materials)
    • Stratified sampling (for critical materials or multiple containers)
  2. Follow guidelines in Annexure-1 for number of containers and sample quantity.

5.3 Sampling Technique

  1. Use cleaned and dried sampling tools (e.g., thief sampler, pipette).
  2. Wear gloves and PPE before sampling.
  3. Open container under LAF or designated area to prevent contamination.
  4. Transfer sample to clean, labeled container indicating:
    • Material Name
    • Batch/Lot Number
    • Date of Sampling
    • Sampler’s Initials
  5. Seal the sample container and send it to the QC lab.
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5.4 Sample Identification and Coding

  1. Assign a unique Raw Material Sample Number as per internal coding format (e.g., RM/25/04/XXX).
  2. Enter details in the Sampling Logbook (Annexure-2).

5.5 Analytical Testing

  1. Test raw material samples as per the respective Standard Test Procedure (STP).
  2. Perform identity, assay, impurity, pH, LOD, and other tests based on material specifications.
  3. Record results in analytical worksheets and sign off upon completion.

5.6 Review and Release

  1. Compare results against the approved specification.
  2. If compliant, release the material with “Approved” status label and update inventory system.
  3. If out-of-specification (OOS), initiate investigation and inform QA.

5.7 Retention Sample

  1. Store a representative sample (minimum 25 g or as per policy) of each raw material batch in labeled container for reference.
  2. Store retention samples under defined conditions for at least 1 year after material expiry.

6. Abbreviations

  • QC: Quality Control
  • QA: Quality Assurance
  • RM: Raw Material
  • STP: Standard Test Procedure
  • OOS: Out of Specification
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7. Documents

  1. Sampling Logbook (Annexure-2)
  2. Raw Material Specification and STP
  3. Analytical Report
  4. Retention Sample Log

8. References

  • ICH Q7 – GMP for APIs
  • 21 CFR Part 211
  • WHO Technical Report Series No. 986

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 Guideline

Number of Containers Containers to Sample Composite Quantity
1 to 3 100% From each
4 to 10 √n + 1 Equal quantity from each
>10 √n + 1 Composite sample

Annexure-2: Sampling Logbook

Date Material Name Batch No. Sample No. Quantity Sampler Status
13/04/2025 Mannitol RM20250413 RM/25/04/101 100 g Ravi Kumar Sent to QC

Revision History:

Revision Date Revision No. Details Reason Approved By
01/01/2022 1.0 Initial SOP Procedure Standardization QA Head
13/04/2025 2.0 Added retention sample and coding system Regulatory Feedback QA Head
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